Improved process for producing alkali metal methoxides

Abstract

The present invention relates to a method for producing at least one alkali metal methoxide by reactive distillation in at least one reaction column. At the bottom of the reaction column, the respective alkali metal methoxide dissolved in methanol is withdrawn. The methanol / water mixture obtained at the top of the reaction column is separated by distillation in a rectification column. The vapor obtained at the top of the rectification column is compressed in at least two stages, and the energy of each compressed vapor is advantageously transferred to the bottom stream and the side stream of the rectification column. This allows the method according to the invention to use the energy of the compressed vapor particularly efficiently. Furthermore, the energy of the alkali metal methoxide product stream obtained at the bottom of the reaction column is advantageously transferred to the vapor stream from the rectification column, which is then subjected, in particular, to compression. The energy of the compressed vapor can further be used to operate the reaction column or to operate a reaction column in which a process for alcohol exchange of alkali metal alkoxides is carried out.

Description

[Technical Field]

[0001] The present invention relates to a process for producing at least one alkali metal methoxide by reactive distillation in at least one reaction column, at the bottom of which the respective alkali metal methoxide dissolved in methanol is withdrawn, and the methanol / water mixture obtained at the top of the reaction column is separated by distillation in a rectification column.

[0002] The vapors obtained at the top of the rectification column are compressed in at least two stages, and the energy of each compressed vapor is advantageously transferred to the bottom stream and the side stream of the rectification column. This allows the process according to the invention to use the energy of the compressed vapors particularly efficiently. Furthermore, the energy of the alkali metal methoxide product stream obtained at the bottom of the reaction column is advantageously transferred to the vapor stream from the rectification column, which is then subjected, in particular, to compression.

[0003] The energy of the compressed vapor can further be used to operate a reaction column or columns in which the process of alcohol exchange of alkali metal alkoxides is carried out.

[0004] 1. Background of the Invention Alkali metal alkoxides are used as strong bases in the synthesis of many chemicals, such as the production of active pharmaceutical or agrochemical ingredients. Additionally, alkali metal alkoxides are applied as catalysts in transesterification and amidation reactions.

[0005] Alkali metal alkoxides are prepared, for example, by electrolysis, as described in EP-A-3885470.

[0006] A further possibility for producing alkali metal alkoxides is the conversion of alkali metal alkoxides with other alcohols. This "alcohol exchange" is described, for example, in Czechoslovak Federal Republic Patent No. 213119. This is advantageously carried out in a reaction column, as described in WO 2021 / 122702, U.S. Pat. No. 3,418,383, and DE 2726491.

[0007] Alternatively and most commonly, the production of alkali metal alkoxides (MOR) is carried out by reactive distillation from alkali metal hydroxides (MOH) and alcohol (methanol) in a countercurrent distillation column, following the reaction <1> The water of reaction formed according to is removed together with the distillate.

[0008] [ka]

[0009] Such a process principle is described, for example, in U.S. Pat. No. 2,877,274, WO 01 / 42178, CN 109627145, CN 208632416, WO 2021 / 148174, and WO 2021 / 148175, in which an aqueous alkali metal hydroxide solution and gaseous methanol are conveyed countercurrently in at least one reactive rectification column.

[0010] Similar processes, which additionally use an entrainer such as benzene, are described in GB 377,631 and U.S. Pat. No. 1,910,331. In this case, the entrainer serves to separate the water and the water-soluble alcohol. In both patents, the condensate is subjected to phase separation to separate the water of reaction.

[0011] Correspondingly, German Patent No. 968903 describes a process for the continuous production of alkali metal alkoxides in a reaction column, in which a water-alcohol mixture withdrawn at the top is condensed and subsequently subjected to phase separation. In this case, the aqueous phase is discarded, and the alcohol phase is returned to the column at the top together with fresh alcohol. A similar process is described in European Patent Application No. 0299577, in which water separation from the condensate is carried out using a membrane.

[0012] The most important alkali metal alkoxides industrially are those of sodium and potassium, in particular the methoxides and ethoxides, the synthesis of which has been described many times in the prior art, for example in EP 1 997 794 A1.

[0013] In the synthesis of alkali metal alkoxides by reactive rectification as described in the prior art, steam containing the used alcohol and water is usually obtained. For economic reasons, it is reasonable to reuse the alcohol contained in the steam as a reactant in reactive distillation. Therefore, the steam is usually supplied to a rectification column, and the alcohol contained therein is separated (for example, as described in GB 737453 and U.S. Pat. No. 4,566,947). The alcohol thus recovered is supplied, for example, as a reactant for reactive distillation.

[0014] Alternatively or additionally, a portion of the alcohol vapor can be used to heat the rectification column, as described, for example, in WO 2010 / 097318, EP 4074684, and EP 4074685. However, this requires compressing the vapor to reach the temperature required to heat the rectification column. Multistage compression of the vapor is particularly thermodynamically advantageous. In this case, the vapor is cooled between compression stages. Furthermore, intercooling helps to prevent the maximum allowable temperature of the compressor from being exceeded. A drawback of this cooling, as implemented in conventional methods, is that the extracted energy is dissipated without being utilized.

[0015] Therefore, there is a need for an improved process for producing alkali metal methoxides in which the resulting methanol / water mixture is worked up by a fractionation column. It is desirable that this process be characterized by low overall energy requirements, particularly efficient utilization of the energy contained in the compressed steam to operate the fractionation column. Therefore, it is desirable that this process enable efficient utilization of the heat generated during compression and cooling of the steam. Furthermore, it is desirable that this process be particularly gentle on the equipment (compressors) used during compression, thereby extending their lifespan. Finally, it is desirable that this process simplify the handling of the resulting product stream from the reaction column, such as during processing and storage.

[0016] 2. Summary of the invention The present invention solves the problem of the present invention by providing a compound of formula M A OCH3 [wherein, M A is selected from sodium, potassium, lithium, in particular selected from sodium, potassium, preferably sodium.

[0017] Optionally, the formula M A Simultaneously with and spatially separated from the conversion of OCH3 to alkali metal methoxide, a second reactor RR B Within, the formula MB OCH3 [wherein, M B is selected from sodium, potassium, lithium, in particular selected from sodium, potassium, preferably potassium], a further alkali metal methoxide is produced.

[0018] Here, the reactor RR A or reactor RR A and R.R. B At the top of the AB or two steam streams S AB and S BB The flow S AB or flow S AB and S BB are fed to the rectification column RD separately (i.e., not mixed with each other) or mixed with each other. A where it is separated by distillation into water and methanol. A Steam flow S at the head OA The vapor flow S OA is done in at least two stages, OA1 (Stage 1) or S OA2 (stage 2) and the compressed vapor stream S OA1 or S OA2 Or a part of the energy thereof can be advantageously transferred to a rectification column RD A Side stream S extracted from ZA (S OA1 (in the case of ) or bottom flow S UA Or some of them UA1 (S OA2 (if applicable) are integrated into the process of communicating

[0019] Furthermore, the energy is A The bottom product stream S AP and / or reactor RR B The bottom product stream S BP Flow S OA ,S OA1 ,S OA2, whereby the heat integration and therefore the energy efficiency is improved even further.

[0020] Bottom product flow S AP and / or bottom product stream S BP Flow S OA ,S OA1 ,S OA2 This transfer of energy to at least a portion of at least one of the flows S to which energy is transferred is preferably OA ,S OA1 ,S OA2 before being compressed. This prevents the formation of liquid phases in the stream to be compressed before and / or during compression, which could damage the compression equipment.

[0021] A further advantageous effect is that the bottom product stream S is cooled without energy being wasted and without additional energy having to be consumed for cooling. AP or bottom product stream S BP is cooled simultaneously. AP or bottom product stream S BP are easier to handle during processing or storage.

[0022] In a further preferred embodiment, the present invention relates to a method for the alcohol exchange of alkali metal alkoxides, in particular carried out in a reaction column, in which the alkali metal alkoxide M C The alcohol residue of OR' is replaced with another alcohol R"OH, where R' and R" are two different C1-C7 hydrocarbon residues, in particular R'=methyl and R"=C2-C7 hydrocarbon residues, preferably R'=methyl and R"=ethyl, n-propyl, isopropyl, more preferably R'=methyl and R"=ethyl. Here, S OA1 ,S OA2 Energy from at least a portion of the stream selected from is used in the process for alcohol exchange. [Brief explanation of the drawings]

[0023] [Figure 1] FIG. 1 illustrates a non-inventive embodiment of a method for producing alkali metal methoxide. [Figure 2] FIG. 10 illustrates a further embodiment of a method not according to the present invention. [Figure 3] FIG. 10 illustrates a further embodiment of a method not according to the present invention. [Figure 4] FIG. 10 illustrates a further embodiment of a method not according to the present invention. [Figure 5] 1 illustrates an embodiment of a method according to the invention; [Figure 6] FIG. 4 illustrates a further embodiment of the method according to the invention. [Figure 7] FIG. 4 illustrates a further embodiment of the method according to the invention. [Figure 8] FIG. 4 illustrates a further embodiment of the method according to the invention. [Figure 9] 1 illustrates an embodiment of a method according to the invention; [Figure 10] 1 illustrates an embodiment of a method according to the invention; [Figure 11] 1 illustrates an embodiment of a method according to the invention; [Figure 12] 1 illustrates an embodiment of a method according to the invention; [Figure 13] 1 illustrates an embodiment of a method according to the invention; [Figure 14] 1 illustrates an embodiment of a method according to the invention; [Figure 15] 1 illustrates an embodiment of a method according to the invention; [Figure 16A] 12 shows an embodiment of a heat transfer device in an embodiment according to the invention according to FIG. 11. FIG. [Figure 16B] FIG. [Figure 17] FIG. 1 illustrates the energy savings of the method according to the invention.

[0024] 3. Figure 3.1 Figure 1 FIG. 1 shows a non-inventive embodiment of a method for producing alkali metal methoxides, in which the distillative separation of the methanol-water mixture is carried out as in the prior art (substantially corresponding to FIG. 1 of WO 2010 / 097318).

[0025] Here, an aqueous NaOH solution is added to the reactor RR A <100> It is converted into sodium methoxide by methanol in the reactor RR. A <100> At the top of the column, an aqueous NaOH solution is introduced into the starting material stream S AE2 <102> Alternatively, a methanolic NaOH solution is also added to the starting stream S AE2 <102> To prepare the corresponding potassium methoxide, an aqueous or methanolic KOH solution can be added to the starting material stream S AE2 <102> To prepare the corresponding lithium methoxide, an aqueous or methanolic LiOH solution is added to the starting material stream S AE2 <102> Reactor RR A <100> Above the bottom of the AE1 <103> It is added in vapor form as

[0026] Reactor RR A <100> At the bottom of the AP <104> The corresponding alkali metal methoxide mixture is withdrawn from column RR. A <100> Bottom evaporator V SA <105> and an optional evaporator V SA’ <106> By S AP <104> The concentration of the sodium methoxide solution (or K solution or LiOCH3 solution) obtained as above is adjusted to the desired value.

[0027] Reactor RR A <100> At the head of the AB<107> is extracted. Condenser K RRA <108> Within, the steam flow S AB <107> A part of the liquid is condensed and refluxed in the reactor RR A <100> However, the condenser K RRA <108> and reflux generation is optional. Sodium methoxide solution S to the desired value AP <104> The concentration of can also be controlled by reflux.

[0028] The resulting vapor flow S AB <107> is a rectification column RD, which is a column for separating water and methanol. A <300> All or part of the product is fed to the rectification column RD. A <300> is the internal structure <310> Inside it, the steam flow S AB <107> is separated by distillation, and at the top, methanol is separated into the vapor stream S OA <302> It is recovered by distillation. A <300> In this case, a reflux stream can be generated. OA <302> Part of the condenser K RD <407> and then again in the rectification column RD A <300> It will be returned to S. OA <302> the remainder of the vapor stream S, or the complete vapor stream S in embodiments where reflux is not generated. OA <302> is the compressor VD AB2 <303> The image is pre-compressed by

[0029] If reflux is generated, alternatively or additionally, in particular alternatively, S intended as reflux OA <302> Part of S OA <302> is the compressor VD AB2 <303> Only after being pre-compressed in S OA <302> This possibility is indicated by the dashed line in each figure. <311> It is represented by:

[0030] This pre-compressed steam SOA <302> Part of S OA△ <307> is the reactor RR A <100> It is recycled into OA△ <307> is the starting material stream S AE1 <103> Used as.

[0031] S OA <302> The rest of S OA◆ <306> is compressor VD1 <401> So, this S OA◆ <306> is further compressed to form a vapor stream S OA1 <403> From there, an optional intercooler WT X <402> (shown in dotted lines in Figure 1 and each figure) OA1 <403> is the compressor VD x <405> The resulting steam S is then compressed again by OA2 <404> is used for heating the rectification column RD A <300> The bottom of the evaporator V SRD <406> This steam is then supplied to OA2 <404> optionally, a stream of fresh methanol <408> (depicted by the dashed line) is added, and this steam S OA2 <404> However, the rectification tower RD A <300> The reflux is fed back to the rectification column RD A <300> If generated by OA2 <404> This is RD A <300> before being returned to the reflux, i.e., K RD <407> Mix with condensate from the RD A <300> The rectification column RD can be fed to A <300> At the bottom of the UA <304> This water flow S UA <304> is at least partially (flow S UA1 <320> ) Rectification tower RD A <300> It was sent back to the UA <304> is the bottom evaporator V SRD<406> The other part is sent through the bottom evaporator V SRD’ <410> can be sent via

[0032] 3.2 Figure 2 Figure 2 shows a further embodiment of a method not according to the invention, which substantially corresponds to the embodiment shown in Figure 2 of WO 2010 / 097318.

[0033] This corresponds to the embodiment described in FIG. 1, but with the following additional or different features: a bottom evaporator V SRD’ <406> and V SRD’ <410> In addition, the rectification column RD A <300> is the intermediate evaporator V ZRD <409> Side flow S ZA <305> is the rectification tower RD A <300> is extracted from the intermediate evaporator V ZRD <409> Then it is sent to the rectification tower RD A <300> The steam flow S OA <302> Part of the compressor VD AB2 <303> The vapor flow S OA <302> The reflux branch from the steam stream S OA <302> Pre-compressor VD AB2 <303> Alternatively or additionally, reflux <311> This is the pre-compressor VD AB2 <303> After passing through S OA <302> It can also be branched from the partial flow S OA△ <307> is the reactor RR A <100> After being split into OA◆ <306> is compressor VD1 <401> The vapor is compressed in OA1 <403> This vapor flow S OA1 <403> For heating, an intermediate evaporator V ZRD <409> Supplied to S OA1 <403> Evaporator V by SRD <406> or evaporator VSRD’ <410> No heating occurs. ZRD <409> The steam flow S used to heat the OA1 <403> is K RD <407> mixed with condensate from the <408> and mixed with the reflux of the rectification column RD A <300> It will be returned to S. OA <302> From the rectification tower RD A <300> It is equally possible to return the reflux to the reactor separately.

[0034] 3.3 Figure 3 Figure 3 shows a further embodiment of the process not according to the invention, which corresponds to the embodiment described in Figures 1 and 2. Rectification column RD A <300> is the intermediate evaporator V ZRD <409> and bottom evaporator V SRD <406> , and optionally a bottom evaporator V SRD’ <410> It has.

[0035] The embodiment according to the invention has the following differences with respect to the previous embodiment: 1. Compressor VD1 <401> Steam flow in S OA <302> Part of S OA◆ <306> After compression, the vapor flow S OA1 <403> is divided into two parts S OA11 <4031> and S OA12 <4032> is separated into

[0036] 2.S OA11 <4031> The flow S ZA <305> To heat the intermediate evaporator V ZRD <409> are supplied to.

[0037] 3.S OA12 <4032> Furthermore, the compressor VD x <405> It is compressed and flows inside S OA2 <404> becomes S OA2 <404> The flow S UA1<320> To heat the bottom evaporator V SRD <406> are supplied to.

[0038] 4.S OA11 <4031> and S OA2 <404> is the temperature of each evaporator V ZRD <409> and V SRD <406> After exiting the condenser, they are combined and the combined stream is called the reflux stream (i.e., K RD <407> condensate from the <408> and mixed with the rectification column RD A <300> For this purpose, these streams are returned to the condensate container shown in FIG. <419> Alternatively, the condensate may be collected in a condensate container first, as described in the rectification column RD. A <300> Separate return of these flows to the .

[0039] 5.S OA△ <307> S OA <302> After being separated from S OA△ <307> In some cases, the compressor VD △ <411> It is compressed by OA△ <307> is the starting material stream S AE1 <103> As the reactor RR A <100> Used in additional compressor VD △ <411> By using the starting material stream S AE1 <103> The flow S is reused as OA△ <307> The pressure in the reactor RR A <100> This allows precise adjustment of the desired pressure ratio within the

[0040] Therefore, the difference with respect to the embodiment according to FIGS. 1 and 2 is the steam flow S OA is compressed in two stages, first to vapor S OA1 <403> , followed by steam S OA2 <404> The weaker compressed steam flow S OA1 <403> or a part thereof OA11 <4031> However, the side flow SZA <305> is used to heat the steam, while the more highly compressed steam is used to heat the bottom stream S UA <304> Part of S UA1 <320> By using it to heat the rectification column RD A <300> Heating of the gas is performed more efficiently compared to the embodiment of FIGS. 1 and 2 by steam flow.

[0041] 3.4 Figure 4 FIG. 4 shows a further embodiment of a method not according to the invention.

[0042] This corresponds to the embodiment described in FIG. 3, but with the following differences: 1. Compressor VD AB2 <303> Steam flow through S OA No pre-compression is performed. <401> It is supplied to and compressed into S OA1 <403> The steam flow S OA <302> Part of S OA◆ <306> is the condenser K RD <407> condensed by the rectification column RD A <300> The steam flow S minus the portion returned to the OA <302> Corresponds to.

[0043] 2. In this embodiment, additionally or alternatively, preferably alternatively, a compressed vapor stream S OA1 <403> A part of the reflux S OA13 <4033> Condenser K as RD <407> The condensate is condensed by the distillation column RD A <300> can be returned to.

[0044] 3.S OA1 <403> From some S OA● <308> is separated, and the starting material stream S AE1 <103> Here, S OA● <308> Optional compressor VD ● <415> It can be compressed by SOA● <308> is self-evident, but S OA11 <4031> and S OA12 <4032> Unlike, naturally, S OA13 <4033> It is also different from.

[0045] As already described for the embodiment according to FIG. 3, also in the embodiment according to FIG. OA11 <4031> But the flow S ZA <305> Intermediate evaporator V to heat ZRD <409> Supplied to S OA12 <4032> However, the compressor VD x <405> It is further compressed and flows inside OA2 <404> This compressed flow then becomes the flow S UA1 <320> To heat the bottom evaporator V SRD <406> Energy savings are achieved by transferring the differentially compressed streams to the side stream S ZA <305> and bottom flow S UA1 <320> This division results in greater energy efficiency.

[0046] 3.5 Figure 5 Figure 5 shows an embodiment of the method according to the invention, which corresponds to the embodiment described in Figure 3, but in which the heat transfer device WT ◆ <412> Energy in the form of heat is converted into S AP <104> From S OA◆ <306> In addition to the energy savings described for the embodiment according to Figs. AP <104> Further energy savings are achieved by reintegrating the residual heat in the steam stream S into the process rather than allowing it to dissipate unused. OA◆ <306> Heat exchanger WT ◆ <412> This is then heated by the compressor VD1 <401> This heating may further advantageously result in a vapor stream SOA◆ <306> Condensed liquid droplets present in the flow are transferred to a gaseous state or unwanted condensation of vapor is prevented before or during compression. Such droplets can have adverse effects on the compressor mechanism, and their avoidance therefore increases the lifespan of the equipment. Here, the flow S AP <104> It is also possible to utilize only a portion of the energy of the flow S AP <104> Only a portion of the energy in the flow is transferred, while the other portion <309> The energy of the part is not utilized. <309> is shown by a dashed line.

[0047] 3.6 Figure 6 FIG. 6 shows a further embodiment of the method according to the invention.

[0048] This corresponds to the embodiment described in FIG. 4, where the compressor VD ● <415> is not optional, but mandatory.

[0049] A further difference with respect to the embodiment according to FIG. 4 is that the heat transfer device WT ● <416> Energy in the form of heat is converted into S AP <104> From S OA● <308> In addition to the energy saving advantages described for the embodiment according to FIGS. AP <104> Further energy savings are achieved because residual heat in the S is reintegrated into the process rather than being dissipated unused. AP <104> Energy from the heat exchanger WT ● <416> The vapor flow S OA● <308> and then S OA● <308> The compressor VD ● <415> This heating may result in a further advantage of the steam flow S OA● <308> The condensed droplets present in the vapor stream S are converted to a gaseous state or vapor stream S before or during compression. OA●<308> Such droplets can have a negative effect on the compressor mechanism, and their avoidance therefore increases the lifespan of the equipment. Here, the flow S AP <104> It is also possible to utilize only a portion of the energy of the flow S AP <104> Only a portion of the energy in the flow is transferred, while the other portion <309> The energy of the part is not utilized. <309> is shown by a dashed line.

[0050] 3.7 Figure 7 FIG. 7 shows a further embodiment of the method according to the invention.

[0051] This corresponds to the embodiment described in FIG. 3, where the compressor VD △ <411> is not optional, but mandatory.

[0052] A further difference with respect to embodiment 3 is that the heat transfer device WT △ <417> Energy in the form of heat is converted into S AP <104> From S OA△ <307> In addition to the energy saving advantages described for the embodiment according to FIG. AP <104> Further energy savings are achieved because the residual heat in S is reintegrated into the process rather than being dissipated unused. AP <104> Energy from the heat transfer device WT △ <417> Integrating by means of the steam flow S OA△ <307> is heated, and then this is passed through the compressor VD △ <411> This heating may result in a vapor stream S OA△ <307> Condensed liquid droplets present in the flow are transferred to a gaseous state or unwanted condensation of vapor is prevented before or during compression. Such droplets can have adverse effects on the compressor mechanism, and their avoidance therefore increases the lifespan of the equipment. Here, the flow S AP<104> It is also possible to utilize only a portion of the energy of the flow S AP <104> Only a portion of the energy in the flow is transferred, while the other portion <309> The energy of the part is not utilized. <309> is shown by a dashed line.

[0053] 3.8 Figure 8 FIG. 8 shows a further embodiment of the method according to the invention.

[0054] This corresponds to the embodiment described in FIG. 4, where the compressor VD ● <415> is not optional, but mandatory.

[0055] A further difference with respect to embodiment 4 is that the heat transfer device WT ◆ <412> Energy in the form of heat is converted into S AP <104> From S OA◆ <306> The purpose is to communicate this to the public.

[0056] In addition, the flow S OA11 <4031> This is the intermediate evaporator V ZRD <409> Energy is transferred to the side stream S ZA <305> After transferring the heat to the heat transfer device WT ◆ <412> The residual energy in the form of heat is transferred via S OA11 <4031> From S OA◆ <306> In addition to the energy saving advantages described for the embodiment according to FIG. AP <104> and flow S OA11 <4031> Further energy savings are achieved because residual heat in the S is reintegrated into the process rather than being dissipated unused. AP <104> and S OA11 <4031> Energy from the heat exchanger WT ◆ <412> Integrating by this gives the steam flow S OA◆ <306> Then, the steam flow S OA◆<306> Compressor VD1 <401> This heating may further advantageously result in a vapor stream S OA◆ <306> The condensed liquid droplets present in the vapor S are converted to a gaseous state or vapor S before or during compression. OA◆ <306> Such droplets can have a negative effect on the compressor mechanism, and their avoidance therefore increases the lifespan of the equipment. Here, the flow S AP <104> It is also possible to utilize only a portion of the energy of the flow S AP <104> Only a portion of the energy in the flow is transferred, while the other portion <309> The energy of the part is not utilized. <309> is shown by a dashed line. Similarly, the flow S OA11 <4031> Only a portion of the residual heat is used. ◆ <412> It can also be used for energy integration by (not shown in Figure 8).

[0057] 3.9 Figure 9 9 shows an embodiment of the method according to the invention, which corresponds to the embodiment described in FIG.

[0058] The difference with respect to embodiment 3 is that the heat transfer device WT AB2 <418> By this, energy in the form of heat is converted into AP <104> From the compressor VD AB2 <303> Pre-compressed in S OA <302> The purpose is to transmit it as part of the flow.

[0059] In addition, the flow S OA11 <4031> This is the intermediate evaporator V ZRD <409> Energy is transferred to the side stream S ZA <305> After transferring the heat to the heat transfer device WT AB2 <418> The residual energy in the form of heat is transferred via S OA11 <4031> From VD AB2 <303> The flow to be precompressed by S OA<302> Transmit to part of.

[0060] In addition to the energy saving advantages described for the embodiment according to FIG. 3, it is thereby possible to reduce the bottom flow S AP <104> and flow S OA11 <4031> Further energy savings are achieved because the residual heat in S is reintegrated into the process rather than being dissipated unused. AP <104> and S OA11 <4031> Energy from the heat transfer device WT AB2 <418> The integration by OA <302> A part of the AB2 <303> This heating may result in a vapor stream S OA <302> The condensed liquid droplets present in this portion of the vapor S are converted to a gaseous state or vapor S before or during precompression. OA <302> Such droplets can have a negative effect on the compressor mechanism, and their avoidance therefore increases the lifespan of the equipment. Here, the flow S AP <104> It is also possible to utilize only a portion of the energy of the flow S AP <104> Only a portion of the energy in the flow is transferred, while the other portion <309> The energy of the part is not utilized. <309> is shown by a dashed line. Similarly, the flow S OA11 <4031> It is also possible to utilize only a portion of the residual heat (not shown in FIG. 9).

[0061] The method implemented in Example 4 (Section 5.4) according to the present invention is based on the apparatus shown in FIG. 9, and in Example 4, the compressor VD △ <411> Flow by S OA△ <307> No compression was performed.

[0062] 3.10 Figure 10 Figure 10 shows an embodiment of the method according to the invention, which corresponds to the embodiment described in Figure 3, but with the following differences: Second reactor RR B <200> In the RR A <100> It is converted to potassium methoxide by methanol, which is also used in the conversion in situ.

[0063] Reactor RR B <200> At the top of the column, an aqueous KOH solution is introduced into the starting material stream S BE2 <202> Alternatively, a methanolic KOH solution is also added to the starting stream S BE2 <202> It can be added as the reactor RR B <200> Above the bottom of the BE1 <203> It is added in vapor form as

[0064] Reactor RR B <200> At the bottom of the BP <204> The mixture of corresponding methoxides in the column RR is withdrawn. B <200> The bottom evaporator V at the bottom of SB <205> and an optional evaporator V SB’ <206> Potassium methoxide solution S BP <204> The concentration of is adjusted to the desired value.

[0065] Reactor RR B <200> At the head of the BB <207> is extracted. Condenser K RRB <208> Within, the steam flow S BB <207> A part of the liquid is condensed and refluxed in the reactor RR B <200> However, the condenser K RRB <208> and reflux generation is optional. Potassium methoxide solution S to the desired value BP <204> The concentration of can also be controlled by reflux.

[0066] The resulting steam S BB <207> is the condenser K RRA <108> The steam S that was not condensed in AB <107> It is mixed with a part of the rectification column RD A <300> are supplied to.

[0067] A further difference with respect to the embodiment according to FIG. 3 is that the steam flow S OA <302> The pre-compressed part S OA△ <307> However, the reactor RR A <100> and reactor RR B <200> where this pre-compressed part S OA△ <307> is the starting material flow S AE1 <103> or S BE1 <203> It is used as.

[0068] A further difference with respect to the embodiment according to FIG. 3 is that the heat transfer device WT AB2 <418> By this, energy in the form of heat is converted into AP <104> From the compressor VD AB2 <303> Pre-compressed in S OA <302> The purpose is to transmit it as part of the flow.

[0069] In addition, the flow S BP <204> Similarly, the heat transfer device WT AB2 <418> The residual energy in the form of heat is transferred via S BP <204> From VD AB2 <303> The precompressed flow S OA <302> Transmit to part of.

[0070] In addition to the energy saving advantages described for the embodiment according to FIG. 3, it is thereby possible to reduce both bottom flows S AP <104> and S BP <204> Further energy savings are achieved because residual heat in the S is reintegrated into the process rather than being dissipated unused. AP <104> and S BP<204> Energy in the heat transfer device WT AB2 <418> The integration by OA <302> A part of the AB2 <303> This heating may further advantageously result in a vapor stream S OA <302> The condensed droplets present in the S are converted to a gaseous state or the S before or during precompression OA <302> Such droplets can have a negative effect on the compressor mechanism, and their avoidance therefore increases the lifespan of the equipment. Here, the flow S AP <104> Part of and / or flow S BP <204> Only a part of the energy of WT AB2 <418> (not shown in FIG. 10).

[0071] 3.11 Figure 11 Figure 11 shows an embodiment of the method according to the invention, which corresponds to the embodiment described in Figure 10, but with the following differences: 1) S OA2 <404> Part of S OA21 <4041> Only the bottom evaporator V SRD <406> It is used to heat the S OA2 <404> The rest of the towers are A <100> The bottom of the evaporator V SA’ <106> and Tower RR B <200> The bottom of the evaporator V SB’ <206> It is used to heat the

[0072] 2) As shown in Figure 10, the energy in the form of heat is transferred to the heat transfer device WT AB2 <418> By S AP <104> and S BP <204> From the compressor VD AB2 <303> Pre-compressed in S OA<302> In addition, the flow S OA11 <4031> This is the intermediate evaporator V ZRD <409> Energy is transferred to the side stream S ZA <305> After transferring the heat to the heat transfer device WT AB2 <418> The heat is transferred through the OA11 <4031> The residual energy at S OA11 <4031> From VD AB2 <303> The flow to be precompressed by S OA <302> Transmit to part of.

[0073] 3) The following flows are directed to the condensate container: <419> (described in Section 4.9.5) and then these are combined and released into the rectification column RD A <300> Sent to: - Condenser K as reflux RD <407> The flow S sent through OA <302> Part of; -S OA11 <4031> and this flow passes through the intermediate evaporator V ZRD <409> and heat transfer device WT AB2 <418> The one after passing through; -S OA2 <404> and this flow is fed to the bottom evaporator V SRD <406> Partially passes through the bottom evaporator V SA’ <106> and V SB’ <206> after partial passage of ; - Optional flow of fresh methanol <408> .

[0074] 4) In addition, a condensate container <419> From the rectification tower RD A <300> The conduit leading to the condenser K RD <407> Advantageously, a pressure equalization is established by connecting the supply to the <420> The reflux is drawn as a dashed line. <311> In an embodiment, the connection <420> Also, a condensate container <419> From the rectification tower RD A<300> From the conduit leading to <311> It may occur up to.

[0075] Compressor VD AB2 <303> The advantages obtained in terms of energy efficiency and extended life span correspond to those described for the embodiment according to FIG.

[0076] 3.12 Figure 12 Figure 12 shows an embodiment of the method according to the invention, which corresponds to the embodiment described in figure 10, but with the following differences: 1) Reactor RR A <100> and R.R. B <200> is the intermediate evaporator V ZA <110> and V ZB <210> Each has a side flow S ZAA <111> is the reactor RR A <100> Extracted from V ZA <110> and then sent to the reactor RR A <100> The side stream S ZBA <211> is the reactor RR B <200> Extracted from V ZB <210> and then sent to the reactor RR B <200> is supplied again.

[0077] 2) S OA2 <404> Part of S OA21 <4041> Only the bottom evaporator V SRD <406> It is used to heat the S OA2 <404> The rest of the towers are A <100> The bottom of the evaporator V SA’ <106> It is used to heat the

[0078] 3) S OA1 <403> Part of the intermediate evaporator V ZB <210> It is used to heat the

[0079] 4) Pre-compressor VD AB2<303> Steam flow S OA <302> Pre-compression of some of the is optional.

[0080] 5) Compressor VD △ <411> is not optional, but mandatory.

[0081] Heat Transfer Unit WT △ <417> The energy in the form of heat is S AP <104> and S BP <204> From S OA△ <307> is transmitted to.

[0082] Compressor VD △ <411> The advantages obtained in terms of energy efficiency and extended life span correspond to those described for the embodiment according to FIG.

[0083] 3.13 Figure 13 Figure 13 shows an embodiment of the method according to the invention, which corresponds to the embodiment described in figure 10, but with the following differences: 1) Reactor RR A <100> is the intermediate evaporator V ZA <110> Side flow S ZAA <111> is the reactor RR A <100> Extracted from V ZA <110> and then sent to the reactor RR A <100> is supplied again.

[0084] 2) S OA2 <404> Part of S OA21 <4041> Only the bottom evaporator V SRD <406> It is used to heat the S OA2 <404> The rest of the towers are B <200> The bottom of the evaporator V SB’ <206> Used to heat the

[0085] 3) Intermediate evaporator V ZA <110> The heat is transferred to the intercooler WTX <402> Inside S OA12 <4032> Absorbed from intermediate evaporator V ZA <110> Discharge within the pump <501> Heat transfer medium W1 transported by <502> , especially heated by water.

[0086] 4) Heat Transfer Unit WT AB2 <418> The energy in the form of heat is S BP <204> From S OA <302> is transmitted to part of the flow, but S AP <104> It is not transmitted from

[0087] The energy advantages obtained correspond to those described for the embodiment according to FIG.

[0088] 3.14 Figure 14 Figure 14 shows an embodiment of the method according to the invention, which corresponds to the embodiment described in Figure 10, but with the following differences: 1) Reactor RR A <100> and R.R. B <200> is the intermediate evaporator V ZA <110> and V ZB <210> Each has a side flow S ZAA <111> is the reactor RR A <100> Extracted from V ZA <110> and then sent to the reactor RR A <100> The side stream S ZBA <211> is the reactor RR B <200> Extracted from V ZB <210> and then sent to the reactor RR B <200> is supplied again.

[0089] 2) S OA2 <404> Part of S OA21 <4041> Only the bottom evaporator V SRD <406> It is used to heat the S OA2 <404> The rest of the towers areA <100> The bottom of the evaporator V SA’ <106> and tower RR for heating B <200> The bottom of the evaporator V SB’ <206> Used to heat the

[0090] 3) Heat Transfer Unit WT AB2 <418> The energy in the form of heat is S BP <204> From S OA <302> is transmitted to part of the flow, but S AP <104> It is not transmitted from

[0091] 4) In addition, Figure 14 shows that the flow S OA12 <4032> Reactive rectification column RR for alcohol exchange of sodium methoxide to sodium ethoxide, operated with energy from C <600> Shows Tower RR C <600> is the bottom evaporator V SC <605> and V SC’ <606> It has.

[0092] Here, sodium methoxide solution S CE1 <602> is the reactor RR C <600> In the countercurrent, ethanol S CE2 <603> to sodium ethoxide, which is extracted as an ethanolic solution.

[0093] Reactor RR C <600> At the bottom of the column, a bottom product stream S containing sodium ethoxide is obtained. CP <604> is extracted.

[0094] Reactor RR C <600> At the head of the CB <607> Here, the condenser K RRC <608> Within, the steam flow S CB<607> At least a portion of the condensed mixture is refluxed in the reaction column RR. C <600> Here, the steam flow S CB <607> is gaseous and condenser K RRC <608> (shown in dashed lines) and / or <609> As a liquid in the condenser K RRC <608> is pulled out behind.

[0095] Side flow S ZC <610> is the reactor RR C <600> It is preferable to extract the side stream S ZC <610> Intermediate evaporator V ZC <611> Energy is transferred by, and then, S ZC <610> RR C <600> can be sent back again.

[0096] Sodium methoxide solution S CE1 <602> Preferably, the reaction column RR A <100> and R.R. B <200> The bottom flow S obtained within AP <104> and S BP <204> At least a portion of the

[0097] Bottom evaporator V SC’ <606> The heat is transferred to the intercooler WT X <402> Inside S OA12 <4032> Absorbed from the bottom evaporator V SC’ <606> Discharge within the pump <501> Heat transfer medium W1 transported by <502> , especially heated by water.

[0098] Alternatively, the energy can be expressed as S OA2 <404> ,S OA11 <4031> ,S OA11 <4031> and S OA12 <4032> Before separation into S OA1 <403> From the other stream selected from the bottom evaporator VSC’ <606> or other bottom evaporator V SC <605> It can also be transmitted to the flow S OA1 <403> ,S OA11 <4031> ,S OA12 <4032> ,S OA2 <404> , bottom product flow S AP <104> , bottom product flow S BP <204> Similarly, energy is extracted from at least one of the ethanol stream S CE1 <603> , sodium methoxide solution S CE1 <602> , or side flow S ZC <610> to achieve even better energy integration.

[0099] S AP <104> From compressor VD AB2 <303> The flow S to be precompressed OA <302> The energy benefits obtained by integrating the energy into a part of the compressor VD AB2 <303> The protection of the device corresponds to that described for the embodiment according to FIG.

[0100] 3.15 Figure 15 Figure 15 shows an embodiment of the method according to the invention, which corresponds to the embodiment described in Figure 14, but with a bottom evaporator V SC’ <606> Heating is S OA2 <404> The difference is that it is carried out directly by some of the

[0101] 3.16 Figures 16A and 16B FIG. 16A shows a heat transfer device WT in an embodiment according to the invention, for example, according to FIG. AB2 <418> It can be used as a heat transfer device <8> This embodiment of the heat transfer device is shown. <8> There are three plates <81> , <82> and <83> These plates are <84> The area enclosed by <80> , <87> , <88> and <89> Separate them from each other.

[0102] plate <81> , <82> and <83> is a hollow body through which the bottom product stream S AP <104> (plate <81> ) and S BP <204> (plate <82> ), as well as flow S OA11 <4031> (plate <83> ) is introduced. Here, each flow is <85> The valves are connected to each plate. <86> The air is discharged from each plate through the

[0103] The gaseous stream to be heated, in the case shown, the steam stream S OA <302> is supplied to the container, e.g. via a valve. <84> Area <80> Guided by the plate <81> , <82> and <83> or area <80> , <87> , <88> and <89> The heated gaseous stream, in the case shown, the vapor stream S OA <302> is supplied to the container, e.g. via a valve. <84> Area <89> Exit again.

[0104] In this way, the plate <81> , <82> and <83> is a container <84> and / or steam flow S OA <302> can pass through them, and at the same time the energy S OA <302> and the flow S through each plate AP <104> ,S BP <204> ,S OA11 <4031> The shape is designed so that it can be exchanged between the plates. <81> , <82> and <83> The flow S OA <302> Perforation holes through which fluid flows <90> It is understood that these perforations may be hollow bodies (e.g. holes such as slots). <90> is a plate <81> , <82> and <83> The installation must be such that the medium flowing through it does not leak.

[0105] This embodiment is shown in FIG. 16B as a plate <83> In FIG. 16A, the plate <83> is drawn horizontally, and the flow S OA <302> The side <831> From the side <832> In Figure 16B, the plate <83> The side <831> is depicted in plan view.

[0106] Alternatively, perforations <90> No plates <81> , <82> and <83> In this case, these plates are arranged so that the flow to be heated is <81> , <82> and <83> for example, obliquely, i.e., so that their maximum extension is <84> The inner diameter of the container must be smaller than <84> Finally, in the case of tube bundle evaporators, the plate <81> , <82> and <83> Instead, a tube or tube bundle is used.

[0107] Here, according to the present invention, in an embodiment, energy in the form of heat is AP <104> ,S BP <204> and S OA11 <4031> From S OA <302> Therefore, S AP <104> ,S BP <204> and S OA11 <4031> is more energetic at the time of supply to each plate, as indicated by each solid arrow, than at the time of discharge, as indicated by each dashed arrow. OA <302> is the heat transfer rate, which is higher than the discharge rate (solid arrow). <8> Here, the energy is less when the valve is supplied to the <85> and <86> is a plate <81> and <82> may be located on the same side of the vessel as shown in <83> They may be arranged on opposite sides as shown.

[0108] Obviously, the number of plate packages can be varied depending on the flow from which energy is used to load the energy stream. OA <302> , plate package <81> , <82> , <83> Through the flow S AP <104> ,S BP <204> and S OA11 <4031> Energy from is loaded.

[0109] Optionally, if additional flow is utilized as an energy source, a heat transfer device <8> can be extended to further plates, e.g., a fourth plate. Alternatively, these additional plates (or similarly <81> , <82> or <83> ) can be operated by an external heat source, which is particularly advantageous for the start-up process. AP <104> ,S BP <204> and S OA11 <4031> Only the energy from one of the steam flows S OA <302> Optionally, if the plate needs to be transmitted to <81> , <82> , <83> One or two of these can be omitted.

[0110] In the embodiment according to FIG. 9 (example 4 according to the invention), for example, S AP <104> and S OA11 <4031> Only the energy from S OA <302> In this embodiment, the last plate <83> , and therefore the area <88> can be omitted.

[0111] 3.17 Figure 17 17 illustrates the energy savings in the method according to Example 4 compared to the non-inventive methods according to Examples 1-3. The x-axis represents each example, and the y-axis represents the applied power (heating steam power and compressor power) in kW. The shaded portion of the bar represents the required heating power from low-pressure steam, and the white portion of the bar represents the total compressor power.

[0112] 4. Detailed Description of the Invention The present invention relates to a compound of formula M A OCH3 [wherein, M A is a metal selected from sodium, potassium and lithium, in particular sodium and potassium, preferably sodium.

[0113] The process according to the invention is carried out in at least one reactive rectification column, in which the vapor stream comprising methanol and water obtained therein is subsequently at least partially separated into water and methanol in the distillative separation, which allows for efficient integration of the energy of the vapors obtained therein and of the energy of the product stream obtained in the at least one reactive rectification column.

[0114] 4.1 Process (a1) 4.1.1 General description of step (a1) In step (a1) of the process according to the invention, a starting material stream S comprising methanol is AE1 is M A OH-containing starting material stream S AE2 By this, the reactive rectification column RR A Countercurrently converted within the A OCH3, water, methanol, M A Crude product RP containing OH A becomes.

[0115] According to the present invention, a "reactive rectification column" is defined as a rectification column in which at least some parts undergo the conversion according to step (a1) or step (a2) of the process according to the invention. This may also be abbreviated as "reaction column".

[0116] In step (a1), RR A At the bottom of A a bottom product stream S containing OCH AP is extracted. RR A At the top of the column, a vapor stream S containing water and methanol is generated. AB is extracted.

[0117] M A is selected from sodium, potassium, and lithium. A is in particular selected from sodium and potassium. A = sodium.

[0118] Starting material stream S AE1 In a preferred embodiment, S AE1 The mass fraction of methanol in the mixture is 95% by weight or more, and even more preferably 99% by weight or more. AE1 In particular, it comprises water.

[0119] In step (a1), the starting material stream S AE1 The methanol used as may be commercially available methanol having a mass fraction of more than 99.8% by weight and a mass fraction of water up to 0.2% by weight.

[0120] Starting material stream S AE1 is preferably added in vapor form.

[0121] Starting material stream S AE2 is M A In a preferred embodiment, S AE2 is M A In addition to OH, it contains at least one further compound selected from water, methanol. Even more preferably, S AE2 is M A In addition to OH, it also contains water, in this case S AE2 is M A It is an aqueous solution of OH.

[0122] Starting material stream SAE2 M A If OH and water are included, S AE2 M based on the total weight of the aqueous solution forming A The mass fraction of OH is in particular in the range of 10 to 75% by weight, preferably 15 to 54% by weight, more preferably 30 to 53% by weight, and particularly preferably 40 to 52% by weight.

[0123] Starting material stream S AE2 M A When OH and methanol are included, S AE2 M in methanol based on the total weight of the solution forming A The mass fraction of OH is in particular in the range of 10 to 75% by weight, preferably 15 to 54% by weight, more preferably 30 to 53% by weight, and particularly preferably 40 to 52% by weight.

[0124] Starting material stream S AE2 M A In certain cases containing both water and methanol in addition to OH, S AE2 M in methanol and water based on the total weight of the solution forming A It is particularly preferred that the mass fraction of OH is in the range of 10 to 75% by weight, preferably 15 to 54% by weight, more preferably 30 to 53% by weight, and particularly preferably 40 to 52% by weight.

[0125] Step (a1) is carried out in a reactive rectification column (or "reaction column") RR A It will be carried out within

[0126] Step (a2), which will be described in more detail in Section 4.2, also involves a reactive rectification column (or "reaction column") RR B It will be carried out within

[0127] Preferably, the reaction column is a RR A or RR B includes internals. Suitable internals are, for example, trays, structured packing, or unstructured packing. A or RR BIf reactor RR contains trays, bubble cap trays, valve trays, tunnel cap trays, Thoman trays, cross-slot bubble cap trays, or sieve trays are suitable. A or RR B If the system includes trays, preferably trays are selected such that a maximum of 5% by weight of liquid, preferably less than 1% by weight, penetrates each tray. The construction measures required to minimize liquid penetration are common to those skilled in the art. In the case of valve trays, for example, particularly tight-sealing valve types are selected. Furthermore, by reducing the number of valves, the steam velocity at the tray openings can be increased by twice the value normally adjusted. When using sieve trays, it is particularly advantageous to reduce the diameter of the tray openings while maintaining or even increasing the number of openings.

[0128] When structured or unstructured packing is used, structured packing is preferred for uniform distribution of liquid.

[0129] In the case of columns with unstructured packing, especially packings, and in the case of columns with structured packing, the desired liquid distribution characteristics can be obtained by reducing the liquid trickle density in the edge region of the column cross section adjacent to the column shell, which corresponds to about 2-5% of the total column cross section, by up to 100%, preferably 5-15%, compared to the rest of the cross section. This can be achieved, for example, by targeting the drip points or holes of the liquid distributor by simple means.

[0130] The process according to the invention can be carried out both continuously and discontinuously. Preferably, the process is carried out continuously.

[0131] According to the present invention, a "methanol-containing starting material stream S AE1 , M A OH-containing starting material stream S AE2 By In countercurrent "Converting" refers in particular to the reaction column RR A In step (a1), the methanol-containing starting material stream SAE1 At least some of the supply points of M A OH-containing starting material stream S AE2 This is ensured by being below the supply point of

[0132] Reactor RR A is preferably the starting material stream S AE1 The feed point and the starting material flow S AE2 Between the feed point and the reactor, there are at least two, in particular 15 to 40 theoretical plates.

[0133] Reactor RR A can be operated as a pure stripping column. A In the lower region of the AE1 is supplied in vapor form.

[0134] Step (a1) comprises the step of: AE1 Part of M A OH-containing starting material stream S AE2 Although the feed point of the reactor RR is below the feed point of the reactor RR, A This also includes the case where the gas is added in vapor form to the top or top region of the reactor RR. A The size of the lower region of the starting material stream S containing methanol can be reduced. AE1 Part of the reaction column RR A When the methanol is fed to the top or top region of the reaction column RR, only a fraction of 10 to 70 wt. %, preferably 30 to 50 wt. % (each based on the total amount of methanol used in step (a1)) is fed to the top or top region of the reaction column RR. A The remaining part is fed in a single stream or distributed into several part streams to the bottom end of the sieve, preferably on 1 to 10 theoretical plates, particularly preferably on 1 to 3 theoretical plates, M A OH-containing starting material stream S AE2 It is added in vapor form below the feed point of

[0135] Reactor RR A Then, a starting material stream S containing methanol is AE1However, the reaction described earlier <1> According to M A OH-containing starting material stream S AE2 is converted by M A OCH3 and HO, and since this is an equilibrium reaction, these products are the same as the reactants methanol and M A Thus, in step (a1), the crude product RP A is the reactor RR A The crude product RP A is the product M A In addition to OCH3 and water, methanol and M A Includes OH.

[0136] RR A At the lower end of A a bottom product stream S containing OCH AP is obtained and then extracted.

[0137] RR A The upper end of the A At the top of the column, a vapor stream S containing water and methanol is generated. AB A methanol stream, still containing water, called "methanol stream" is withdrawn.

[0138] This vapor stream S containing water and methanol AB In step (a3), at least part of the rectification column RD A where the RD A A methanol-containing vapor stream S is withdrawn at the top of OA and R.D. A At least one stream S containing water to be extracted at the lower end of UA Furthermore, in embodiments of the present invention in which step (a2) is performed, the vapor stream S BB At least part of AB Mixed with or S AB Separated from the rectification column RD A is led to.

[0139] During the distillation in step (a3), the flow SOA A part of the methanol obtained in the reactor RR A Starting material stream S AE1 If step (a2) is carried out, then alternatively or additionally, in step (a2), the reaction column RR B Starting material stream S BE1 It can be supplied as

[0140] In a more preferred embodiment of the method according to the invention, the vapor stream S OA 5 to 95 wt. %, preferably 10 to 90 wt. %, more preferably 20 to 80 wt. %, even more preferably 30 to 70 wt. %, even more preferably 50 to 60 wt. %, even more preferably 56.7 wt. % of the starting material stream S AE1 or, if step (a2) is performed, alternatively or additionally in step (a2) as starting material stream S BE1 Used as.

[0141] In this preferred embodiment, the starting material stream S AE1 or starting material stream S BE1 Used as flow S OA It is advantageous to compress a portion of the

[0142] In this regard, preferred embodiments △, ●, ◇ are described in section 4.10.

[0143] Starting material stream S AE1 The amount of methanol contained in the bottom product stream S AP Alkali metal methoxide M obtained in A Preferably, the starting material stream S AE1 The amount of methanol in the reactor RR A At the bottom of the A a bottom product stream S containing OCH AP The concentration of the alkali metal methoxide solution is selected to be the desired concentration.

[0144] In a preferred embodiment of the method according to the invention, in particular S AE2 M A If the starting material stream S AE1 The total weight (mass; unit: kg) of methanol used as starting material in step (a1) is AE2 Used as M A The ratio of the total weight (mass; unit: kg) of OH is 4:1 to 50:1, more preferably 8:1 to 48:1, even more preferably 10:1 to 45:1, even more preferably 20:1 to 40:1, and even more preferably 22:1.

[0145] Reactor RR A may be operated with or without reflux, preferably with reflux.

[0146] "With reflux" refers to each tower, and in step (a1), the reaction tower RR A In optional step (a2), the reaction column RR B A vapor stream S containing water and methanol is withdrawn at the top end of the AB or S BB In other words, in this case, in step (a3), the vapor flow S AB or S BB is the rectification tower RD A In step (a1), the reaction mixture is not completely introduced into the reaction column RR but is at least partially, preferably partially, introduced into each column as reflux. A In optional step (a2), the reaction column RR BIn this context, if such a reflux is generated, the reflux ratio is preferably 0.01 to 1, more preferably 0.02 to 0.9, even more preferably 0.03 to 0.34, even more preferably 0.04 to 0.27, even more preferably 0.05 to 0.24, even more preferably 0.06 to 0.10, even more preferably 0.07 to 0.09. Reflux ratio is generally understood within the meaning of the present invention to mean the ratio of the proportion of the mass flow rate (kg / h) withdrawn from the column that is returned to the column in liquid form (reflux) to the proportion of this mass flow rate (kg / h) that is discharged from the respective column in liquid or gaseous form.

[0147] The reflux can be generated by installing a condenser at the head of each column. In step (a1), therefore, in particular the reaction column RR A Condenser K RRA In step (a2), for this purpose, in particular the reaction column RR B Condenser K RRB In each condenser, each vapor flow S AB or S BB is at least partially condensed and fed to each column in step (a1) into the reaction column RR A In step (a2), the reaction column RR B is supplied again.

[0148] Reactor RR A In the embodiment where reflux is generated in step (a1), starting material stream S AE2 Used as M A OH can also be at least partially mixed with the reflux stream and the resulting mixture can then be fed to step (a1).

[0149] Step (a1) is in particular carried out at a temperature in the range from 45°C to 150°C, preferably in the range from 47°C to 120°C, more preferably in the range from 60°C to 110°C, and at a pressure in the range from 0.5 bar (absolute) to 40 bar (absolute), preferably in the range from 0.7 bar (absolute) to 5 bar (absolute), more preferably in the range from 0.8 bar (absolute) to 4 bar (absolute), more preferably in the range from 0.9 bar (absolute) to 3.5 bar (absolute), even more preferably in the range from 1.0 bar (absolute) to 3 bar (absolute), even more preferably at 1.25 bar (absolute).

[0150] In step (a1) of the process according to the invention, the reaction column RR A At the bottom of A a bottom product stream S containing OCH AP is extracted.

[0151] Preferably, S AP are S AP % by weight, preferably 5 to 35% by weight, more preferably 15 to 35% by weight, and most preferably 20 to 35% by weight, based on the total weight of A OCH3 mass fraction.

[0152] Here, S AP The mass fraction of residual water in AP Preferably, it is less than 1% by weight, preferably less than 0.8% by weight, more preferably less than 0.5% by weight, based on the total mass of the

[0153] Here, S AP reactant M in A The mass fraction of OH is S AP Preferably, it is less than 1% by weight, preferably less than 0.8% by weight, more preferably less than 0.5% by weight, based on the total mass of the

[0154] 4.1.2 Intermediate evaporator, bottom evaporator In a preferred embodiment, the reaction column RR A is especially suitable for intermediate evaporators. ZA and bottom evaporator VSA The reaction column RR includes at least one evaporator selected from the group consisting of: A Particularly preferably, at least one bottom evaporator V SA Includes.

[0155] According to the present invention, the "intermediate evaporator" V Z Above the bottom of each column, especially the reaction column RR A or RR B above the bottom of the ZA " or "V ZB "), or rectification column RD A above the bottom of the ZRD The evaporator located in the RR A or RR B In the case of A or RP B are evaporated and these crude products are discharged from the column as a side stream S ZAA or S ZBA It is extracted as.

[0156] According to the invention, the "bottom evaporator" V S The bottom of each column, especially the reaction column RR A Or RR B or RR as used in preferred embodiments and further described in more detail below. C The bottom of the SA " or "V SA’ " or "V SB " or "V SB’ " or "V SC " or "V SC’ "), or rectification column RD A The bottom of the SRD " or "V SRD’ It is an evaporator that heats the refrigerant (called "RR"). A or RR B In the case of AP or S BP At least a portion of the RR is evaporated. CIn the case of CP is evaporated. RD A In the case of UA Part of S UA1 is evaporated. A or RR B In the case of S AP Each alkali metal methoxide M A OCH3 or S BP M inside B The mass fraction of OCH3 can be adjusted, especially increased. AP M inside A OCH3 or S BP M inside B The desired concentration of OCH3 is adjusted by the reaction of each reactor RR. A or RR B This can also be achieved by controlling the reflux in the reaction column RR. A or RR B Control by reflux in each and each bottom evaporator V SA Or V SA’ or V SB Or V SB’ The combination with control by S AP M inside A OCH3 or S BP M inside B It is particularly advantageous for adjusting the desired concentration of OCH3.

[0157] In another preferred embodiment, S AP M inside A OCH3 or S BP M inside B To adjust the concentration of OCH3, especially to lower it, simply add fresh methanol. AP or S BP It may also be added to.

[0158] In another preferred embodiment, the reaction column RR A At least one bottom evaporator V SA In this case, the bottom evaporator V SA via the bottom product stream SAP is partially introduced into the bottom product stream S AP is partially removed from S AP M inside A The mass fraction of OR increases.

[0159] Here, the bottom product stream S AP M inside A The mass fraction of OCH3 is SA In particular, the bottom product stream S AP M inside A The mass fraction of OCH3 is SA During passage through the above, the content increases in particular by 0.5% to 10%, preferably 1% to 5%, more preferably 2% to 4%, and even more preferably 2.5% to 3.5%.

[0160] The evaporators are usually arranged outside each reaction or rectification column. In the evaporators, energy, in particular heat, is transferred from one stream to another, and therefore they are heat transfer devices WT. The mixture to be evaporated is withdrawn from the column via a draw and fed to at least one evaporator. The reaction column RR A or RR B In the case of A or RP B During intermediate evaporation, this is extracted and fed to at least one intermediate evaporator V ZA or V ZB are supplied to.

[0161] Rectification tower RD A In the case of intermediate evaporation, at least one side stream S ZA But, RD A is extracted ("extracted") from at least one intermediate evaporator V ZRD are supplied to.

[0162] Rectification tower RD A In the case of bottom evaporation, at least one stream S UA But, RDA and at least a portion, preferably a portion, is withdrawn from at least one bottom evaporator V SRD are supplied to.

[0163] Via at least one feed, the evaporated mixture, possibly together with residual liquid fractions, is returned to the respective column. If the evaporator is an intermediate evaporator, i.e., this is in particular the intermediate evaporator V ZA or V ZB or V ZRD In this case, the draw point from which each mixture is drawn and fed to the evaporator is a side draw point, and the inlet through which the evaporated mixture is fed back to each column is a side feed point. If the evaporator is a bottom evaporator, i.e., if the column bottom is heated, this is especially the bottom evaporator V SA or V SB or V SRD When at least a portion of the bottom draw stream, in particular S AP or S BP is fed to the bottom evaporator, evaporated and returned to the respective column in the bottom region. Alternatively, however, for example, on suitable trays when intermediate evaporators are used, or at the bottom of each column, tubes are formed into which a heat transfer medium, for example the respective compressed vapor stream S OA11 Or S OA21 (V S or V Z is the rectification tower RD A It is also possible to flow a heat transfer medium W1 through the column (if present). In this case, evaporation occurs on the trays or at the bottom of the column. However, it is preferable to arrange an evaporator outside each column.

[0164] Suitable evaporators that can be used as intermediate and bottom evaporators include, for example, natural circulation evaporators, forced circulation evaporators, forced circulation flash evaporators, boiler evaporators, falling film evaporators, and thin film evaporators. In natural circulation evaporators and forced circulation evaporators, tube bundle or plate devices are usually used as the heat transfer device of the evaporator. When using a tube bundle or plate evaporator, a heat transfer medium, for example, a rectification column RD, is used. A V inSRD Or V ZRD Compressed vapor flow in S OA11 Or S OA21 , or the heat transfer medium W1 flows through the tubes or plates, and the mixture to be evaporated flows around the tubes or through the heat transfer medium, for example, the rectification column RD A V in SRD Or V ZRD Compressed vapor flow in S OA11 Or S OA21 , or the heat transfer medium W1 flows around the tubes or plates, and the mixture to be evaporated flows through the tubes or plates. Figure 16A shows a specific embodiment of a plate package evaporator that can be used as a suitable evaporator within the scope of the method according to the invention, in particular as an intermediate evaporator and a bottom evaporator.

[0165] In the case of a falling film evaporator, the mixture to be evaporated is usually added as a thin film inside the tubes, which are heated from the outside. In contrast to a falling film evaporator, a thin film evaporator also has a rotor with a wiper, by means of which the liquid to be evaporated is distributed on the inner wall of the tubes in the form of a thin film.

[0166] However, in addition to those mentioned, any other evaporator type known to those skilled in the art that is suitable for use in a rectification column can also be used.

[0167] For example, the compressed steam flow S OA11 Or, if the evaporator operated by the heat medium W1 as heating steam is an intermediate evaporator, the intermediate evaporator AB or steam flow S AB and S BB The region between the feed point of the rectification column RD and above the bottom of the column A It is preferable that the reaction column RR is disposed in the stripping section of the reaction column RR. A or RR B In the case of AE2 or S BE2Preferably, the intermediate evaporator is located below the feed point of the intermediate evaporator and above the bottom of the column. This allows a large portion of the heating energy to be introduced by the intermediate evaporator. Thus, for example, it is possible to introduce more than 80% of the energy by the intermediate evaporator. According to the invention, the intermediate evaporator is preferably arranged and / or configured so as to introduce more than 10%, in particular more than 20%, of the total energy required for the distillation.

[0168] When an intermediate evaporator is used, it is particularly advantageous to arrange the intermediate evaporator so that each rectification column or reaction column has 1 to 50 theoretical plates below the intermediate evaporator and 1 to 200 theoretical plates above the intermediate evaporator. It is particularly preferred that each rectification column or reaction column has 2 to 10 theoretical plates below the intermediate evaporator and 20 to 80 theoretical plates above the intermediate evaporator.

[0169] The mixture from the rectification column or reaction column is transferred to the intermediate evaporator V Z The side draw flow fed to the intermediate evaporator V Z The side feed, through which the evaporated mixture from is fed back into each rectification or reaction column, can be located between the same trays of the column. However, the side draw and the side feed can also be at different heights.

[0170] Such an intermediate evaporator V ZA So, reactor RR A Existing within M A OCH3, water, methanol, M A Liquid crude product RP containing OH A can be at least partially, preferably partially, transferred to the gaseous state, thus improving the efficiency of the conversion according to step (a1) of the process according to the invention.

[0171] Such an intermediate evaporator V ZB So, reactor RR B Existing within M B OCH3, water, methanol, M B Liquid crude product RP containing OH Bcan be at least partially, preferably partially, transferred to the gaseous state, thus improving the efficiency of the conversion according to step (a2) of the process according to the invention.

[0172] Reactor RR A or RR B One or more intermediate evaporators V in the upper region of ZA or V ZB By placing A or RR B The dimensions of the lower region of at least one, preferably several intermediate evaporators V ZA or V ZB In an embodiment having a reaction column RR A or RR B It is also possible to feed a partial stream of methanol in liquid form into the upper region of the column.

[0173] 4.2 Step (a2) (optional) 4.2.1 General description of optional step (a2) Step (a2) represents an optional embodiment of the method according to the invention, which means that step (a2) in the method according to the invention may or may not be performed.

[0174] In optional step (a2), simultaneously with and spatially separated from step (a1), a starting material stream S comprising methanol is BE1 is M B OH-containing starting material stream S BE2 By this, the reactive rectification column RR B Countercurrently converted within the B OCH3, water, methanol, M B Crude product RP containing OH B becomes.

[0175] In optional step (a2) of the method according to the invention, RR B At the bottom of B a bottom product stream S containing OCH BP is extracted. RR BAt the top of the BB is extracted.

[0176] M B is selected from sodium, potassium, and lithium. B is in particular selected from sodium and potassium. B = Potassium.

[0177] Starting material stream S BE1 In a preferred embodiment, S BE1 The mass fraction of methanol in the mixture is 95% by weight or more, and even more preferably 99% by weight or more. BE1 In particular, it comprises water.

[0178] In optional step (a2) of the process according to the invention, the starting material stream S BE1 The methanol used as may be commercially available methanol having a mass fraction of more than 99.8% by weight and a mass fraction of water up to 0.2% by weight.

[0179] Starting material stream S BE1 is preferably added in vapor form.

[0180] Starting material stream S BE2 is M B In a preferred embodiment, S BE2 is M B In addition to OH, it contains at least one further compound selected from water, methanol. Even more preferably, S BE2 is M B In addition to OH, it also contains water, in this case S BE2 is M B It is an aqueous solution of OH.

[0181] Starting material stream S BE2 M B If OH and water are included, S BE2 M based on the total weight of the aqueous solution forming BThe mass fraction of OH is in particular in the range of 10 to 75% by weight, preferably 15 to 54% by weight, more preferably 30 to 53% by weight, and particularly preferably 40 to 52% by weight.

[0182] Starting material stream S BE2 M B When OH and methanol are included, S BE2 M in methanol based on the total weight of the solution forming B The mass fraction of OH is in particular in the range of 10 to 75% by weight, preferably 15 to 54% by weight, more preferably 30 to 53% by weight, and particularly preferably 40 to 52% by weight.

[0183] Starting material stream S BE2 M B In certain cases containing both water and methanol in addition to OH, S BE2 M in methanol and water based on the total weight of the solution forming B It is particularly preferred that the mass fraction of OH is in the range of 10 to 75% by weight, preferably 15 to 54% by weight, more preferably 30 to 53% by weight, and particularly preferably 40 to 52% by weight.

[0184] Optional step (a2) of the process according to the invention is the rectification of a reactive rectifier (or "reaction column") RR B The reaction is carried out in the reactor RR. B A preferred embodiment of is described in Section 4.1.1.

[0185] According to the present invention, a "methanol-containing starting material stream S BE1 , M B OH-containing starting material stream S BE2 By In countercurrent "Converting" refers in particular to the reaction column RR B In the optional step (a2), the methanol-containing starting material stream S BE1 At least some of the supply points of M B OH-containing starting material stream S BE2 This is ensured by being below the supply point of

[0186] Reactor RRB is preferably the starting material stream S BE1 The feed point and the starting material flow S BE2 Between the feed point and the reactor, there are at least two, in particular 15 to 40 theoretical plates.

[0187] Reactor RR B can be operated as a pure stripping column. B In the lower region of the BE1 is supplied in vapor form.

[0188] Optional step (a2) comprises the step of: BE1 Part of M B OH-containing starting material stream S BE2 Although the feed point of the reactor RR is below the feed point of the reactor RR, B This also includes the case where the gas is added in vapor form to the top or top region of the reactor RR. B The size of the lower region of the starting material stream S containing methanol can be reduced. BE1 Part of the reaction column RR B When the methanol is fed to the top or top region of the reaction column RR, only a fraction of 10 to 70 wt. %, preferably 30 to 50 wt. % (each based on the total amount of methanol used in step (a2)) is fed to the top or top region of the reaction column RR. B The remaining part is fed in a single stream or distributed into several part streams to the bottom end of the sieve, preferably on 1 to 10 theoretical plates, particularly preferably on 1 to 3 theoretical plates, M B OH-containing starting material stream S BE2 It is added in vapor form below the feed point of

[0189] Reactor RR B Then, a starting material stream S containing methanol is BE1 However, the reaction described earlier <1> According to M B OH-containing starting material stream S BE2 is converted by M B OCH3 and HO, and since this is an equilibrium reaction, these products are the same as the reactants methanol and M BOH. Therefore, in optional step (a2) of the process according to the invention, the reaction column RR B Crude product RP B This crude product RP B is the product M B In addition to OCH3 and water, methanol and M B Includes OH.

[0190] RR B At the lower end of B a bottom product stream S containing OCH BP is obtained and then extracted.

[0191] RR B The upper end of the B At the top of the column, a vapor stream S containing water and methanol is generated. BB A methanol stream, still containing water, called "methanol stream" is withdrawn.

[0192] This vapor stream S containing water and methanol BB In step (a3), at least part of the rectification column RD A where the RD A A methanol-containing vapor stream S is withdrawn at the top of OA and R.D. A At least one stream S containing water to be extracted at the lower end of UA During the distillation in step (a3), the stream S OA A part of the methanol obtained in the reactor RR B Starting material stream S BE1 It can be supplied as

[0193] Here, if step (a2) is carried out, then in step (a3) ​​of the method according to the invention, the vapor stream S BB At least part of the AB with or without mixing with (i.e., in this case, S AB (separated from the rectification column RD) APreferably, in step (a3) ​​of the process according to the invention, the vapor stream S BB and S AB are mixed, and the mixture is then passed through a rectification column RD A is led to.

[0194] Starting material stream S BE1 The amount of methanol contained in the bottom product stream S BP Alkali metal methoxide M obtained in B Preferably, the starting material stream S BE1 The amount of methanol in the reaction column is determined by the amount of methanol and M B a bottom product stream S containing OCH BP The concentration of the alkali metal methoxide solution is selected to be the desired concentration.

[0195] In a preferred embodiment of the method according to the invention, in particular S BE2 M B In optional step (a2), the starting material stream S BE1 The total weight (mass; unit: kg) of methanol used as starting material stream S in optional step (a2) BE2 Used as M B The ratio of the total weight (mass; unit: kg) of OH to the total weight (mass; unit: kg) of OH is 4:1 to 50:1, more preferably 8:1 to 48:1, even more preferably 10:1 to 45:1, even more preferably 20:1 to 40:1, and most preferably 22:1.

[0196] Reactor RR B may be operated with or without reflux, preferably with reflux.

[0197] Reactor RR B In the embodiment where reflux is generated in optional step (a2), starting material stream S BE2 Used as M BOH can also be at least partially mixed with the reflux stream and the resulting mixture can then be fed to optional step (a2).

[0198] The optional step (a2) is especially carried out at a temperature in the range from 45°C to 150°C, preferably in the range from 47°C to 120°C, more preferably in the range from 60°C to 110°C, and at a pressure in the range from 0.5 bar (absolute) to 40 bar (absolute), preferably in the range from 0.7 bar (absolute) to 5 bar (absolute), more preferably in the range from 0.8 bar (absolute) to 4 bar (absolute), more preferably in the range from 0.9 bar (absolute) to 3.5 bar (absolute), even more preferably in the range from 1.0 bar (absolute) to 3 bar (absolute) and most preferably at 1.25 bar (absolute).

[0199] In step (a2) of the process according to the invention, the reaction column RR B At the bottom of B a bottom product stream S containing OCH BP is extracted.

[0200] Preferably, S BP are S BP % by weight, preferably 5 to 35% by weight, more preferably 15 to 35% by weight, and most preferably 20 to 35% by weight, based on the total weight of B OCH3 mass fraction.

[0201] Here, S BP The mass fraction of residual water in BP Preferably, it is less than 1% by weight, preferably less than 0.8% by weight, more preferably less than 0.5% by weight, based on the total mass of the

[0202] Here, S BP reactant M in B The mass fraction of OH is S BP Preferably, it is less than 1% by weight, preferably less than 0.8% by weight, more preferably less than 0.5% by weight, based on the total mass of the

[0203] 4.2.2 Intermediate evaporator, bottom evaporator In a preferred embodiment, the reaction column RR B is especially suitable for intermediate evaporators. ZB and bottom evaporator V SB The reaction column RR includes at least one evaporator selected from the group consisting of: B Particularly preferably, at least one bottom evaporator V SB This bottom evaporator V SB In particular, the bottom product stream S BP is partially introduced into the bottom product stream S BP is partially removed from S BP M inside B The mass fraction of OR increases.

[0204] Here, the bottom product stream S BP M inside B The mass fraction of OCH3 is SB In particular, the bottom product stream S BP M inside B The mass fraction of OCH3 is SB During passage through the above, the content increases in particular by 0.5% to 10%, preferably 1% to 5%, more preferably 2% to 4%, and even more preferably 2.5% to 3.5%.

[0205] 4.2.3 Separating Wall Tower (TRD) Step (a2) of the process according to the invention, in the embodiment of the invention in which it is carried out, is carried out simultaneously with and spatially separated from step (a1). The spatial separation means that steps (a1) and (a2) are carried out in both reaction columns RR A and R.R. B This can be ensured by implementing it internally.

[0206] In an advantageous embodiment of the invention, the reaction column RR A and R.R. BThe column is housed in a column shell, and the column is at least partially divided by at least one dividing wall. Such a column having at least one dividing wall is referred to as a "TRD." Such dividing wall columns are known to those skilled in the art and are described, for example, in U.S. Pat. No. 2,295,256, EP 0122367, EP 0126288, WO 2010 / 097318, WO 2021 / 148174, WO 2021 / 148175, and I. Dejanovic, Lj. Matijasevic, Z. Olujic, Chemical Engineering and Processing 2010, 49, 559-580.

[0207] CN Patent Publication No. 105218315 also describes a dividing wall column used in the rectification of methanol.

[0208] In the dividing wall column of the present invention, the dividing walls preferably extend to the trays and extend over at least one-quarter, more preferably at least one-third, even more preferably at least one-half, even more preferably at least two-thirds, and even more preferably at least three-quarters of the column's length. They separate the column into at least two reaction spaces in which spatially separated reactions can occur. The reaction spaces created by the at least one dividing wall may be of the same size or different sizes.

[0209] In this embodiment, the bottom product stream S AP and S BP can be withdrawn separately, preferably by means of a bottom evaporator V mounted for each reaction space formed by at least one reaction wall. SA or V SB Methanol can be introduced via S AP or S BP can be at least partially removed from

[0210] Therefore, in a preferred embodiment of the process according to the invention, the rectification column RD A , reaction tower RR A and reaction column RR if step (a2) is carried out. B At least two, and even more preferably exactly two, of the columns selected from are housed within the column shell, the columns being at least partially separated from each other by a separation wall extending to the column trays.

[0211] In the process according to the invention, the reaction column RR A (or in the embodiment in which step (a2) is performed, reaction column RR A and reactor RR B ) and rectification column RD A In the complex with the rectification tower RD A are preferably operated at pressures selected to provide a low pressure gradient between the columns.

[0212] As previously described, in an advantageous embodiment of the invention, the rectification column RD A , reaction tower RR A and reaction column RR if step (a2) is carried out. B In the above-mentioned preferred embodiment in which step (a2) is carried out and the process according to the invention is carried out in a TRD, at least two columns selected from the group consisting of: A and R.R. B and rectification tower RD A The reaction zones corresponding to are separated from each other in the column shell by two separating walls, which extend up to the trays of the column.

[0213] In this preferred embodiment, in particular in a portion of the TRD, the crude product RP according to step (a1) A or the crude product RP from steps (a1) and (a2) A and R.P. B The reaction is carried out with the starting material stream SAE2 and optionally starting material stream S BE2 is added below but approximately at the height of the upper end of the separating wall, and the starting material stream S AE1 and optionally starting material stream S BE1 is added in vapor form at the bottom end. The methanol / water mixture formed above the feed point of the starting material stream then passes above the dividing wall into the rectification column RD A The second or third lower part of the column separated by a dividing wall is distributed throughout the column section that serves as the rectifying section of the rectifying column RD. A The energy required for distillation is then supplied via an evaporator at the bottom end of the second part of the column separated by a dividing wall, which may be conventionally heated or may be supplied by a compressed vapor stream S OA2 If the evaporator is conventionally heated, the compressed vapor stream S OA11 An intermediate evaporator heated by a portion of the

[0214] 4.2.4 Fresh Methanol In the process according to the invention, methanol is consumed and therefore needs to be replaced with fresh methanol, especially when the process is carried out continuously.

[0215] Here, the fresh methanol supply is in particular a methanol-containing starting material stream S AE1 As the reactor RR A In the embodiment in which step (a2) is carried out directly in the reactor RR A and R.R. B will be held.

[0216] During the distillation in step (a3), the flow S OA A part of the methanol obtained in the reactor RR A Starting material stream S AE1 and if step (a2) is carried out, alternatively or additionally, in step (a2) the reaction column RR B Starting material stream S BE1In an embodiment, fresh methanol is supplied to rectification column RD A In embodiments △, ●, ◇ (described in Section 4.10), fresh methanol is added to rectification column RD A It is equally preferable to add

[0217] Fresh methanol is fed to the rectification column RD A When added to the rectification column RD, it is preferably A or fed to the rectifying section of the rectifying column RD A The optimum feed point depends on the water content of the fresh methanol used, on the one hand, and on the other hand, on the vapor stream S OA The higher the water content in the methanol used, and the higher the desired residual water content in the vapor stream S OA The higher the purity requirement in the rectification column RD A It is more convenient to feed the rectification column RD to several theoretical plates below the top of the rectification column. A It is preferable to place it below the head.

[0218] Fresh methanol is fed to the rectification column RD A When added to the rectification column RD, it is added at a temperature up to the boiling point, preferably at room temperature. A In this case, a dedicated feed for fresh methanol may be provided or fresh methanol may be added at the top of the rectification column RD A After condensing and returning a portion of the methanol extracted at the top of the column, it is mixed with this methanol and A In this case, fresh methanol can be fed into the vapor stream S OA It is particularly preferred that the methanol condensed from the condensate be added to a condensate container where it is collected (described in more detail in Section 4.9.5).

[0219] 4.3 Process (a3) In step (a3) ​​of the process according to the invention, a vapor stream S ABand at least a portion of the vapor stream S if step (a2) is performed. BB At least part of AB Mixed with or S AB Separated from the rectification column RD A Guided by RD A Within, RD A At least one vapor stream S containing methanol is withdrawn at the top end of OA and R.D. A At least one stream S containing water to be extracted at the lower end of UA and are separated into

[0220] In embodiments of the invention in which step (a2) is performed, step (a3) ​​comprises the step of adding a vapor stream S AB and at least a portion of the vapor stream S BB and then mixed with at least a portion of the A However, alternatively, S AB and S BB at two different feed points to the rectification column RD A It can also lead to.

[0221] In step (a3) ​​of the process according to the invention, a vapor stream S AB and at least a portion of the vapor stream S if step (a2) is performed. BB At least part of AB Mixed with or S AB Separated from the rectification column RD A Guided by RD A Within, RD A At least one vapor stream S containing methanol is withdrawn at the top end of OA and R.D. A At least one stream S containing water to be extracted at the lower end of UA and are separated into

[0222] "RD A At least one vapor stream S containing methanol is withdrawn at the top end of OA " is RD AThis means that the steam obtained at the top of the steam generator may be withdrawn there as one or more steam streams. If this steam stream is withdrawn there as more than one steam stream, the m steam streams are referred to as "steam stream S OAI ", "Vapor flow S OAII ", [...], "Steam flow S OAm " and "m" stands for RD A Indicates the number of steam streams (Roman numerals) extracted at the top of the

[0223] "RD A At least one stream S containing water to be extracted at the lower end of UA " is RD A This means that the water available at the lower end of the pipe may be withdrawn there as more than one stream. If this water is withdrawn as more than one stream, the n streams are referred to as "stream S" UAI ", "Flow S UAII ", [...], "Flow S UAn " and "n" stands for RD A The bottom end indicates the number of flows (Roman numerals) to be extracted.

[0224] Here, the steam flow S AB and at least a portion of the vapor stream S if step (a2) is performed. BB at least a portion of which is fed to rectification column RD via one or more feed points A These vapor streams can be, for example, those in which step (a2) is carried out in the method according to a preferred embodiment of the present invention and in which step (a3) ​​a vapor stream S BB At least part of AB In this embodiment, the steam flow S is introduced through multiple feed points. AB and at least a portion of the vapor stream S BB at least a portion of which is passed through rectification column RD as two separate streams. A is led to.

[0225] Steam flow S AB and at least a portion of the vapor stream S if step (a2) is performed. BBat least a portion of which is separated into two or more streams from the rectification column RD A In the embodiment of the present invention where the feed points of the individual streams are directed to the rectification column RD A Advantageously, the electrodes are at substantially the same height.

[0226] In a preferred embodiment of step (a3) ​​of the process according to the invention, the vapor stream S AB and at least a portion of the vapor stream S if step (a2) is performed. BB At least a portion of the A Within, RD A A methanol-containing vapor stream S is withdrawn at the top of OA and R.D. A The flow S containing the water extracted at the bottom UA and are separated into

[0227] Another name for the "top" of a rectification column is the "head."

[0228] Another term for the "lower end" of a rectification column is the "bottom" or "foot."

[0229] At least one steam flow S OA The pressure that OA " and its temperature is called "T OA This is particularly true when this vapor stream is fed to the rectification column RD in step (a3). A At least one vapor stream S when withdrawn from OA is related to the pressure and temperature.

[0230] Pressure p OA is in particular in the range of 0.5 bar (absolute) to 8 bar (absolute), more preferably in the range of 0.6 bar (absolute) to 7 bar (absolute), more preferably in the range of 0.7 bar (absolute) to 6 bar (absolute), even more preferably in the range of 1 bar (absolute) to 5 bar (absolute), even more preferably in the range of 1 bar (absolute) to 4 bar (absolute), even more preferably in the range of 1.0 to 2.0 bar (absolute), and most preferably 1.1 bar (absolute).

[0231] temperature T OA is particularly in the range of 45°C to 150°C, more preferably in the range of 48°C to 140°C, more preferably in the range of 50°C to 130°C, even more preferably in the range of 60°C to 120°C, even more preferably in the range of 60°C to 110°C, even more preferably in the range of 65°C to 80°C, and most preferably 67°C.

[0232] The rectification column RD in step (a3) ​​of this method A Any rectification column known to those skilled in the art can be used as the rectification column RD. Preferably, the rectification column RD A includes internals. Suitable internals are, for example, trays, non-structured packing, or structured packing. As trays, bubble cap trays, sieve trays, valve trays, tunnel cap trays, or slotted trays are typically used. Non-structured packing is generally random packing. As packing, Raschig rings, Pall rings, Burl saddles, or Intalox® saddles are typically used. Structured packing is, for example, sold under the trade name Mellapack® by Sulzer. In addition to the internals listed, further suitable internals are known to those skilled in the art and can be used as well.

[0233] Preferred internal structures have a low specific pressure drop per theoretical stage. Structured packings and packings, for example, have a significantly lower pressure drop per theoretical stage than trays. This includes rectification columns, RD A The advantage is that the pressure drop in the compressor remains as low as possible and therefore the mechanical power of the compressor and the temperature of the methanol / water mixture to be evaporated remain low.

[0234] Rectification tower RD A If structured or unstructured packing is included within the scalar, these packings may be separated or there may be consecutive packings. However, there are usually at least two packings: 1) It is preferable if: - If step (a2) is not performed: one packing is S AB above the supply point of; - Step (a2) is performed, and S AB and S BB are mixed and then A If you are guided to: 1 packing S AB and S BB above the feed point of the mixture with; - Step (a2) is performed, and S AB and S BB is separated and A If you are guided to: 1 packing S AB and S BB above the supply point. 2) Additionally, it is preferable if: - If step (a2) is not performed: one packing is S AB below the supply point of; - Step (a2) is performed, and S AB and S BB are mixed and then A If you are guided to: 1 packing S AB and S BB and below the feed point of the mixture; - Step (a2) is performed, and S AB and S BB is separated and A If you are guided to: 1 packing S AB and S BB below the supply point of

[0235] One packing is S AB or S AB and S BB and a plurality of trays are provided above the supply point of S AB or S AB and S BBIt is also possible for the packing to be located below the feed point of the separator. When non-structured packing, such as packed packing, is used, the packing is typically on a suitable support grid (such as a sieve tray or grid tray).

[0236] In each embodiment, S AB or S AB and S BB The supply point of Tower RD A Preferably, the lower half of S AB or S AB and S BB Tower RD A The mixture is fed to the lower half, preferably the lower third, and more preferably the lower quarter of the mixture.

[0237] Then, in step (a3) ​​of the process according to the invention, at least one vapor stream S comprising methanol is OA However, the rectification tower RD A This steam flow S OA The preferred mass fraction of methanol therein is 99% by weight or more, more preferably 99.6% by weight or more, even more preferably 99.9% by weight or more, the remainder being in particular water.

[0238] RD A at least one water-containing stream S, which may have preferably less than 1 wt. % methanol, more preferably not more than 5000 ppm by weight, and even more preferably not more than 2000 ppm by weight UA is extracted.

[0239] In the context of the present invention, the rectification column RD A At the top of the OA In particular, the extraction of at least one steam flow S OA as a head stream or as a side draw from rectification column RD A This means that the device is extracted above the internal structure.

[0240] In the context of the present invention, the rectification column RD AAt least one stream S containing water at the bottom of UA In particular, the extraction of at least one flow S UA as a bottom stream or fractionator RD A This means that the item will be removed from the bottom tray.

[0241] Rectification tower RD A may be operated with or without reflux, preferably with reflux.

[0242] "With reflux" means that the rectification column RD A The steam flow S extracted at the top of OA However, instead of being completely discharged, it is partially condensed and discharged into each rectification column RD A Here, when such a reflux is generated, the reflux ratio is preferably 0.0001 to 10, more preferably 0.1 to 5, even more preferably 0.5 to 2, even more preferably 0.7 to 1, and even more preferably 0.76.

[0243] Reflux is the rectification column RD A Condenser K at the head of RD It can be generated by installing a condenser K RD Within, the steam flow S OA is partially condensed and A is supplied again.

[0244] 4.4 Process (b) In step (b) of the process according to the invention, at least one vapor stream S OA At least a portion of ("at least one vapor stream S OA At least part of" = "S OA At least one vapor stream S compressed in step (b) is OA This part of "S OA◆ ". As a result, S OA Compared to the compressed vapor flow S OA1 is obtained.

[0245] Steam flow SOA1 The pressure that OA1 " and its temperature is called "T OA1 "It is called "

[0246] Pressure p OA1 is p OA Higher than. p OA1 The exact value of p OA1 >p OA As long as the above condition is met, a person skilled in the art can adjust it according to the requirements of step (d). OA1 / p OA (where each pressure is in bar (absolute pressure)) is preferably in the range of 1.1 to 10, more preferably 1.2 to 8, more preferably 1.25 to 7, and most preferably 1.3 to 6.

[0247] temperature T OA1 is especially at temperature T OA Higher than T OA1 / T OA (where temperatures are in °C) is preferably in the range of 1.03 to 10, more preferably 1.04 to 9, more preferably 1.05 to 8, more preferably 1.06 to 7, more preferably 1.07 to 6, and most preferably 1.08 to 5.

[0248] p OA1 and T OA1 The preferred value of is preferably S OA11 and S OA12 Also applies to.

[0249] The vapor stream S in step (b) OA At least part of S OA◆ The compression of can be carried out in any arbitrary manner known to those skilled in the art. Thus, the compression can be carried out, for example, mechanically, in a single stage or in multiple stages, preferably in multiple stages. In the case of multiple stage compression, several compressors of the same type or compressors of different types can be used. Multistage compression can be carried out using one or more compressors. The use of single stage or multistage compression depends on the compression ratio and therefore on the vapor flow S. OA At least part of S OA◆It depends on how much pressure it is desired to compress.

[0250] In the process according to the invention, in particular in step (b), the vapor stream S OA At least part of S OA◆ Compress it to S OA1 or in step (e) S OA12 Compress it to S OA2 The compressor for this purpose is any compressor known to those skilled in the art, preferably a mechanical compressor capable of compressing a gas flow, such as a single-stage or multi-stage turbine, a piston compressor, a screw compressor, a centrifugal compressor or an axial compressor.

[0251] In the case of multistage compression, a compressor appropriate for each pressure stage to be overcome is used.

[0252] In certain embodiments of step (b), stream S OA This is the rectification tower RD A and optionally at the top of the rectification column RD A The reflux to S OA After being separated from the first compressor VD AB2 and then the precompressed flow S OA At least part of S OA◆ is fed to step (b) and compressed by compressor VD1 to produce S OA1 becomes.

[0253] Here, if the embodiment Δ is also implemented, preferably S OA◆ The part S that is different from OA△ The pre-compressed flow S OA and even more preferably at least one further compressor VD △ is compressed by

[0254] Alternatively or additionally, in this preferred embodiment of step (b), rectification column RD A connected downstream of S OAis pre-compressed, compressor VD AB2 Instead of rectification column RD A Compressor VD connected upstream of AB1 This compressor can also be used with VD AB1 By S AB ,S BB or S AB and S BB The mixture of each flow is A It is compressed before being introduced into the

[0255] Steam flow S OA If S is subjected to several compression stages, according to the invention, it is only in the last compression stage that S OA Flow S OA1 is formed, and then S OA1 is the stream S used in step (d) according to the invention OA11 Then, in step (e), it is further compressed to S OA2 The flow S OA12 and S OA Compress it to S OA1 This compression is performed by compressor VD1 (shown in the figure) in the example. <401> The procedure is carried out by the

[0256] 4.5 Process (c) In step (c) of the method according to the invention, at least one side stream S ZA But, RD A Extracted from RD A will be sent back again.

[0257] In a preferred embodiment of step (c) of the method according to the invention, the side stream S ZA But, RD A Extracted from RD A will be sent back again.

[0258] According to the present invention, "RD A Side flow from S ZA "The flow is RD A Extraction point E below the head and above the bottom ZA In particular, RD AThe supply point Z is below the head and above the bottom. ZA (This means that each side stream S ZA is the rectification tower RD A (which is the point where the sample is sent back to the RD) A This means that the item will be sent back to the original address.

[0259] This is especially true for the rectification column RD A Each side flow S ZA Sampling point E ZA and preferably a supply point Z ZA Also, RD A All steam flows S extracted from OA Sampling point E OA and preferably at least one, even more preferably at least five, even more preferably at least ten theoretical plates are below the sampling point E OA is the rectification tower RD A The furthest down in RD A Steam flow S extracted from OA Sampling point E OA This means that it is below the

[0260] Furthermore, this is particularly true for the rectification column RD A Each side flow S ZA Sampling point E ZA and preferably a supply point Z ZA Also, RD A All flows S extracted from UA Sampling point E UA and preferably at least one, even more preferably at least two, even more preferably at least four theoretical plates are located above the sampling point E UA is the rectification tower RD A The flow S is furthest above UA Sampling point E UA This means that it is above the

[0261] Additionally, at least one vapor stream S OA is at least partially contained in the rectification column RD A (This is, for example, when the reflux is A), in particular, at least one steam stream S OA Supply point Z OA (This means that at least one vapor stream S OA is at least partially contained in the rectification column RD A The point at which the sample is returned to the supplier is the sampling point E ZA Above, especially, RD A All side streams S extracted from ZA Supply point Z ZA and preferably at least 1, even more preferably at least 5, even more preferably at least 10 theoretical plates are above the RD A All side streams S extracted from ZA above the highest point of all the extraction and feeding points.

[0262] Additionally, at least one flow S UA is at least partially contained in the rectification column RD A In particular, at least one flow S UA Supply point Z UA (This means that at least one flow S UA is at least partially contained in the rectification column RD A The point at which the sample is returned to the supplier is the sampling point E ZA Below, especially, RD A All side streams S extracted from ZA Supply point Z ZA and preferably at least one, even more preferably at least two, even more preferably at least four theoretical plates are below the RD A All side streams S extracted from ZA below the lowest point of all the sampling and feeding points.

[0263] Rectification tower RD A Side flow S ZA Sampling point E ZA and side flow S ZA Supply point Z ZA RD A However, it is also possible that they are at different heights.

[0264] In a preferred embodiment of the process according to the invention, the rectification column RD A At least one side stream S in ZA Sampling point E ZA and preferably a supply point Z ZA Also, RD A Supply point Z SAB and above the bottom of the rectification column RD. A At least one side stream S in ZA Sampling point E ZA and preferably a supply point Z ZA Also, RD A It is located below the enrichment section.

[0265] Supply point Z SAB RD A Inside S AB All supply points of RD A Inside S BB All supply points of RD A Inside S AB and S BB represents the lowest feed point of all feed points of the mixture.

[0266] In a particularly preferred embodiment of the process according to the invention, the rectification column RD A At least one side stream S in ZA Sampling point E ZA and more preferably supply point Z ZA Also, supply point Z SAB Below and RD A All flows S extracted from UA the rectification column RD above the highest of the withdrawal and feed points of A Preferably, the area is in the upper 4 / 5, preferably the upper 3 / 4, preferably the upper 7 / 10, more preferably the upper 2 / 3, more preferably the upper 1 / 2 of the area.

[0267] In this case, even more preferably, the rectification column RD A At least one side stream S in ZA Sampling point E ZA and preferably a supply point Z ZA Also, RD AIt is located below the enrichment section.

[0268] In a further particularly preferred embodiment of the process according to the invention, the rectification column RD A includes the rectifying section, and the rectifying column RD A At least one side stream S in ZA Sampling point E ZA and more preferably supply point Z ZA Also, below the enrichment section and RD A All flows S extracted from UA the rectification column RD above the highest of the withdrawal and feed points of A Preferably, the area is in the upper 4 / 5, preferably the upper 3 / 4, preferably the upper 7 / 10, more preferably the upper 2 / 3, more preferably the upper 1 / 2 of the area.

[0269] 4.6 Process (d) In step (d) of the process according to the invention, energy is transferred to a compressed vapor stream S OA1 The first part S OA11 From S ZA and then S ZA RD A will be returned to.

[0270] S OA1 In particular, in step (d), first, at least two portions S OA11 and S OA12 It is divided into S OA11 and S OA12 The mass flow ratio (kg / h) of the catalyst to the catalyst is preferably in the range of 1:99 to 99:1, more preferably in the range of 1:50 to 50:1, even more preferably in the range of 1:20 to 30:1, and even more preferably in the range of 5:20 to 15:1.

[0271] In step (d) of the method according to the invention, the energy is transferred to a first portion S OA11 From S ZA By step (d), S OA11 The energy of the flow S decreases, and therefore OA11 is at least partially condensed.

[0272] According to the invention, "transfer of energy" means in particular "heating", i.e. the transfer of energy in the form of heat.

[0273] "Compressed steam flow S OA1 The first part S OA11 From S ZA "Transfer of energy to" is S OA11 and S OA12 Different from S OA1 This also includes cases where a further part of S is separated. OA11 and S OA12 The steam flow S is different from OA1 Part of ("S OA● ") is called S OA1 is separated from the OA● In step (a1), the starting material stream S AE1 and if step (a2) is carried out, alternatively or additionally in step (a2) the starting material stream S BE1 This is applicable in the embodiments of the present invention where the term is used as a

[0274] S OA11 From S ZA Transfer of energy to, preferably S OA11 by S ZA The heating is preferably carried out directly or indirectly.

[0275] "Direct" means that both flows are not mixed. OA11 S ZA and thus energy, especially heat, is released into the OA11 From S ZA This means to transmit to

[0276] This is S OA11 and S ZA However, the rectification tower RD A In the intermediate evaporator V ZRD Guided through S OA11 S ZA This can be done by heating.

[0277] Heat transfer devices (another term for "heat transfer device" = "heat exchanger") include, in particular, the heat transfer device WT listed below. X ,WT Y ,WT Z In step (d) of the process according to the invention, in particular, a heat transfer device, such as a evaporator, which is customary to those skilled in the art, can be used. OA11 From S ZA The transfer of energy, or more preferably heat, to the intermediate evaporator V ZRD It is carried out internally.

[0278] "Indirectly" means, in particular, OA11 a heat transfer medium W1 and preferably at least one heat transfer device WT X The heat transfer medium is contacted through S ZA Instead, W1 is S ZA Therefore, energy, preferably heat, flows through the S without mixing of both flows. OA11 Heat is then transferred from W1 to S ZA By contacting with W1 to S ZA and S ZA and W1 are mixed or not mixed, preferably not mixed. Here, W1 and S ZA If not mixed, the transfer of energy, preferably heat, is carried out in particular by a further heat transfer device WT Y It is carried out internally.

[0279] In a further embodiment of the method according to the invention, S OA11 From S ZA Indirect energy transfer to, especially S OA11 by S ZA In the case of heating, first, energy, preferably heat, is introduced into the OA11 to W1, preferably at least one heat exchanger WT X can be transmitted by contact through W1 to S ZA and a further heat transfer medium W2 different from the at least one heat exchanger WT Y Then, in the final step, W2 is transferred to S ZAHeat is transferred to S ZA and W2 may be mixed or not mixed, preferably not mixed. Here, W2 and S ZA If not mixed, the transfer of energy, preferably heat, is carried out in particular by a further heat transfer device WT Z It is carried out internally.

[0280] It will therefore be appreciated that further embodiments of the present invention may utilize further heat transfer media W3, W4, W5 etc.

[0281] The heat transfer medium W1 or the additional heat transfer mediums W2, W3, W4, and W5 can be any heat transfer medium known to those skilled in the art, preferably selected from the group consisting of air, water, alcohol-water solutions, and salt-water solutions, including ionic liquids such as LiBr solutions, dialkylimidazolium salts, particularly dialkylimidazolium dialkylphosphates, mineral oils such as diesel oil, heat transfer oils such as silicone oils, organic oils such as limonene, and aromatic hydrocarbons such as dibenzyltoluene. Most preferably, the heat transfer medium W1 is water or air, and even more preferably water.

[0282] Usable salt-water solutions are also described, for example, in DE 102005028451 A1 and WO 2006 / 134015.

[0283] Following step (d), S OA11 optionally with fresh methanol and / or in the rectification column RD A together with the reflux of the rectification column RD A In a preferred embodiment, the OA11 From, especially S ZA After the transfer of energy to the

[0284] In a preferred embodiment of the method according to the invention, S OA11 Energy, preferably heat, from S OA11The energy of S ZA After transmitting to S OA To, especially S OA This S OA A portion of S is fed to the compression, preferably to the compression of step (b), which may be carried out in multiple stages. OA Pre-compression or S OA S OA1 This may be the final compression to flow S OA Tower RD A This is the first compression applied after exiting from S OA To heat the OA11 It is possible to use some of the residual energy or heat in the process that is still stored by S OA Any liquid droplets present therein will evaporate, thereby preventing their introduction into the compressor, thereby increasing its lifespan.

[0285] S OA11 Other preferred further reductions in energy, preferably heat, in are described further below.

[0286] Step (d) of the method of the present invention reflects an aspect of the unexpected effect of the present invention. Here, the vapor stream S OA The compressed steam flow S OA1 The excess energy gained in the process is used in rectification rather than being wasted. OA S OA1 This results in a compression of S OA11 From S ZA This allows for adjustment to a value that is optimal for energy transfer to S OA11 The part S that is different from OA12 is further compressed to S OA2 This is done so that it can become. OA12 Further compress and further S OA2The heat of condensation obtained in the process is fed to the bottom evaporator column. The additional compressor power required is less than the heating steam power saved thereby. The process according to the present invention requires less energy than the prior art shown in Examples 1 and 2. OA2 By compressing it to S OA2 From S UA1 or S UA To ensure optimal energy transfer to the OA2 The pressure and temperature can be adjusted.

[0287] 4.7 Process (e) In step (e) of the method of the present invention, S OA11 The compressed vapor flow S OA1 Part of S OA12 is further compressed, thereby OA11 Compared to the compressed vapor flow S OA2 is obtained.

[0288] Although it is self-evident, S OA2 After step (e) is performed, S OA12 and S OA1 It is compressed compared to

[0289] Steam flow S OA2 The pressure with p OA2 " and its temperature is called "T OA2 "It is called "

[0290] Pressure p OA2 is p OA1 higher than p OA2 / p OA1 (where each pressure is in bar (absolute pressure)) is preferably in the range of 1.1 to 10, more preferably 1.2 to 8, more preferably 1.25 to 7, and most preferably 1.3 to 6.

[0291] temperature T OA2 is especially at temperature T OA1 Higher than T OA2 / T OA1(where temperatures are in °C) is preferably in the range of 1.03 to 10, more preferably 1.04 to 9, more preferably 1.05 to 8, more preferably 1.06 to 7, more preferably 1.07 to 6, and most preferably 1.08 to 5.

[0292] S in step (e) OA12 The compression of the vapor S can be carried out by methods familiar to those skilled in the art. Thus, the compression can be carried out, for example, mechanically, in a single stage or in multiple stages, preferably in multiple stages. In the case of multiple stage compression, several compressors of the same type or compressors of different types can be used. The use of single stage or multiple stage compression is advantageous in that the vapor S OA12 It depends on how much pressure you want to compress S OA The pre-compression described in the context of step (b) is OA12 S OA2 In particular, step (e) can be carried out in one stage, i.e. in particular in a compressor VD X Compression using is sufficient.

[0293] 4.8 Process (f) In step (f) of the process according to the invention, energy, preferably heat, is added to the reaction mixture by the addition of S OA2 At least part of S OA21 At least one flow S UA At least part of S UA1 and then S UA1 RD A will be returned to.

[0294] Preferably, in step (f) of the process according to the invention, the energy, preferably heat, is OA2 At least part of S OA21 At least one flow S UA Part of S UA1 and then S UA1 RD A will be returned to.

[0295] By step (f), S OA2At least part of S OA21 The energy of the flow S decreases, and therefore OA21 is at least partially condensed.

[0296] Step (f) of the method according to the present invention comprises the following preferred embodiments (f1), (f2), (f3): (f1) Energy is S OA2 At least part of S OA21 At least one flow S UA Part of S UA1 and then S UA1 RD A be returned to; (f2) Energy is S OA2 At least part of S OA21 At least one flow S UA Part of S UA1* and then S UA1* From some S UA1 RD A be returned to; (f3) Energy is S OA2 At least part of S OA21 Flow S UA The flow is then transmitted to the entire UA Whole or flow S UA Part of S UA1 Only, preferably flow S UA Part of S UA1 Only, RD A will be returned to.

[0297] S OA2 At least part of S OA21 At least one flow S UA At least part of S UA1 Transfer of energy to, preferably, S OA2 At least part of S OA21 At least one flow S UA At least part of S UA1 The heating is preferably carried out directly or indirectly.

[0298] "Direct" means that the two flows do not mix, and OA2 At least part of S OA21 There is at least one flow S UA At least part of S UA1 and so that energy, in particular heat, is transferred at least in part to S OA2 At least one flow S UA At least part of S UA1 This means to transmit to

[0299] This is S OA2 At least part of S OA21 and at least one flow S UA At least part of S UA1 However, the rectification tower RD A In the bottom evaporator V SRD Guided through S OA2 At least part of S OA21 But there is at least one flow S UA At least part of S UA1 This can be done by heating.

[0300] The heat transfer devices include, in particular, the heat transfer devices WT listed below. X ,WT Y ,WT Z In step (f) of the process according to the invention, in particular, a heat exchanger, such as a evaporator, can be used. OA2 At least one flow S from at least a portion of UA At least part of S UA1 The transfer of energy, preferably heat, to the bottom evaporator V SRD It is carried out internally.

[0301] "Indirect" means, in particular, OA2 At least part of S OA21 at least one heat transfer medium W1 and preferably at least one heat exchanger WT X and the heat transfer medium is contacted through at least one stream S UA At least part of S UA1That is, W1 is different from this, so that energy, preferably heat, flows through S without mixing both flows. OA2 At least part of S OA21 to at least one heat transfer medium W1, and then the heat is transferred from W1 to at least one flow S by contacting W1 with the component of interest. UA At least part of S UA1 and at least one flow S UA At least part of S UA1 and W1 means mixed or unmixed, preferably unmixed.

[0302] In a further embodiment of the method according to the invention, S OA2 At least part of S OA21 At least one flow S UA At least part of S UA1 In particular, in the case of indirect energy transfer to S OA2 At least part of S OA21 At least one flow S UA At least part of S UA1 In the case of heating, first, energy, preferably heat, is introduced into the OA2 to W1, preferably at least one heat exchanger WT X and then at least one flow S from W1 UA At least part of S UA1 and a further heat transfer medium W2 different from the at least one heat exchanger WT Y Then, in the final step, at least one flow S UA At least part of S UA1 Heat is transferred to at least one flow S UA At least part of S UA1 and W2 may be commingled or uncombined, preferably uncombined.

[0303] It will therefore be appreciated that further embodiments of the present invention may utilize further heat transfer media W3, W4, W5 etc.

[0304] The heat transfer medium W1 or the additional heat transfer mediums W2, W3, W4, and W5 can be any heat transfer medium known to those skilled in the art, preferably selected from the group consisting of air, water, alcohol-water solutions, and salt-water solutions, including ionic liquids such as LiBr solutions, dialkylimidazolium salts, particularly dialkylimidazolium dialkylphosphates, mineral oils such as diesel oil, heat transfer oils such as silicone oils, organic oils such as limonene, and aromatic hydrocarbons such as dibenzyltoluene. Most preferably, the heat transfer medium W1 is water or air, most preferably water.

[0305] Usable salt-water solutions are also described, for example, in DE 102005028451 A1 and WO 2006 / 134015.

[0306] Then, following step (f), S OA2 At least part of S OA21 optionally with fresh methanol and / or in the rectification column RD A together with the reflux of and / or the stream S obtained after carrying out step (d) OA11 Together with the rectification column RD A To this end, in a preferred embodiment, these streams are collected in a condensate vessel, as described in Section 4.9.5.

[0307] In a preferred embodiment, S OA2 At least part of S OA21 From, especially S UA At least part of S UA1 After the transfer of energy to the

[0308] In a preferred embodiment of the method according to the invention, the energy, more preferably heat, is OA2 At least part of S OA21 Energy is transferred from SUA At least part of S UA1 After being transmitted to S OA2 At least part of S OA21 From S OA To, especially S OA This S OA A portion of the S is fed to compression, preferably compression in step (b), which is OA Pre-compression or S OA S OA1 This may be a compression to a flow S OA Tower RD A This is the first compression applied after exiting from S OA To heat at least part of the OA2 This allows for the use of some of the residual energy or heat in the process that is still stored by the

[0309] S OA2 Other preferred further reductions in energy, preferably heat, in at least a portion of are described further below (see section 4.3).

[0310] 4.9 Characterization step (g) As shown in the examples (Compare Example 3 with Examples 1 and 2), the compressed steam S OA1 Stage (S OA11 The shape of the side flow S ZA is used to transfer energy to S OA1 Compared to steam S, which is more strongly compressed OA2 Stage (S OA2 At least part of S OA21 The bottom flow S UA At least part of S UA1 Stage-compressed steam S used to transfer energy to OA The use of already results in energy savings. This increased energy efficiency of the method according to the invention is therefore already ensured by the combination of steps (b) to (f).

[0311] This energy efficiency is further increased by the characterization step (g) of the method according to the invention.

[0312] 4.9.1 General In the characterization step (g) of the method according to the invention, energy, preferably heat, is added to the AP One or more flows S from at least a portion of XA and if step (a2) is carried out, additionally or alternatively, energy, preferably heat, is transferred to at least a portion of S BP One or more flows S from at least a portion of XB is transmitted to at least a portion of the

[0313] S XA and S XB is S OA ,S OA1 ,S OA2 In particular, S XA and S XB is S OA ,S OA1 Preferably, S XA and S XB are S OA is.

[0314] In other words, in the characterization step (g), the energy, preferably heat, is AP From at least part of S OA ,S OA1 ,S OA2 Preferably selected from S OA ,S OA1 and if step (a2) is carried out, additionally or alternatively, energy, preferably heat, is transferred to at least a portion of one or more streams selected from S BP From at least part of S OA ,S OA1 ,S OA2 Preferably selected from S OA ,S OA1 is conveyed to at least a portion of one or more streams selected from

[0315] Therefore, in a particularly preferred embodiment of characterizing step (g) of the method according to the invention, the energy, preferably heat, is AP Flow from at least part of S OA and if step (a2) is carried out, additionally or alternatively, energy, preferably heat, is transferred to at least a portion of S BP Flow from at least part of S OA is transmitted to at least a portion of the

[0316] By step (g) according to the invention, the bottom product stream S AP and / or bottom product stream S BP The residual energy, in particular the residual heat, in step (g) is not dissipated unused but is instead integrated into the process according to the invention, and the energy balance of the process according to the invention is therefore further improved compared to a process not according to the invention (i.e. a process carried out without step (g)).

[0317] S AP One or more flows S from at least a portion of XA to at least a portion of, or S BP One or more flows S from at least a portion of XB The transfer of energy to at least a portion of is preferably done directly or indirectly.

[0318] "Direct" means S AP or S BP At least part of AP and S XA or S BP and S XB Without mixing, one or more flows S XA or S XB so that energy, in particular heat, is transferred to the S AP At least part of S XA or S BP From S XB This means to transmit to

[0319] This is SAP and at least a portion of one or more streams S XA or S BP and at least a portion of one or more streams S XB At least a portion of the heat transfer device WT (for example, the heat transfer device WT shown in the figure) ◆ ,WT △ or W.T. ● etc.), and the energy is AP From S XA or S BP From S XB In particular, XA S AP By or S XB S BP This can be done by heating the mixture by

[0320] The heat transfer devices include, in particular, the heat transfer devices WT listed below. X ,WT Y ,WT Z or the heat transfer devices WT, WT mentioned above ◆ ,WT △ or W.T. ● As the heat exchanger, a heat exchanger, in particular an evaporator, which is common to those skilled in the art can be used.

[0321] "Indirect" means, in particular, AP or S BP At least a part of the heat transfer medium W1 and preferably at least one heat exchanger WT X The heat transfer medium W1 is contacted through S OA ,S OA1 or S OA2 That is, W1 is different from these, so that energy, preferably heat, flows through S without mixing both flows. AP or S BP This means that at least a portion of the heat transfer medium W1 is transferred to at least one heat transfer medium W1. Then, W1 and one or more flows S XA or S XB At least a portion of the heat exchanger WT Yand both streams are mixed or not mixed, preferably not mixed, so that energy, preferably heat, is transferred from W1 to S XA or S XB to be communicated to.

[0322] In a further embodiment of the method according to the invention, also in the case of indirect energy transfer, energy, preferably heat, is first transferred to a AP or S BP from at least a portion of W1 to preferably at least one heat exchanger WT X and then from W1 to a further heat transfer medium W2, preferably through at least one heat exchanger WT Y The heat transfer can be achieved by contact through the heat transfer medium W1 and W2. OA ,S OA1 or S OA2 Then, in the final step, one or more streams S are drawn from W2. XA or S XB and heat is transferred to at least a portion of W2 and S XA or S XB may be mixed or unmixed, preferably unmixed.

[0323] It will therefore be appreciated that further embodiments of the present invention may utilize further heat transfer media W3, W4, W5 etc.

[0324] The heat transfer medium W1 or the additional heat transfer mediums W2, W3, W4, and W5 can be any heat transfer medium known to those skilled in the art, preferably selected from the group consisting of air, water, alcohol-water solutions, and salt-water solutions, including ionic liquids such as LiBr solutions, dialkylimidazolium salts, particularly dialkylimidazolium dialkylphosphates, mineral oils such as diesel oil, heat transfer oils such as silicone oils, organic oils such as limonene, and aromatic hydrocarbons such as dibenzyltoluene. Most preferably, the heat transfer medium W1 is water or air, most preferably water.

[0325] Usable salt-water solutions are also described, for example, in DE 102005028451 A1 and WO 2006 / 134015.

[0326] In step (g) of the method according to the invention, S AP or S BP One or more flows S into which energy is transferred XA and at least a portion of one or more streams S XB At least a portion of each flow S OA ,S OA1 ,S OA2 It may be the whole or each flow S OA ,S OA1 ,S OA2 It may be only a part of.

[0327] In particular, in step (g), the flow S XA and at least a portion of flow S XB At least some of the are, independently of one another, at least one of the following streams (the underlined ones are preferred): - S OA At least part of S OA◆ ; - When the above-described "embodiment △" is implemented, S OA Part of S OA△ (described in Section 4.10.1); -S OA11 and S OA12 Flow before separation S OA1 ; - Flow S OA1 Part of S OA11 ; - Flow S OA1 Part of S OA12 ; - When the previously described "embodiment ●" is implemented, flow S OA1 Part of S OA● (described in Section 4.10.2); -S OA2 At least part of S OA21 ; - When the above-described "embodiment ◇" is implemented, flow S OA2 Part of S OA◇ (described in Section 4.10.3).

[0328] 4.9.2 S XA and / or S XB S before compression AP and / or S BP Transfer of energy from In a more preferred embodiment of step (g), the stream S XA At least a portion of the energy is converted to S AP and compressed after being transferred from at least a portion of the stream S XB At least a portion of the energy is converted to S BP is compressed after being transmitted from at least a portion of the

[0329] This more preferred embodiment thereby reduces the product stream S AP and / or product stream S BP This is particularly advantageous because not only does it ensure the integration of energy in the steam to be compressed, but also because energy, in particular heat, is supplied to the steam to be compressed before its compression. This causes any liquid present in the steam to be compressed, which is typically in the form of droplets, to be converted into a gaseous state and / or prevents unwanted condensation of the steam before or during compression. This has the advantage that liquid in the stream to be compressed adversely affects the compressor's mechanics, and therefore avoidance of this increases the compressor's service life.

[0330] "S AP and, if step (a2) is performed, additionally or alternatively, S BP "At least a part of" is referred to below as "S AP or S BP" is abbreviated as ".

[0331] In this embodiment, the flow S compressed by the method according to the invention XA At least a portion of or flow S XB energy, preferably heat, S AP or S BP At the same time, S AP or S BP Flow S XA At least a portion of or flow S XB This transfer of energy, preferably heat, to at least a portion of the material occurs before the at least a portion of the material is compressed.

[0332] In certain embodiments, 4.9.2.1, in step (g), the energy is S AP or S BP Flow S OA At least part of S OA◆ which is then compressed in step (b). If this compression in step (b) is carried out in multiple stages, preferably in step (g) the energy is transferred to S AP or S BP Flow S OA At least part of S OA◆ and then the flow S OA At least some of this OA◆ is compressed in the first stage.

[0333] In a further specific embodiment 4.9.2.2, in step (g), the energy is S AP or S BP Flow S OA12 This is then compressed in step (e). OA12 If this compression is carried out in multiple stages, preferably in step (g) the energy is AP or S BP Flow from at least part of S OA12 and then the flow S OA12 is compressed in the first stage.

[0334] A further specific embodiment 4.9.2.3 is as follows: In embodiment Δ (described in section 4.10.1), the flow S OA△ But the steam flow S OA After separation from the starting material stream S AE1 and if step (a2) is carried out, alternatively or additionally in step (a2) starting material stream S BE1 When used as the energy in step (g), S AP or S BP Flow S OA△ It is even more preferable if the signal is transmitted to a signal S and then compressed. OA△ If this compression is carried out in multiple stages, preferably in step (g) the energy is AP or S BP Flow from at least part of S OA△ and then the flow S OA△ is compressed in the first stage.

[0335] A further specific embodiment 4.9.2.4 is as follows: In embodiment ● (described in section 4.10.2), the flow S OA● But the steam flow S OA1 After separation from the starting material stream S AE1 and if step (a2) is carried out, alternatively or additionally in step (a2) starting material stream S BE1 When used as the energy in step (g), S AP or S BP Flow S OA● It is even more preferable if the signal is transmitted to a signal S and then compressed. OA● If this compression is carried out in multiple stages, preferably in step (g) the energy is AP or S BP Flow from at least part of S OA● and then the flow S OA● is compressed in the first stage.

[0336] A further specific embodiment 4.9.2.5 is as follows: In the embodiment ◇ (described in section 4.10.3), the flow S OA◇ But the steam flow S OA2 After separation from the starting material stream S AE1 and if step (a2) is carried out, alternatively or additionally in step (a2) starting material stream S BE1 When used as the energy in step (g), S AP or S BP Flow S OA◇ It is even more preferable if the signal is transmitted to a signal S and then compressed. OA◇ If this compression is carried out in multiple stages, preferably in step (g) the energy is AP or S BP Flow from at least part of S OA◇ and then the flow S OA◇ is compressed in the first stage.

[0337] S XA and S XB But, S OA ,S OA1 In the embodiments of step (g) of the method according to the invention, each independently selected from the group consisting of:

[0338] S XA and S XB are S OA In the embodiment of step (g) of the method according to the invention, wherein:

[0339] 4.9.3 Preferred Embodiment Ω S XA and S XB are S OA The embodiment of step (g) of the process according to the invention, in which: is referred to below as "embodiment Ω", is particularly advantageous.

[0340] In other words, in embodiment Ω in step (g) of the method according to the invention, energy, preferably heat, is added to the reaction mixture S AP Flow from at least part of S OA and if step (a2) is carried out, additionally or alternatively, energy, preferably heat, is transferred to at least a portion of S BP Flow from at least part of S OA is transmitted to at least a portion of the

[0341] When carrying out the method according to the invention according to embodiment Ω, the flow S OA1 ,S OA2 A part of the energy, preferably heat, of the side stream S ZA Transmission to (S OA1 Part of S OA11 (in the case of step (f)) or bottom flow S UA At least part of S UA1 Transmission to (S OA2 At least part of S OA21 By utilizing even more in addition to the case of (in the case of), it is possible to reduce the energy efficiency even further, thereby making an even further contribution to improving the overall energy efficiency of the method according to the invention.

[0342] Therefore, in the embodiment Ω, energy, preferably heat, is converted into S OA1 ,S OA2 a crude product RP from at least a portion of the stream selected from A and, if step (a2) is carried out, alternatively or additionally, the crude product RP B It is preferable to transmit the information to

[0343] "[...]crude product RP A and, if step (a2) is carried out, alternatively or additionally, the crude product RP B [...]" is referred to below as "RP A or RP B " is abbreviated as ".

[0344] "S OA1 RP from at least part ofA or RP B "Transfer of energy, preferably heat, to" refers in particular to (i-1) S OA11 Before being used in step (d), S OA11 From RP A or RP B the transfer of energy, preferably heat, to; (ii-1) In step (d), S OA11 After is used, S OA11 From RP A or RP B the transfer of energy, preferably heat, to; (iii-1) S OA11 ,S OA12 and S OA● Different from the flow S OA1 Part of S OA14 From RP A or RP B Transfer of energy, preferably heat, to Includes.

[0345] Here, embodiments (ii-1) and (iii-1) are preferred, with embodiment (iii-1) being even more preferred.

[0346] "S OA2 RP from at least part of A or RP B "Transfer of energy, preferably heat, to" refers in particular to (i-2) S OA2 At least some of this OA21 Before being used in step (f), S OA2 At least part of S OA21 From RP A or RP B the transfer of energy, preferably heat, to; (ii-2) S OA2 At least some of this OA21 After being used in step (f), S OA2 At least part of S OA21 From RP A or RP B the transfer of energy, preferably heat, to; (iii-2) S OA21 Different from the flow S OA2 Part of S OA22 From RP A or RP B Transfer of energy, preferably heat, to Includes.

[0347] Here, embodiments (ii-2) and (iii-2) are preferred, with embodiment (iii-2) being even more preferred.

[0348] To that end, in a preferred embodiment of embodiment Ω, S OA1 ,S OA2 at least a portion of the flow to which energy from the flow has previously been transferred, preferably S OA1 ,S OA2 Alternatively, a portion of the flow selected from the heat transfer medium W1 is passed through the intermediate evaporator V ZA or V ZB Guided through S OA1 ,S OA2 Energy from the flow selected from W1 is extracted via a side outlet RR A or RR B In particular, S OA1 ,S OA2 At least a portion of the stream selected from W1 or W2 is fed to the evaporator V ZA or V ZB It is used to heat the

[0349] Alternatively, and even more preferably, in embodiment Ω, S OA1 ,S OA2 at least a portion of the flow to which energy from the flow has previously been transferred, preferably S OA1 ,S OA2 Or a portion of the flow selected from the heat transfer medium W1 is fed to the bottom evaporator V SA or V SB Guided through S OA1 ,S OA2or W1, the energy from at least a portion of the stream selected from the bottom product stream S AP or S BP In particular, S OA1 ,S OA2 or W1, the flow selected from the evaporator V SA or V SB It is used to heat the

[0350] 4.9.4 Plate Package Evaporator A particular embodiment of an evaporator that can be used as a heat transfer device in the context of the present invention, but that is advantageously used to transfer energy, particularly in the context of characterizing step (g), is a tube bundle evaporator, preferably one that includes a plate package. An example of such a plate package evaporator is shown in Figures 16A and 16B.

[0351] 4.9.5 Condensate container In a preferred embodiment of the present invention, the vapor stream S obtained following steps (d) and (f) OA11 or S OA21 RD A This is preferably done by collecting them in a container, in particular a condensate container, which preferably contains fresh methanol to be optionally supplied and optionally RD A The reflux stream generated within the RD is also collected. Each stream can be fed to the vessel by discharging them into the vessel through a valve. The combined, optionally condensed vapors are then passed from the vessel to the RD. A Corresponding embodiments <419> is shown in Figure 11.

[0352] 4.10 Starting Material Stream S AE1 and / or S BE1 Rectification column RD as A Steam recycling In a preferred embodiment, S OA ,S OA1 ,S OA2a portion of at least one of the vapors selected from the starting material stream S AE1 and if step (a2) is carried out, alternatively or additionally in step (a2) the starting material stream S BE1 Even more preferably, steam S OA ,S OA1 a portion of at least one of the starting material streams S AE1 and if step (a2) is carried out, alternatively or additionally in step (a2) the starting material stream S BE1 Used as.

[0353] In a more preferred embodiment, S OA ,S OA1 ,S OA2 a portion of one of the vapors selected from the starting material stream S AE1 and if step (a2) is carried out, alternatively or additionally in step (a2) the starting material stream S BE1 Even more preferably, steam S OA ,S OA1 A portion of one of the starting material streams S AE1 and if step (a2) is carried out, alternatively or additionally in step (a2) the starting material stream S BE1 Even more preferably, steam S OA A portion of the starting material stream S AE1 and if step (a2) is carried out, alternatively or additionally in step (a2) the starting material stream S BE1 Used as.

[0354] Therefore, in certain embodiments of the method according to the present invention, it is advantageous to select at least one of the embodiments △, ●, ◇ described below, preferably one of the embodiments △, ● described below, most preferably embodiment △.

[0355] 4.10.1 Steam flow S OA At the stage of... In a preferred embodiment of the method according to the invention, SOA◆ Different from the steam flow S OA Part of S OA△ But, S OA is separated from the OA△ In step (a1), the starting material stream S AE1 and if step (a2) is carried out, alternatively or additionally in step (a2) the starting material stream S BE1 This embodiment is abbreviated as "embodiment △."

[0356] Even more preferably, in embodiment △, the flow S OA△ is the steam flow S OA After separation from the starting material stream S AE1 and if step (a2) is carried out, alternatively or additionally in step (a2) the starting material stream S BE1 Used as.

[0357] Flow S OA△ The compression of flow S by step (b) in section 4.4 OA◆ As described for the compression of S, the compression can be carried out by means common to those skilled in the art. Thus, the compression can be carried out, for example, mechanically, in a single stage or in multiple stages, preferably in multiple stages. In the case of multiple stage compression, multiple compressors of the same type or compressors of different types can be used. Multistage compression can be carried out using one or more compressors. The use of single stage or multistage compression depends on the compression ratio, and therefore on the S OA△ It depends on how much pressure is desired to be compressed. Typically, S OA△ is the starting material flow S AE1 or S AE2 It is desirable to use the reactor RR as A and / or RR B up to the pressure level corresponding to the pressure level in OA△ Compression is performed.

[0358] S OA△ Preferably, at least one compressor VD △and then in step (a1) the starting material stream S AE1 and if step (a2) is carried out, alternatively or additionally in step (a2) the starting material stream S BE1 Used as.

[0359] Therefore, in particular, S OA△ At least one compressor VD △ is used. Compressor VD △ Any compressor known to those skilled in the art, preferably a mechanical compressor capable of compressing a gas flow, is suitable as the compressor, for example a single-stage or multi-stage turbine, a piston compressor, a screw compressor, a centrifugal compressor or an axial compressor.

[0360] 4.10.2 Steam flow S OA1 At the stage of... In a further preferred embodiment of the method according to the invention, S OA11 and S OA12 Different from the steam flow S OA1 Part of S OA● But, S OA1 is separated from the OA● In step (a1), the starting material stream S AE1 and if step (a2) is carried out, alternatively or additionally in step (a2) the starting material stream S BE1 This embodiment is abbreviated as "Embodiment ●".

[0361] Even more preferably, in the embodiment, the flow S OA● is the steam flow S OA1 After separation from the starting material stream S AE1 and if step (a2) is carried out, alternatively or additionally in step (a2) the starting material stream S BE1 Used as.

[0362] Flow S OA● The compression of flow S by step (b) in section 4.4 OA◆As described for the compression of S, the compression can be carried out by means common to those skilled in the art. Thus, the compression can be carried out, for example, mechanically, in a single stage or in multiple stages, preferably in multiple stages. In the case of multiple stage compression, multiple compressors of the same type or compressors of different types can be used. Multistage compression can be carried out using one or more compressors. The use of single stage or multistage compression depends on the compression ratio, and therefore on the S OA● It depends on how much pressure is desired to be compressed. Typically, S OA● is the starting material flow S AE1 or S AE2 It is desirable to use the reactor RR as A and / or RR B up to the pressure level corresponding to the pressure level in OA● Compression is performed.

[0363] To this end, in particular at least one compressor VD ● is used. Compressor VD ● Any compressor known to those skilled in the art, preferably a mechanical compressor capable of compressing a gas flow, is suitable as the compressor, for example a single-stage or multi-stage turbine, a piston compressor, a screw compressor, a centrifugal compressor or an axial compressor.

[0364] 4.10.3 Steam flow S OA2 At the stage of... In a further preferred embodiment of the method according to the invention, S OA21 Different from the steam flow S OA2 Part of S OA◇ But, S OA2 is separated from the OA◇ In step (a1), the starting material stream S AE1 and if step (a2) is carried out, alternatively or additionally in step (a2) the starting material stream S BE1 This embodiment is abbreviated as "Embodiment ◇".

[0365] Even more preferably, in the embodiment ◇, the flow SOA◇ is the steam flow S OA2 After separation from the starting material stream S AE1 and if step (a2) is carried out, alternatively or additionally in step (a2) the starting material stream S BE1 Used as.

[0366] Flow S OA◇ The compression of flow S by step (b) in section 4.4 OA◆ As described for the compression of S, the compression can be carried out by means common to those skilled in the art. Thus, the compression can be carried out, for example, mechanically, in a single stage or in multiple stages, preferably in multiple stages. In the case of multiple stage compression, multiple compressors of the same type or compressors of different types can be used. Multistage compression can be carried out using one or more compressors. The use of single stage or multistage compression depends on the compression ratio, and therefore on the S OA◇ It depends on how much pressure is desired to be compressed. Typically, S OA◇ is the starting material flow S AE1 or S AE2 It is desirable to use the reactor RR as A and / or RR B up to the pressure level corresponding to the pressure level in OA◇ Compression is performed.

[0367] To this end, in particular at least one compressor VD ◇ is used. Compressor VD ◇ Any compressor known to those skilled in the art, preferably a mechanical compressor capable of compressing a gas flow, is suitable as the compressor, for example a single-stage or multi-stage turbine, a piston compressor, a screw compressor, a centrifugal compressor or an axial compressor.

[0368] 4.11 Preferred embodiment: Alcohol exchange method for alkali metal alkoxides In an advantageous embodiment of the invention, the flow S OA1 ,S OA2The energy contained in at least one of these processes is used to operate other industrial processes. This is particularly advantageous in complexes (chemical parks, technology parks) where heating is constantly required. This energy can be used advantageously, particularly in complexes with multiple alkali metal alkoxide production facilities. Such complexes typically also include a method for producing alkali metal alkoxides by alcohol exchange. Such alcohol exchange methods are known to those skilled in the art and are described, for example, in WO 2021 / 122702, U.S. Pat. No. 3,418,383, DE 2726491, and CZ 213119.

[0369] In the method according to the invention, in a particular embodiment of the invention, S OA1 ,S OA2 The energy from at least a portion of the stream selected from C OR'' is used in the method for producing M C OR' is converted by R''OH to M C A crude product containing OR″, R′OH and optionally R″OH is obtained.

[0370] Here, R' and R'' are two different C1-C7 hydrocarbon residues, and in a preferred embodiment the hydrocarbon residue R' has at least one less carbon atom than R''.

[0371] The C1-C7 hydrocarbon residue is in particular a C1-C7 alkyl group.

[0372] Even more preferably, R' is methyl and R'' is selected from ethyl, n-propyl, isopropyl, sec-butyl, 2-methyl-2-butyl, tert-butyl, 2-methyl-2-pentyl, 3-methyl-3-pentyl, 3-ethyl-3-pentyl, 2-methyl-2-hexyl, 3-methyl-3-hexyl, in particular ethyl, isopropyl, 2-methyl-2-butyl, 3-methyl-3-pentyl, 3-ethyl-3-pentyl.

[0373] Preferably, R' and R" here are two different C1-C4 hydrocarbon residues, and in an even more preferred embodiment the hydrocarbon residue R' has at least one carbon atom less than R". The C1-C4 hydrocarbon residue is in particular a C1-C4 alkyl group.

[0374] Even more preferably, R' is methyl and R" is a C2-C4 hydrocarbon residue, which is preferably a C2-C4 alkyl group. Even more preferably, R' is methyl and R" is selected from ethyl, n-propyl, isopropyl, sec-butyl.

[0375] Most preferably, R'=methyl and R''=ethyl.

[0376] M C is a metal selected from lithium, sodium, and potassium, preferably potassium or sodium, more preferably sodium.

[0377] S OA1 ,S OA2 A preferred method of alcohol exchange using the energy of at least a portion of a stream selected from can be carried out by methods known to those skilled in the art.

[0378] In one embodiment, for example, M C OR' is mixed with R''OH in a suitable vessel, e.g., a stirred vessel, and the conversion is carried out by OA1 ,S OA2The energy supply is carried out by means of a heat transfer device WT, for example, whereby the energy is transferred to the flow S OA1 ,S OA2 M from at least a portion of the stream selected from C The alcohol R'OH formed is evaporated and M C A crude product containing OR″ and optionally R″OH is obtained.

[0379] In the method according to the present invention, in a preferred embodiment of the present invention, the reactive rectification column RR C Within, M C a starting material stream S comprising OR′ and optionally R′OH; CE1 is a starting material stream S containing R″OH CE2 By M C Crude product RP containing OR″ and R′OH C is converted countercurrently to RR C At the bottom of M C Bottom product stream S containing OR'' CP is extracted, RR C At the top of the vapor stream S containing R'OH CB is extracted, Katsu S OA1 ,S OA2 and wherein the energy from at least a portion of the stream selected from the group consisting of: C is transmitted to.

[0380] The process according to a preferred embodiment of the present invention (hereinafter also referred to as "alcohol exchange") is carried out in particular in a reactive rectification column RR C The reaction is carried out in the RR column. A For this purpose, columns such as those described in section 4.1.1 in the context of step (a1) are suitable.

[0381] Reactor RR C The can be operated with or without reflux, preferably with reflux. When reflux is generated, in particular steam S CB is partially or completely condensed RRCThe condensed vapor is then directed through the reactor RR C or, if R' = methyl, the starting material stream S AE1 or S BE1 This can be used as RD when R'=methyl. A It can also be used as a fresh methanol stream within the reactor.

[0382] When changing alcohol, RR C At the bottom of M C Bottom product stream S containing OR'' CP is extracted. RR C At the top of the vapor stream S containing R'OH CB is extracted.

[0383] In a preferred embodiment, when R'=methyl, M C a starting material stream S comprising OR′ and optionally R′OH; CE1 As for S AP When at least a part of (M A and M B or M when A and M B is the same alkali metal, especially M A and M B are different alkali metals) or additional (especially M A and M B are the same alkali metal), S BP At least a portion of the following is used. Particularly preferably, R"=ethyl. Thus, an alcohol exchange occurs from the alkali metal methoxide to the corresponding alkali metal ethoxide.

[0384] S BP and S AP If both streams contain the same alkali metal methoxide, then both streams can be separated or mixed to form S CE1 It is also possible to use as a column, i.e. in particular by first mixing and then C Starting material stream S CE1Can be led as or separated into towers RR C Two starting material streams S CE1 It can be derived as:

[0385] Starting material stream S CE2 In a preferred embodiment, S CE2 The mass fraction of R″OH in the CE2 is especially M C OR'' or other modifiers. Starting material stream S CE2 The alcohols R″OH used as may be commercially available alcohols with an alcohol mass fraction of more than 99.8% by weight and a water mass fraction of up to 0.2% by weight.

[0386] According to the present invention, "M C a starting material stream S comprising OR′ and optionally R′OH; CE1 a starting material stream S containing R″OH CE2 By In countercurrent "Converting" refers in particular to the reaction column RR C In M C Starting material stream S containing OR' CE1 At least some of the feed points of the starting material stream S containing R″OH CE2 This is ensured by being above the supply point of

[0387] Reactor RR C may be operated with or without reflux, preferably with reflux.

[0388] In a preferred embodiment, the reaction column RR C is especially suitable for intermediate evaporators. ZC and bottom evaporator V SC The reaction column RR includes at least one evaporator selected from the group consisting of: C Particularly preferably, at least one bottom evaporator V SC Includes.

[0389] Reactor RR C In the case of intermediate evaporation, at least one side stream SZC But, RR C is extracted ("extracted") from at least one intermediate evaporator V ZC are supplied to.

[0390] Reactor RR C In the case of , at the bottom evaporation, at least one stream, e.g., S CP But, RR C extracted ("extracted") from, at least in part, S CP In this case, preferably part of the at least one bottom evaporator V SC are supplied to.

[0391] Suitable evaporators that can be used as intermediate and bottom evaporators are described in Section 4.2.2.

[0392] During alcohol exchange, energy, preferably heat, is released into the OA1 ,S OA2 a crude product RP from at least a portion of the stream selected from C This is preferably done by transferring the energy to S OA1 ,S OA2 S from at least a portion of the stream selected from CE1 or S CE2 This is then transmitted to RR C Then, S CE1 or S CE2 From these, they are mixed, RR C The crude product RP present in C This occurs when the signal is transmitted to the

[0393] Therefore, energy, preferably heat, is OA1 ,S OA2 At least a portion of the stream selected from, in particular, S OA11 ,S OA12 ,S OA2 At least one stream selected from, preferably S OA11 ,S OA2 a crude product RP from at least one stream selected from the C is transmitted to.

[0394] "S OA1 from at least a portion of the crude product RP C "The transfer of energy, preferably heat, to OA11 ,S OA12 ,S OA11 ,S OA12 flow before its separation into S OA1 a crude product RP from at least one stream selected from C It also involves the transfer of energy, preferably heat, to the

[0395] In addition, the crude product RP C is the intermediate evaporator V ZC Or bottom evaporator V SC may be guided through V ZC Or V SC In the OA1 ,S OA2 a crude product RP from at least a portion of the stream selected from C may be transmitted to

[0396] In addition, the bottom product stream S CP is partially in the bottom evaporator V SC and then partially RR C may be sent back to V SC Within, energy, preferably heat, is OA1 ,S OA2 S from at least a portion of the stream selected from CP The returned part is then transmitted to the tower RR. C Within, S CP The crude product RP present in the column C is transmitted to.

[0397] Here, S OA1 ,S OA2 The transfer of energy from at least some of the streams selected from to the mentioned streams takes place directly or indirectly, i.e. without or with a heat transfer medium W1, correspondingly as described in section 4.1.4.

[0398] A preferred embodiment of the method according to the invention is OA1 ,S OA2 From, especially S OA2 ,S OA11 ,S OA12 This allows for efficient use of energy from the grid, thereby lowering overall energy requirements.

[0399] 5. Example Examples 1-3 not according to the invention and Example 4 according to the invention were carried out as shown in Figures 1-3 and 9, but the optional reflux route shown in Figures 1-3 and 9 was not used. <311> , and the compressor VD shown in Figs. △ <411> Flow by S OA△ <307> Compression of the above was not achieved in each of Examples 1-4.

[0400] 5.1 Example 1 (not according to the invention), corresponding to Figure 1: A flow of aqueous NaOH (50 wt%) S of 100 kg / h AE2 <102> is the reactor RR at 30°C. A <100> A vaporous methanol stream S of 1034.9 kg / h is fed countercurrently to the top of the reactor. AE1 <103> is the reactor RR A <100> The reactor RR is fed to the bottom of the reactor. A <100> The column RR is operated at a head pressure of 2.15 bar (absolute). A <100> At the bottom of the reactor, 219.7 kg / h of the nearly anhydrous product stream S AP <104> (30% by weight sodium methoxide in methanol) is withdrawn from the reactor RR. A <100> Evaporator V SA <105> A heating power of about 24 kW is delivered using low-pressure steam. AB <107> However, the reactor RR A <100> Of this, 80 kg / h is extracted from the head of the condenser K RRA <108> and refluxed in the reactor RR A<100> The remaining flow of 915.2 kg / h is sent back to the rectification column RD A <300> It is supplied to the rectification column RD A <300> is operated at a head pressure of 2.0 bar (absolute). A <300> At the bottom of the tank, a liquid water flow S of 72.2 kg / h UA <304> (500 ppm by weight of methanol) is discharged. A <300> At the head of the OA <302> (2 bar, 83°C, 200 ppm by weight of water) was extracted, of which 63.9 kg / h was extracted into the condenser K RD <407> The remaining flow is condensed in the first compressor VD AB2 <303> where it is compressed to 2.6 bar (absolute pressure). Subsequently, the stream is split to produce a stream S OA△ <307> is the reactor RR A <100> The remaining 804.8 kg / h is returned to S. OA◆ <306> is fed to a multi-stage compression with intercooling. Compressor VD1 <401> Within, the flow is p OA1 = 4.8 bar (absolute pressure) and T OA1 = 156°C, and the flow rate is S OA1 <403> Intercooler WT X <402> In the subsequent intercooling in the compressor VD, the flow is cooled to 145°C and approximately 4.4 kW of heat is rejected via the cooling water. x <405> Inside, the flow S OA1 <403> is further compressed to 9.0 bar and 200 °C, resulting in the stream S OA2 <404> At the same time, the fractionator RD A <300> Bottom evaporator V SRD <406> In the downstream condenser, a heating power of about 238 kW is applied to the rectification column RD A<300> The methanol stream condensed here becomes available for <404> is 191.9 kg / h of fresh methanol (1000 ppm by weight of water) <408> and 63.9 kg / h of pre-condensed steam, mixed together and fed to the rectification column RD A <300> The head is delivered and returned.

[0401] The total compressor power is approximately 55 kW. Combined with 24 kW of heating steam, the compressor and heating steam power requirements are approximately 79 kW.

[0402] 5.2 Example 2 (not according to the invention), corresponding to Figure 2: The arrangement in Example 2, which is not according to the invention, corresponds to that according to Example 1, with the following differences: Rectification tower RD A <300> is the intermediate evaporator V ZRD <409> Here, the rectification column RD A <300> to 94°C liquid flow S ZA <305> is extracted. ZRD <409> Approximately 230 kW of heat is transferred within the column, and the stream is partially evaporated and subsequently passed through the rectification column RD A <300> is supplied again.

[0403] Rectification tower RD A <300> At the head of the OA <302> (200 ppm by weight of water) was extracted, of which 89.4 kg / h was extracted by the condenser K RD <407> The remaining flow is condensed in the first compressor VD AB2 <303> Subsequently, a partial flow of 1034.9 kg / h is transferred to the reactor RR A <100> The remaining 762.8 kg / h is compressed to 5.6 bar (absolute pressure) and 168°C and sent back to stream S OA1 <403> At the same time, the fractionator RD A <300> Intermediate evaporator V ZRD<409> In the downstream condenser, a heating power of about 230 kW is applied to the rectification column RD A <300> The methanol stream condensed here becomes available for <403> 191.9 kg / h of fresh methanol <408> and 89.4 kg / h of pre-condensed steam, mixed together and fed to the rectification column RD A <300> The rectification column RD is then returned to the top of the column. A <300> Bottom evaporator V SRD <406> In comparison with Example 1, the intermediate evaporator V ZRD <409> The boiling temperature in the bottom evaporator V SRD <406> Because the vapor flow is lower than the ZRD <409> It does not need to be compressed to 9 bar (absolute) but only to 5.6 bar (absolute) so that it can be released at 1000 kJ / s.

[0404] Therefore, the compressor output is only about 38 kW in total (instead of 55 kW), but the heating steam requirement is therefore SRD <406> A heating power of 20 kW is required within the furnace, which increases to approximately 44 kW compared to Example 1 because heat is introduced by the low pressure.

[0405] The total compressor and heating steam power requirement is therefore approximately 82 kW.

[0406] 5.3 Example 3 (not according to the invention), corresponding to Figure 3: The arrangement in Example 3, which is not according to the invention, corresponds to that according to Examples 1 and 2, with the following differences: Rectification tower RD A <300> At the head of the OA <302> (200 ppm by weight of water) was extracted, of which 33.9 kg / h was extracted by the condenser K RD <407> The remaining flow is condensed in the first compressor VD AB2 <303> The pressure is then compressed to 2.6 bar (absolute pressure) in theOA△ <307> is the reactor RR A <100> The remaining 830.1 kg / h is returned to S. OA◆ <306> is first compressed to 5.6 bar (absolute pressure) and 169°C, and the stream S OA1 <403> Of this flow, a part of S OA11 <4031> (761.7 kg / h) was simultaneously A <300> Intermediate evaporator V ZRD <409> The heating power of about 230 kW is supplied to the rectification column RD A <300> Subsequently, other parts S OA12 <4032> (68.4 kg / h) is the intercooler WT X <402> The temperature is cooled to about 154°C by intermediate cooling in the furnace, and about 0.5 kW of heat is discharged through the cooling water. OA12 <4032> Further compressor VD x <405> compressed within the OA2 =9.0bar and T OA2 Flow S with = 196°C OA2 <404> At the same time, the fractionator RD A <300> Bottom evaporator V SRD <406> In the downstream condenser, a heating power of about 20 kW is applied to the rectification column RD A <300> Intermediate evaporator V ZRD <409> and bottom evaporator V SRD <406> The methanol stream S condensed in OA11 <4031> and S OA2 <404> 191.9 kg / h of fresh methanol <408> and 33.9 kg / h of pre-condensed steam, mixed together and fed to the rectification column RD A <300> The head is delivered and returned.

[0407] The total compressor power is approximately 42 kW (not 55 kW as in Example 1). Bottom evaporator V SRD<406> Since no low pressure steam is required, only about 24 kW needs to be made available through heating steam, as in Example 1. The compressor and heating steam power requirements are therefore reduced to a total of about 66 kW.

[0408] Compared to Example 1, a smaller vapor flow needs to be compressed to 9 bar (absolute pressure), and most of the vapor flow needs to be compressed to 5.6 bar (absolute pressure) as in Example 2, which reduces the overall compressor power. However, compared to Example 2, during steady state operation, the bottom evaporator V SRD <406> No low pressure steam is required within the reactor, so the heating steam requirements are reduced compared to Example 2.

[0409] The total energy required is minimized by the method according to Example 3.

[0410] However, in this embodiment, the flow S AP <104> The drawback is that the energy present in the flow S is dissipated without being utilized. AP <104> With a temperature of 105°C, A <100> This flow S AP <104> Since the resulting temperature of 105°C is not suitable for handling and storage, it is first cooled to 50°C, and then this stream S AP <104> This is usually done by transporting this flow S AP <104> This occurs by cooling the condensed stream, which dissipates some of the energy stored in it without being utilized. <4031> The residual energy usage is also low.

[0411] 5.4 Example 4 (according to the invention), corresponding to Figure 9: The method used in the case of Example 4 according to the invention is depicted in Figure 9. It corresponds to the method according to Example 3, but with the following differences:

[0412] Condenser K as reflux RD <407> Through the rectification tower RD A <300> The steam flow S that is not returned toOA <302> Part of the heat transfer device WT AB2 <418> This heat transfer device WT AB2 <418> consists of a container in which multiple plate heat transfer packages can be installed (see Figure 16A). AB2 <418> Inside, there is a flow AP <104> and S OA1 <4031> Two plate packages are installed to make the residual heat of the condensed flow S available to the system. OA1 <4031> is preferably the first plate package <81> is transported through the bottom flow S AP <104> Preferably, the second plate package <82> In both plate packages, a portion of the residual heat is transferred to the steam flow S OA <302> This steam flow S OA <302> is thereby superheated by 10 K (67 to 77 °C). AB2 <303> On the other hand, the formation of droplets on the suction side of the reactor RR is prevented (due to pressure drop) and the superheat is prevented. A <100> Used in steam-driven bottom evaporators. SA <105> The heating output of the heat transfer device WT AB2 <418> Heat integration of the heat transfer device reduces it by 46%. AB2 <418> Steam flow S conducted through OA <302> Overheating of a portion of the compressor VD AB2 <303> and VD1 <401> The power output of the multistage compressor in the compressor is increased by an additional 3%. Furthermore, this measure significantly reduces the possibility of droplet formation, especially on the suction side of the compressor, which can cause considerable damage to the impeller. The operating time of the multistage compressor is therefore increased. Finally, the bottom flow S AP <104> is cooled to 87°C by this procedure, which significantly simplifies its handling during storage.

[0413] resultThe procedure according to Example 3, in which the vapor stream is compressed in stages, whereby the intermediate evaporator and the bottom evaporator are operated with vapors compressed to different degrees, allows for surprising energy savings. Furthermore, the procedure according to the invention according to Example 4 allows for further energy savings, with the bottom product stream S AP <104> Energy transfer from the steam flow S OA <302> If the bottom product stream S is compressed before the compression of the bottom product stream S, the compressor life can be extended. AP <104> The handling of

[0414] Figure 17 shows a comparison of the energy required for each example, which shows that the process according to the present invention according to Example 4 is the most energy efficient.

[0415] 6. Abbreviations [Table 1-1] [Table 1-2] [Table 1-3]

Claims

1. Formula M Ａ OCH ３ [In the formula, M Ａ is a metal selected from sodium, potassium and lithium, (a1) a starting material stream S comprising methanol ＡＥ１ But M Ａ Starting material stream S containing OH ＡＥ２ By this, the reaction rectification column RR Ａ is converted countercurrently within the Ａ OCH ３ , water, methanol, M Ａ Crude product RP containing OH Ａ and R.R. Ａ At the bottom of Ａ OCH ３ a bottom product stream S ＡＰ is extracted, RR Ａ At the top of the vapor stream S containing water and methanol ＡＢ is extracted, (a2) optionally simultaneously with and spatially separated from step (a1), a methanol-containing starting material stream S ＢＥ１ But M Ｂ Starting material stream S containing OH ＢＥ２ By this, the reaction rectification column RR Ｂ is converted countercurrently within the Ｂ OCH ３ , water, methanol, M Ｂ Crude product RP containing OH Ｂ Become M Ｂ is selected from sodium, potassium, and lithium; R.R. Ｂ At the bottom of Ｂ OCH ３ a bottom product stream S ＢＰ is extracted, RR Ｂ At the top of the vapor stream S containing water and methanol ＢＢ is extracted, (a3) Steam flow S ＡＢ and at least a portion of the vapor stream S if step (a2) is performed. ＢＢ At least a part of ＡＢ Mixed with or S ＡＢ Separated from the rectification column RD Ａ Guided by RD Ａ Within, RD Ａ At least one vapor stream S containing methanol is withdrawn at the top end of ＯＡ and RD Ａ At least one stream S containing water is withdrawn at the lower end of ＵＡ and separated into (b) S ＯＡ At least a part S of ＯＡ◆ is compressed, so that S ＯＡ The compressed vapor flow S ＯＡ１ is obtained, (c) at least one side stream S ＺＡ But, RD Ａ Extracted from RD Ａ was sent back to (d) converting energy into the compressed vapor stream S ＯＡ１ The first part S ＯＡ１１ From S ＺＡ is transmitted to S ＺＡ RD Ａ was returned to (e) S ＯＡ１１ The compressed vapor flow S ＯＡ１ Part S ＯＡ１２ is further compressed, so that S ＯＡ１１ The compressed vapor flow S ＯＡ２ is obtained, (f) The energy is S ＯＡ２ At least a part S of ＯＡ２１ From S ＵＡ At least a part S of ＵＡ１ is transmitted to S ＵＡ１ RD Ａ will be returned to In the method, (g) The energy is S ＡＰ One or more streams S ＸＡ and if step (a2) is carried out, additionally or alternatively, the energy is transferred to at least a portion of S ＢＰ One or more streams S ＸＢ transmitted to at least a portion of S ＸＡ and S ＸＢ But, S ＯＡ , S ＯＡ１ , S ＯＡ２ are each independently selected from the group consisting of A method characterized by:

2. In step (d), the energy is transferred to the intermediate evaporator V ＺＲＤ Inside S ＯＡ１１ From S ＺＡ The method of claim 1 , wherein the

3. In step (f), the energy is transferred to the bottom evaporator V ＳＲＤ Inside S ＯＡ２ At least a part S of ＯＡ２１ From S ＵＡ At least a part S of ＵＡ１ The method of claim 1 , wherein the

4. S ＯＡ１１ The energy from S ＺＡ After being transmitted to S ＯＡ and / or S ＯＡ２ At least a part S of ＯＡ２１ The energy from S ＵＡ At least a part S of ＵＡ１ After being transmitted to S ＯＡ The method of claim 1 , wherein the

5. Rectification tower RD Ａ , reaction tower RR Ａ and reaction column RR if step (a2) is carried out. Ｂ 10. The method of claim 1, wherein at least two of the columns selected from are contained within a column shell, and the columns are at least partially separated from one another by a separating wall extending to the trays of the columns.

6. S ＯＡ◆ The vapor flow S ＯＡ Part S ＯＡ△ But, S ＯＡ is separated from S ＯＡ△ In step (a1), the starting material stream S ＡＥ１ and if step (a2) is carried out, alternatively or additionally in step (a2) the starting material stream S ＢＥ１ The method of claim 1, wherein the compound is used as

7. The flow S ＯＡ△ However, the vapor flow S ＯＡ After separation from the starting material stream S ＡＥ１ and if step (a2) is carried out, alternatively or additionally in step (a2) the starting material stream S ＢＥ１ 7. The method of claim 6, wherein the compound is used as

8. S ＯＡ１１ and S ＯＡ１２ The vapor flow S ＯＡ１ Part S ＯＡ● But, S ＯＡ１ is separated from S ＯＡ● In step (a1), the starting material stream S ＡＥ１ and if step (a2) is carried out, alternatively or additionally in step (a2) the starting material stream S ＢＥ１ The method of claim 1, wherein the compound is used as

9. The flow S ＯＡ● However, the flow S ＯＡ１ After separation from the starting material stream S ＡＥ１ and if step (a2) is carried out, alternatively or additionally in step (a2) the starting material stream S ＢＥ１ 9. The method of claim 8, wherein the compound is used as

10. S ＯＡ２１ The vapor flow S ＯＡ２ Part S ＯＡ◇ But, S ＯＡ２ is separated from S ＯＡ◇ In step (a1), the starting material stream S ＡＥ１ and if step (a2) is carried out, alternatively or additionally in step (a2) the starting material stream S ＢＥ１ The method of claim 1, wherein the compound is used as

11. The flow S ＯＡ◇ However, the vapor flow S ＯＡ２ After separation from the starting material stream S ＡＥ１ and if step (a2) is carried out, alternatively or additionally in step (a2) the starting material stream S ＢＥ１ 11. The method of claim 10, wherein the compound is used as

12. The flow S ＸＡ At least a portion of the energy is converted to S ＡＰ and, if step (a2) is carried out, additionally or alternatively, said stream S ＸＢ At least a portion of the energy is converted to S ＢＰ The method of claim 1 , wherein the signal is compressed after being transmitted from at least a portion of the

13. In step (g), S ＸＡ and S ＸＢ But, S ＯＡ , S ＯＡ１ The method of claim 1, wherein each of the compounds is independently selected from the group consisting of:

14. In step (g), S ＸＡ and S ＸＢ But, respectively, S ＯＡ 14. The method of claim 13, wherein:

15. Energy is S ＯＡ１ , S ＯＡ２ a crude product RP from at least a portion of the stream selected from Ａ and if step (a2) is carried out, alternatively or additionally, the crude product RP Ｂ 15. The method of claim 14, wherein the

16. S ＯＡ１ , S ＯＡ２ The energy from at least a portion of the stream selected from Ｃ OR'', in which M Ｃ OR' is converted by R''OH to M Ｃ resulting in a crude product comprising OR″, R′OH, and optionally R″OH, R′ and R″ are two different C １ ~C ７ is a hydrocarbon residue, M Ｃ is a metal selected from lithium, sodium, and potassium; The method of claim 1.

17. Reactive rectification column RR Ｃ Inside, M Ｃ a starting material stream S containing OR′ ＣＥ１ is a starting material stream S containing R″OH ＣＥ２ is countercurrently converted by M Ｃ Crude product RP containing OR″ and R′OH Ｃ and R.R. Ｃ At the bottom of M Ｃ bottom product stream S containing OR″ ＣＰ is extracted, RR Ｃ At the top of the vapor stream S containing R'OH ＣＢ is extracted, S ＯＡ１ , S ＯＡ２ The energy from at least a portion of the stream selected from the crude product RP Ｃ transmitted to 17. The method of claim 16.

18. 18. The method of claim 17, wherein R' = methyl.

19. S ＡＰ is obtained by the method of claim 1, and S ＡＰ At least a part of ＣＥ１ 19. The method of claim 18, wherein the compound is used as

20. S ＢＰ is obtained by the method of claim 1 by carrying out step (a2), and S ＢＰ At least a part of ＣＥ１ 19. The method of claim 18, wherein the compound is used as

21. 18. The method of claim 17, wherein R''=ethyl.

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