Integrated method for parallel production of alkali metal methanol salts
By splitting the methanol feed stream in a single distillation column to multiple reactive distillation columns and combining it with rectification column processing, the problems of high equipment cost and flexibility in preparing mixtures of different alkali metal methanol salts are solved, and economical and efficient mixture preparation is achieved.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- BASF SE
- Filing Date
- 2021-12-03
- Publication Date
- 2026-05-26
AI Technical Summary
In existing technologies, the preparation of alkali metal methanol salts and methanol mixtures of different concentrations or compositions requires multiple independent plants or frequent adjustments to production parameters, resulting in high equipment costs and an inability to flexibly respond to market demands.
A single distillation column is used to divide the methanol feed into multiple streams, which are then fed into multiple parallel reactive distillation columns for processing, combined with a rectification column, to achieve the simultaneous preparation of various alkali metal methanol salts and methanol mixtures.
It significantly reduces equipment costs, allows for flexible adjustment of the preparation amount of the mixture, adapts to market demands, and reduces the economic cost and operational complexity of production.
Smart Images

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Abstract
Description
[0001] This invention relates to a highly advantageous new method for the simultaneous preparation of alkali metal methoxides in two or more parallel reactive distillation columns. Furthermore, this invention relates to a chemical production apparatus for carrying out this method.
[0002] Methods for preparing a mixture comprising an alkali metal alkoxide and methanol from a methanol feed stream and an aqueous feed stream—containing dissolved alkali metal hydroxides—in a reactive distillation column are described in the prior art. According to these methods, the methanol feed stream fed into the reactive distillation column is prepared by separating methanol from water in a distillation column upstream of the reactive distillation column and using the resulting methanol in the reactive distillation column. For this purpose, see, for example, US 2002 / 0183566 A1, US 2008 / 0296786 A1, or WO 2013 / 168113A1.
[0003] However, according to the teachings of these existing technical documents, only one specific mixture containing an alkali metal methoxide and methanol can be produced. Therefore, to simultaneously produce, for example, two different mixtures containing an alkali metal methoxide and methanol, such as two mixtures containing the same alkali metal methoxide but with different concentrations, or two mixtures containing different alkali metals, two completely independent plants are required, each including a distillation column for purifying the methanol stream and a reactive distillation column. Alternatively, if only one plant is used, the first mixture needs to be produced in the first round, the first process stopped, the production parameters readjusted, and the production of the second mixture started. However, both of these approaches are highly economically disadvantageous because the first approach, which allows the simultaneous production of two or more different mixtures containing an alkali metal methoxide and methanol, requires two or more complete plants, leading to, for example, enormous equipment costs; and the second approach, the continuous production of two different mixtures puts the plant at a disadvantage in terms of flexibility in responding to changing market demands.
[0004] Therefore, an object of the present invention is to provide an economically advantageous method for simultaneously preparing two or more mixtures comprising alkali metal hydroxides and methanol. Another object of the present invention is to provide a method for preparing two or more mixtures comprising alkali metal hydroxides and methanol, which allows for easy adjustment of the preparation quantity of the mixture depending on the corresponding market demand.
[0005] It was surprising to find that these objectives could be achieved by a method that uses a single distillation column to generate a methanol feed stream, which, after being appropriately split into two or more sub-streams, is used as a source of methanol for two or more parallel downstream reactive distillation columns—in which two or more different mixtures containing alkali metal methoxides and methanol are prepared simultaneously.
[0006] Therefore, the present invention relates to an integrated method for simultaneously preparing n mixtures P(i) comprising alkali metal methoxides and methanol, comprising:
[0007] Provide n reactive distillation columns K(i);
[0008] Provide n aqueous liquid streams H(i), where each stream H(i) contains dissolved alkali metal hydroxide A(i)OH, and n is an integer, where n ≥ 2 and i = 1…n; and
[0009] Provide distillation column D;
[0010] The method further includes:
[0011] (a) Provide a feed stream G containing methanol;
[0012] (b) Divide the material flow G into n material flows G(i), each material flow G(i) having the same composition as G;
[0013] (c) Preparing the one or more alkali metal methanol salts, comprising:
[0014] Each feed stream G(i) is fed into the lower part of the corresponding reactive distillation column K(i), and an aqueous liquid stream H(i) containing dissolved alkali metal hydroxide A(i)OH is fed into the upper part of the reactive distillation column K(i); and
[0015] G(i) and H(i) are subjected to reactive distillation conditions in each K(i) to obtain n overhead feed streams W(i) containing methanol and water; and n streams containing alkali metal methanol salt A(i)OMe and methanol are obtained.
[0016] The bottom material flow P(i);
[0017] (d) Feed each feed stream W(i) into the lower part of the distillation column D, and feed the feed stream M containing methanol into
[0018] In distillation column D; and subjecting the n streams W(i) and M to distillation conditions in D to obtain the stream G as the top stream according to (a).
[0019] Compared to the teachings of the prior art, the method of the present invention allows for significant savings in equipment costs, as only one rectification column is required for all reactive distillation columns; furthermore, the method of the present invention allows for great flexibility in responding to market demands regarding the supply of different mixtures comprising alkali metal methoxides and methanol, as the corresponding amounts of different mixtures can be easily adjusted by appropriately dividing the methanol feed stream obtained from the upstream single distillation column.
[0020] Preferably, in the method of the present invention, n is in the range of 2-10, more preferably in the range of 2-5, such as 2, 3, 4 or 5, more preferably 2 or 3, and more preferably 2.
[0021] For the alkali metal hydroxide A(i)OH, preferably each alkali metal hydroxide A(i)OH is selected from lithium hydroxide, sodium hydroxide, and potassium hydroxide, more preferably from sodium hydroxide and potassium hydroxide. According to the method of the invention, it is feasible for at least two alkali metal hydroxides A(i)OH to be identical; in this case, the invention, for example, allows the preparation of a first mixture P(i) containing a first alkali metal hydroxide A(i)OH and having a first alkali metal hydroxide concentration, and a second mixture P(i) containing the first alkali metal hydroxide A(i)OH and having a second alkali metal hydroxide concentration different from that first alkali metal hydroxide concentration; thus, according to this feasible method, two mixtures P(i) with different concentration specifications that may be required in the market can be prepared. Preferably, at least two of the alkali metal hydroxides A(i)OH are different from each other, more preferably, especially if n is 2 or 3, preferably 2, then all alkali metal hydroxides A(i)OH are different from each other.
[0022] A given aqueous stream H(i) contains an alkali metal hydroxide A(i)OH dissolved in water. Preferably, at least one of these streams H(i) may contain a certain amount of methanol in addition to water and the dissolved alkali metal hydroxide A(i)OH. Preferably, the given aqueous stream H(i) consists essentially of an alkali metal hydroxide A(i)OH dissolved in water.
[0023] As described above, according to the present invention, it is preferable to prepare two mixtures P(i) simultaneously. Therefore, the present invention preferably relates to an integrated method for simultaneously preparing two mixtures P(i), wherein mixture P(1) comprises A(1)OMe, more preferably sodium methoxide, and methanol, and mixture P(2) comprises A(2)OMe, more preferably potassium methoxide, and methanol, the method comprising:
[0024] (a) Provide a feed stream G containing methanol;
[0025] (b) Divide the material flow G into at least two material flows G(1) and G(2), G(1) and G(2) having the same characteristics as G.
[0026] Composition;
[0027] (c.1) Preparation of A(1)OMe, including:
[0028] (c.1.1) Feed stream G(1) is fed into the lower part of reactive distillation column K(1), and liquid stream H(1), preferably aqueous liquid stream H(1), is fed into the upper part of reactive distillation column K(1), wherein H(1) contains dissolved A(1)OH, more preferably sodium hydroxide;
[0029] (c.1.2) G(1) and H(1) are subjected to reactive distillation conditions in K(1) to obtain a top stream W(1) containing methanol and water; and a bottom stream P(1) containing A(1)OMe and methanol.
[0030] (c.2) Preparation of A(2)OMe, including:
[0031] (c.2.1) Feed stream G(2) is fed into the lower part of reactive distillation column K(2), wherein K(2) is arranged parallel to K(1), and liquid stream H(2), preferably aqueous liquid stream H(2), is fed into the upper part of reactive distillation column K(2), wherein H(2) contains dissolved A(2)OH, more preferably potassium hydroxide;
[0032] (c.2.2) G(2) and H(2) are subjected to reactive distillation conditions in K(2) to obtain a top stream W(2) containing methanol and water; and a bottom stream P(2) containing A(2)OMe and methanol.
[0033] (d.1) Feed W(1) and W(2) into the lower part of the distillation column D, and feed the methanol-containing stream M into the lower part of the column D.
[0034] It enters distillation column D;
[0035] (d.2) subject W(1), W(2) and M to distillation conditions in D to obtain the feed stream G according to (a) as the overhead feed stream.
[0036] Preferably, feed streams W(1) and W(2) are fed into distillation column D as gas streams. These feed streams can generally be fed into distillation column D independently at any suitable location. Preferably, these feed streams are fed independently between the bottom of distillation column D and the 15th theoretical stage, more preferably between the bottom of the column and the 10th theoretical stage, and even more preferably between the bottom of the column and the 8th theoretical stage. According to the invention, feed streams W(1) and W(2) can be fed into D as separate feed streams or, appropriately, feed streams W(1) and W(2) can be combined and the corresponding combined feed stream W can be fed into D.
[0037] For distillation column D, it is preferable to have 20-100, more preferably 30-80, and even more preferably 40-60 theoretical stages. Feasible preferred ranges are, for example, 40-50, 45-55, or 50-60. The top pressure of distillation column D can generally be freely selected within a wide range, provided the desired separation task is accomplished. Preferably, distillation column D is operated at a top pressure in the range of 0.5-10 bar (abs), more preferably 0.75-6 bar (abs), and even more preferably 1-5 bar (abs). Feasible preferred ranges are, for example, 1-3 bar (abs), 2-4 bar (abs), or 3-5 bar (abs).
[0038] According to the invention, a methanol-containing feed stream M is fed into a distillation column D. This feed stream M, also known as fresh methanol feed stream M, is fed into D to provide sufficient methanol for the entire process, particularly to compensate for methanol losses taken from the process via mixture P(i). There are generally no special requirements regarding the methanol content of M, and a skilled technician can select a suitable methanol feed stream M. However, it is preferred that the feed stream M contains only a small amount of water. Therefore, it is further preferred that 99-100% by weight, more preferably 99.5-100% by weight, and even more preferably 99.9-100% by weight of the feed stream M consists of methanol and optionally, water, wherein the amount of water contained in the feed stream M is preferably at most 2000 ppm by weight, more preferably at most 1500 ppm by weight, even more preferably at most 1000 ppm by weight, such as at most 750 ppm by weight, at most 500 ppm by weight, or at most 250 ppm by weight.
[0039] Typically, feed stream M can be fed into distillation column D at any suitable location. Preferably, feed stream M is fed into the upper part of D, more preferably at least 2, 3, or 4 theoretical stages from the top of D, even more preferably at least 4 theoretical stages from the top of D, more preferably between the 4th and 20th theoretical stages from the top of D, even more preferably between the 6th and 15th theoretical stages from the top of D, such as between the 6th and 10th theoretical stages, or between the 8th and 12th theoretical stages, or between the 10th and 14th theoretical stages, or between the 12th and 15th theoretical stages. Regarding the temperature of feed stream M fed into D below, it is preferably in the range of ambient temperature to the boiling point of methanol at the column pressure of D; more preferably, it is ambient temperature.
[0040] It is generally feasible to operate distillation column D without reflux, i.e., at a reflux ratio of 0:1. However, it is particularly preferred that distillation column D be operated under reflux. Preferably, distillation column D is operated at a reflux ratio in the range of at least 0.5:1, more preferably 0.55:1-1.4:1, and even more preferably 0.6:1-1.4:1. Suitable preferred ranges are, for example, 0.6:1-1.0:1, 0.8:1-1.2:1, or 1.0:1-1.4:1.
[0041] According to the present invention, distillation column D can operate without top vapor recompression. This is illustrated, for example, by the method of the present invention with reflux. Figure 1 , 2The diagram in section 3 provides an overview. When distillation column D is operated without top vapor recompression, achieving the desired reflux ratio preferably involves taking the top stream T(2) from the distillation column in addition to G, passing the stream T(2) through condenser V(4) to obtain liquid stream T(3) and waste stream T(2w), and returning the liquid stream T(3) to the top of distillation column D; with regard to the method feature “taking the top stream T(2) from the distillation column in addition to G”, it covers the possibility of taking two separate streams G and T(2) from the top of D and taking a single stream from the top of D and splitting the single stream into two streams G and T(2). Alternatively, in the case where distillation column D is operating without top vapor recompression, it may be preferable to achieve the desired reflux ratio by taking the top feed stream T(2) from the distillation column in addition to G, passing the feed stream T(2) through condenser V(4) to obtain liquid stream T(2l) and gas stream T(2g); passing the gas stream T(2g) through condenser V(5) to obtain liquid stream T(2gl) and waste gas stream T(2w); and merging the liquid streams T(2l) and (T2gl), for example, in a condensate tank, to obtain a merged liquid stream, which is then returned to the top of distillation column D as feed stream T(3); again, with regard to the method feature “taking the top feed stream T(2) from the distillation column in addition to G”, it covers the possibility of taking two separate feed streams G and T(2) from the top of D as well as taking a single feed stream from the top of D and splitting the single feed stream into two feed streams G and T(2). Of course, if necessary, skilled technicians can also achieve the reflux ratio by using more than two of the above-mentioned condensers V(4) and V(5). As for the waste gas flow T(2w), it is preferably composed of oxygen, nitrogen, carbon dioxide and methanol, wherein the amount of methanol in T(2w) is preferably in the range of 2-80% by weight based on the total weight of T(2w), more preferably in the range of 10-30% by weight.
[0042] Especially considering the overall energy consumption, it is likely preferable that distillation column D is operated with top vapor recompression. For example, refer to the description of the method of the present invention with reflux. Figure 4 , 5 The diagram in section 6 provides an overview. In cases where the distillation column operates with top vapor recompression, achieving this reflux ratio preferably includes:
[0043] (i) Take the top stream T(2) from the distillation column D in addition to G, and pass the stream T(2) through the condenser V(4) to obtain a liquid stream and a waste stream T(2w); As far as the method feature “take the top stream T(2) from the distillation column in addition to G” is concerned, it covers the possibility of taking out two separate streams G and T(2) from the top of D and taking out a single stream from the top of D and splitting the single stream into two streams G and T(2);
[0044] (ii) In addition to G and T(2), another overhead stream T(1) is taken from distillation column D, and said stream T(2) is passed through compressor C(3), and the compressed stream is passed through reboiler V(6) to obtain liquid stream, wherein reboiler V(6) is preferably the reboiler of distillation column D; with regard to the method feature “in addition to G and T(2), another overhead stream T(1) is taken from the distillation column”, it covers taking three separate streams G and T(2) from the top of D and taking a single stream from the top of D and dividing said single stream into three streams G and T(2) and T(1) and taking two separate streams from the top of D.
[0045] And appropriately divide the two material flows into material flows G, T(2) and T(1);
[0046] (iii) The liquid flow obtained according to (i) and (ii) is fed into the top of the distillation column D.
[0047] Of course, for the purposes of step (i) above, a skilled technician may also achieve the reflux ratio by using more than one of the aforementioned condensers V (4), if necessary. A preferred implementation using two condensers V (4) and V (5) is described below.
[0048] When the distillation column is operated under top vapor recompression, it is also preferable to achieve the reflux ratio by: (i) taking the top feed stream T(2) from the distillation column D in addition to G, passing the feed stream T(2) through the condenser V(4) to obtain a liquid stream T(2l) and a gas stream T(2g); passing the gas stream T(2g) through the condenser V(5) to obtain a liquid stream T(2gl) and a waste gas stream T(2w); and merging the liquid stream T(2l) and (T2gl) by, for example, in a condensate tank to obtain a merged liquid stream T(2cl); with regard to the method feature "taking the top feed stream T(2) from the distillation column in addition to G", it covers taking two separate feed streams G and T(2) from the top of D and taking a single feed stream from the top of D and dividing the single feed stream into two
[0049] The probability of stock flow G and T(2);
[0050] (ii) In addition to G and T(2), another overhead stream T(1) is taken from distillation column D, and said stream T(2) is passed through compressor C(3), and the compressed stream is passed through reboiler V(6) to obtain a liquid stream, wherein reboiler V(6) is preferably the reboiler of distillation column D; with regard to the method feature “in addition to G and T(2), another overhead stream T(1) is taken from the distillation column”, it covers taking three separate streams G and T(2) from the top of D and taking a single stream from the top of D and dividing said single stream into three streams G and T(2) and T(1) and taking two separate streams from the top of D and appropriately The possibility of dividing the two streams into streams G, T(2), and T(1); according to the method of the invention, it is likely preferred to first feed the liquid stream obtained from the reboiler V(6) into the condensate from which the gas stream T(1g) and liquid stream T(1l) have been removed, wherein the gas stream T(1g) may, for example, contain one or more inert components; for example, the liquid stream T(1g) may be fed into the condenser (V4) or V(5), preferably V(4), wherein the liquid stream T(1l) is preferably combined with the liquid streams T(2l) and (T2gl), for example, in a condensate tank, preferably in the condensate tank described in step (i) above; refer to the following
[0051] Step (iii);
[0052] (iii) The combined liquid stream obtained according to (i) and the liquid stream obtained according to (ii) are fed into the top of the distillation column D.
[0053] Of course, for the above step (i), skilled technicians may also achieve the reflux ratio by using more than two condensers V (4) and V (5) if needed.
[0054] As described above, preferred (ii) further includes feeding the liquid stream obtained from the reboiler V (6) into a condensate tank, wherein a gas stream T (1g) and a liquid stream T (1l) are taken from the condensate tank, the gas stream T (1g) is fed into the condenser V (4), and the liquid stream T (1l) is fed into the liquid stream obtained according to (ii), wherein more preferably, the liquid stream is depressurized before being fed into the top of the distillation column D according to (iii). Preferably, (iii) includes combining the liquid streams obtained according to (i) and (ii) to obtain a liquid stream T (3) and feeding the feed stream T (3) into the top of the distillation column D.
[0055] Regarding the exhaust gas flow T(2w), it is preferably composed mainly of oxygen, nitrogen, carbon dioxide and methanol, wherein the amount of methanol in T(2w) is preferably in the range of 2-80% by weight based on the total weight of T(2w), more preferably in the range of 10-30% by weight.
[0056] According to (ii), the preferred reboiler V(6) is, for example, as Figure 4 , 5Figure 6 shows the intermediate reboiler of distillation column D. It is also generally feasible that the reboiler V(6) downstream of compressor C(3) is not used as an intermediate reboiler, but rather configured to provide heat to the bottom of column D. In this case, it is advantageous to equip column D with another bottom reboiler instead of V(3) or together with a smaller reboiler V(3), wherein the additional reboiler is preferably smaller in size than V(3) or V(6), and wherein this additional reboiler is primarily used for starting distillation column D. During the normal operating mode of column D, it is feasible to shut down the additional reboiler.
[0057] For the feed stream G provided according to (a) obtained by distillation according to (d.2), preferably the feed stream G comprises methanol and water, wherein more preferably 99.95-100% by weight of G consists of methanol and water and wherein the water content of G is at most 200 ppm by weight, more preferably at most 150 ppm by weight, more preferably at most 100 ppm by weight, wherein more preferably the water content is in the range of 5-100 ppm by weight, more preferably 10-100 ppm by weight, more preferably in the range of 15-100 ppm by weight.
[0058] According to (b), it is preferable to divide the material flow G into two flow streams G(1) and G(2), wherein flow G has a mass flow rate f(G), flow G(1) has a mass flow rate f(G(1)) and flow G(2) has a mass flow rate f(G(2)), where f(G) = f(G(1)) + f(G(2)). Flow G can typically be divided by any feasible method. Preferably, the division according to (b) involves feeding flow G into a diversion device S, which more preferably includes a pipe fitting. In this context, it should be noted that the term "dividing the material flow into two flow streams" refers to a method according to which the flow obtained from the division has the same chemical composition as flow G. With regard to the ratios f(G(1)) / f(G) and f(G(2)) / f(G), the present invention allows for flexible adjustment of the ratios, as the individual flow rates f(G(1)) and f(G(2)) can be selected depending on the required amount of A(2)OMe, preferably potassium methoxide, obtained according to (c.2.2), and the required amount of A(1)OMe, preferably sodium methoxide, obtained according to (c.1.2).
[0059] Before the split according to (b), the feed stream G can be passed through the compressor C, thereby increasing the pressure of G. Preferably, the pressure is increased appropriately so that the pressure of the feed stream after splitting is adapted to the pressure required when the feed stream is fed into the reactive distillation column K(i) and finally returned to D via feed stream W(i). Preferably, the pressure increase is in the range of 0.1-0.8 bar (abs), more preferably 0.15-0.6 bar (abs), and even more preferably 0.2-0.4 bar (abs). According to this embodiment of the invention, the split according to (b) preferably includes feeding the compressed feed stream G into a splitting device S, which preferably includes a pipe joint and at least one control device to allow adjustment of the ratio f(G(1)) / f(G(2)), wherein the at least one control device is located downstream of the pipe joint. At least one of these control devices is located in feed stream G(1), or in feed stream G(2), or in both feed streams G(1) and G(2), and preferably, the at least one control device is a control valve.
[0060] According to the invention, the aforementioned pressure increase is preferably achieved not by compressing the feed stream G before segmentation, but by compressing the feed stream G after segmentation. Therefore, according to the invention, it is preferable to pass the feed stream G(1) through the compressor C(1) before feeding it into the reactive distillation column K(1), thereby achieving a pressure increase of G(1) in the range of 0.1-0.8 bar (abs), preferably 0.15-0.6 bar (abs), more preferably 0.2-0.4 bar (abs). Of course, the compression of G(1) can be combined with the pre-compression of the feed stream G before segmentation; however, it is preferable that this compression of G(1) is carried out without compression of G before segmentation according to (b). Therefore, it is also preferable to pass the feed stream G(2) through the compressor C(2) before feeding it into the reactive distillation column K(2), thereby achieving a pressure increase of G(2) in the range of 0.1-0.8 bar (abs), preferably 0.15-0.6 bar (abs), more preferably 0.2-0.4 bar (abs). Of course, the compression of G(2) can be combined with the pre-compression of the material flow G before the split; however, it is preferable that the compression of G(2) is performed without the compression of G before the split according to (b).
[0061] Regarding the feed stream H(1), preferably 99-100% by weight, more preferably 99.5-100% by weight, and even more preferably 99.9-100% by weight, the feed stream H(1) is composed of Al(1)OH and water, wherein more preferably 37.5-58% by weight, more preferably 40-55% by weight, and even more preferably 42.5-52% by weight, the feed stream H(1) is composed of Al(1)OH, preferably sodium hydroxide. The feed stream H(1) is preferably fed into the reactive distillation column K(1) at a temperature ranging from ambient temperature to its boiling point, more preferably 50-80°C, such as 50-60°C, 60-70°C, or 70-80°C. Heating the feed stream H(1) to this temperature can be achieved using any suitable device such as a heat exchanger. The feed stream H(1) is preferably fed to the top of the reactive distillation column K(1), more preferably to the first theoretical stage from the top.
[0062] For the reactive distillation column K(1), it is preferred that the column has 5-50, more preferably 10-40, and even more preferably 15-30 theoretical stages, such as 15-20, 20-25, or 25-30 theoretical stages. The feed stream G(1) can generally be fed into K(1) at any suitable location; preferably, G(1) is fed into the reactive distillation column K(1) between the bottom and the 5th theoretical stage, more preferably between the bottom and the 3rd theoretical stage, and even more preferably between the bottom and the 2nd theoretical stage. The reactive distillation column K(1) is preferably operated at a top pressure in the range of 0.5-10 bar (abs), more preferably 1-6 bar (abs), and even more preferably 1-5 bar (abs). Suitable preferred ranges are, for example, 1-3 bar (abs), 2-4 bar (abs), or 3-5 bar (abs). Although reactive distillation column K(1) can generally be operated under reflux, it is preferred to operate reactive distillation column K(1) under a reflux ratio of 0:1.
[0063] Regarding the feed stream W(1) obtained from the top of K(1), preferably 99-100% by weight, more preferably 99.5-100% by weight, and even more preferably 99.9-100% by weight of W(1) is composed of methanol and water. More preferably 1-10% by weight, more preferably 2-8% by weight, more preferably 4-7% by weight, and even more preferably 5-6% by weight of the feed stream W(1) is composed of water.
[0064] For the mixture P(1), preferably 99-100% by weight, more preferably 99.5-100% by weight, and even more preferably 99.9-100% by weight of the feed stream P(1) consists of A(1)OMe, preferably sodium methoxide, and methanol. More preferably 10-50% by weight, more preferably 20-40% by weight, and even more preferably 25-35% by weight of the feed stream P(1) consists of A(1)OMe, preferably sodium methoxide. More preferably up to 5000 ppm by weight, more preferably up to 2000 ppm by weight, and even more preferably up to 1000 ppm by weight of the feed stream P(1) consists of water. The maximum feasible water content may, for example, include 750 ppm by weight, 500 ppm by weight, or 250 ppm by weight. The concentration of A(1)OMe, preferably sodium methoxide, in the feed stream P(1) is preferably achieved by a skilled technician by operating the reactive distillation column K(1) at the appropriate reboiler load.
[0065] According to the invention, the top of the reactive distillation column K(1) is preferably equipped with a suitable droplet separation device D(1), preferably a demister. Therefore, the method preferably includes separating droplets containing A(1)OH, preferably sodium hydroxide, from the vapor stream at the top of K(1). Further preferably, especially for cleaning purposes, the demister is suitably treated with a suitable stream M(1). Preferred treatment may include at least temporarily spraying the demister with stream M(1), preferably using it. Regarding the chemical composition of M(1), it is particularly preferred that M(1) contains methanol, more preferably M(1) is bisected from the overhead stream of the condenser taken from the distillation column D, such as one of the aforementioned streams, or preferably a fresh methanol stream, such as a stream bisected from the aforementioned stream M.
[0066] Regarding the feed stream H(2), preferably 99-100% by weight, more preferably 99.5-100% by weight, and even more preferably 99.9-100% by weight, the feed stream H(2) is composed of A(2)OH, preferably potassium hydroxide, and water, wherein more preferably 30-55% by weight, more preferably 40-52.5% by weight, and even more preferably 45-50% by weight, the feed stream H(2) is composed of A(2)OH, preferably potassium hydroxide. The feed stream H(2) is preferably fed into the reactive distillation column K(2) at a temperature ranging from ambient temperature to its boiling point, more preferably 50-80°C, such as 50-60°C, 60-70°C, or 70-80°C. Heating the feed stream H(2) to this temperature can be achieved using any suitable device such as a heat exchanger. The feed stream H(2) is preferably fed to the top of the reactive distillation column K(2), more preferably to the first theoretical stage from the top.
[0067] For the reactive distillation column K(2), it is preferred that the column has 5-50, more preferably 10-40, and even more preferably 15-30 theoretical stages, such as 15-20, 20-25, or 25-30 theoretical stages. The feed stream G(2) can generally be fed into K(2) at any suitable location; preferably, G(2) is fed into the reactive distillation column K(2) between the bottom and the 5th theoretical stage, more preferably between the bottom and the 3rd theoretical stage, and even more preferably between the bottom and the 2nd theoretical stage. The reactive distillation column K(2) is preferably operated at a top pressure in the range of 0.5-10 bar (abs), more preferably 1-6 bar (abs), and even more preferably 1-5 bar (abs). Suitable preferred ranges are, for example, 1-3 bar (abs), 2-4 bar (abs), or 3-5 bar (abs). Although the reactive distillation column K(2) can generally be operated under reflux, it is preferred to operate the reactive distillation column K(2) at a reflux ratio of 0:1.
[0068] Regarding the feed stream W(2) obtained from the top of K(2), preferably 99-100% by weight, more preferably 99.5-100% by weight, and even more preferably 99.9-100% by weight of W(2) is composed of methanol and water. More preferably 1-15% by weight, more preferably 2-12% by weight, and even more preferably 6-10% by weight of the feed stream W(2) is composed of water.
[0069] Regarding the mixture P(2), preferably 99-100% by weight, more preferably 99.5-100% by weight, and even more preferably 99.9-100% by weight of the feed stream P(2) consists of A(2)OMe, preferably potassium methoxide, and methanol. More preferably 10-50% by weight, more preferably 20-40% by weight, and even more preferably 25-35% by weight of the feed stream P(2) consists of A(2)OMe, preferably potassium methoxide. More preferably up to 5000 ppm by weight, more preferably up to 2000 ppm by weight, and even more preferably up to 1000 ppm by weight of the feed stream P(2) consists of water. The maximum feasible water content may, for example, include 750 ppm by weight, 500 ppm by weight, or 250 ppm by weight. The concentration of A(2)OM, preferably potassium methoxide, in the feed stream P(2) is preferably achieved by a skilled technician by operating the reactive distillation column K(2) at the appropriate reboiler load.
[0070] According to the invention, the top of the reactive distillation column K(2) is preferably equipped with a suitable droplet separation device D(2), preferably a demister. Therefore, the method preferably includes separating droplets containing A(2)OH, preferably potassium hydroxide, from the vapor stream at the top of K(2). Further preferably, especially for cleaning purposes, the demister is suitably treated with a suitable stream M(2). Preferred treatment may include at least temporarily spraying the demister with stream M(2), preferably using it. Regarding the chemical composition of M(2), it is particularly preferred that M(2) contains methanol, more preferably M(2) is bifurcated from the overhead stream of the condenser taken from the distillation column D, such as one of the aforementioned streams, or preferably a fresh methanol stream, such as a stream bifurcated from the aforementioned stream M.
[0071] As described above, according to the invention, the feed stream G is passed through compressor C before splitting, and / or the feed stream G(1) is passed through compressor C(1) and the feed stream G(2) is passed through compressor C(2) after splitting, preferably the latter. According to the invention, in addition to at least one of the above-described schemes or preferably as the only corresponding compression, the feed stream W(1) is passed through compressor C(1) before being fed into distillation column D, thereby achieving a pressure increase of W(1) preferably in the range of 0.1-0.8 bar (abs), more preferably 0.15-0.6 bar (abs), more preferably 0.2-0.4 bar (abs), and the feed stream W(2) is passed through compressor C(2) before being fed into distillation column D, thereby achieving a pressure increase of W(2) in the range of 0.1-0.8 bar (abs), more preferably 0.15-0.6 bar (abs), more preferably 0.2-0.4 bar (abs). According to this embodiment of the invention, the material flows W(1) and W(2) can also be appropriately combined in a merging device before passing through the compressor to obtain a corresponding merged material flow W, and the merged material flow W is passed through the compressor before being fed into D, thereby achieving a pressure increase of W(1) preferably in the range of 0.1-0.8 bar (abs), more preferably 0.15-0.6 bar (abs), and even more preferably 0.2-0.4 bar (abs). The merging device preferably includes a pipe fitting and at least one control device, preferably a control valve.
[0072] Regarding the integrated method of the present invention, it should be noted that, in addition to the two mixtures P(1) and P(2) described in detail above, any details of operating the corresponding additional compressors, reactive distillation columns, etc., can be readily derived from the above-described details by a skilled person based on their general knowledge in order to simultaneously prepare a third mixture P(3) and / or a fourth mixture P(4) and / or a fifth mixture P(5), etc. According to the present invention, it is particularly preferred that the method of the present invention is an integrated method for simultaneously preparing three mixtures P(1), P(2), and P(3), wherein mixture P(1) comprises sodium methoxide and methanol, mixture P(2) comprises potassium methoxide and methanol, and mixture P(3) comprises lithium methoxide and methanol, the method comprising:
[0073] (a) Provide a feed stream G containing methanol;
[0074] (b) The material flow G is divided into three material flows G(1), G(2) and G(3), and G(1), G(2) and G(3) have
[0075] Same composition as G;
[0076] (c.1) Preparation of sodium methoxide, including:
[0077] (c.1.1) Feed stream G(1) into the lower part of reactive distillation column K(1) and feed aqueous liquid stream H(1) containing dissolved sodium hydroxide into the upper part of reactive distillation column K(1);
[0078] (c.1.2) G(1) and H(1) are subjected to reactive distillation conditions in K(1) to obtain a top stream W(1) containing methanol and water; and a bottom stream P(1) containing sodium methoxide and methanol.
[0079] (c.2) Preparation of potassium methoxide, including:
[0080] (c.2.1) Feed stream G(2) into the lower part of reactive distillation column K(2), wherein K(2) is arranged parallel to K(1) and aqueous liquid stream H(2) containing dissolved potassium hydroxide is fed into the upper part of reactive distillation column K(2);
[0081] (c.2.2) G(2) and H(2) are subjected to reactive distillation conditions in K(2) to obtain a top stream W(2) containing methanol and water; and a bottom stream P(2) containing potassium methoxide and methanol.
[0082] (c.3) Preparation of lithium methoxide, including:
[0083] (c.3.1) Feed stream G(3) into the lower part of reactive distillation column K(3), wherein K(3) is arranged parallel to K(1) and K(2) and aqueous liquid stream H(3) containing dissolved lithium hydroxide is fed into the upper part of reactive distillation column K(3);
[0084] (c.3.2) G(3) and H(3) are subjected to reactive distillation conditions in K(3) to obtain a top stream W(3) containing methanol and water; and a bottom stream P(3) containing lithium methoxide and methanol.
[0085] (d.1) Feed W(1), W(2) and W(3) into the lower part of distillation column D, and feed containing methanol into the column.
[0086] Flow M is fed into distillation column D;
[0087] (d.2) Subject W(1), W(2), W(3) and M to distillation conditions in D, and obtain the overhead feed as the product.
[0088] According to (a), the material flow G.
[0089] In particular, regarding steps (c.3) including (c.3.1) and (c.3.2), steps (d.1) and (d.2) concerning W(3), a skilled person, based on their general knowledge, can also directly derive the operation of the corresponding additional compressors, such as C(3) similar to C(1) and C(2), the additional reactive distillation column K(3)—including, for example, additional droplet separation devices, preferably a demister, and the preferred additional feed stream M(3)—similar to any details of M(1) and M(2), etc. At least two of the feed streams W(1), W(2) and W(3) can be appropriately combined before being fed into D.
[0090] According to the invention, it is also feasible to separate A(i)OMe at least partially from methanol from at least one feed stream P(i), more preferably to obtain solid A(i)OMe, and even more preferably crystalline A(i)OMe. Thus, solid sodium methoxide, preferably crystalline sodium methoxide, and solid potassium methoxide, preferably crystalline potassium methoxide, can be obtained. According to the above-described method for preparing the two mixtures P(i) therein, it is also preferable that solid lithium methoxide, preferably crystalline lithium methoxide, can be obtained in addition.
[0091] The present invention further relates to a chemical production apparatus for implementing the method of the present invention, comprising:
[0092] - Distillation column D, including:
[0093] --Used to feed material flow M into D, preferably into the upper inlet device of D;
[0094] --At its lower part is an inlet for feeding the material flow W(i) or one or more of its combined material flows into D.
[0095] Device;
[0096] --An outlet device for removing material flow T(2) and G or their combined material flow from the top of D;
[0097] --At least one condenser, preferably condenser V(4) and optionally another condenser V(5) arranged downstream of V(4), having an inlet device for receiving the feed stream T(2) and having a means for taking
[0098] The outlet device for the condensate flow T(3) and the outlet device for the waste gas flow;
[0099] -- An inlet device for feeding the material flow T(3) into the top of D;
[0100] --Bottom reboiler;
[0101] - A diversion device S for dividing a material flow G into n material flows G(i);
[0102] - A device for feeding the material flow G into the diversion device S;
[0103] -n reactive distillation columns K(i), n≥2 and i=1…n; each reactive distillation column K(i) includes:
[0104] --At its upper part, preferably at its top, is an inlet device for feeding the material flow H(i) into K(i);
[0105] --At its lower part is the inlet device for feeding the material flow G(i) into K(i);
[0106] --An outlet device for removing the material flow W(i) from the top of K(i);
[0107] --Bottom reboiler;
[0108] --An outlet device for removing the bottom flow from K(i);
[0109] --A flow divider for separating the material flow P(i) from the bottom material flow taken out from K(i);
[0110] - A device for feeding the feed stream G(i) into the reactive distillation column K(i);
[0111] - A device for feeding the feed stream W(i) into the distillation column D;
[0112] - One or more compressors C(i) for compressing material flow G and / or material flow G(i) and / or material flow W(i).
[0113] Preferably, at least one, more preferably, each reactive distillation column K(i) is equipped with a droplet separator D(i) at its top, and more preferably, a demister, the demister more preferably including an inlet device for feeding a methanol-containing feed stream M(i) into the demister. Preferably, each reactive distillation column K(i) independently comprises 5-50, more preferably 10-40, and more preferably 15-30 theoretical stages. Preferably, the device for feeding the feed stream G(i) into the reactive distillation column K(i) is independently located at the bottom of K(i) and the fifth theoretical stage, more preferably the bottom of K(i) and the third theoretical stage, and more preferably between the bottom of K(i) and the second theoretical stage. Preferably, the device for feeding the feed stream H(i) into the reactive distillation column K(i) is located at the top of K(i), preferably the uppermost theoretical stage. Preferably, at least one, more preferably, each reactive distillation column K(i) does not include a device for operation at a reflux ratio greater than 0:1. Preferably, each reactive distillation column K(i) is equipped with trays.
[0114] Preferably, the apparatus of the present invention comprises n compressors C(i) arranged upstream of K(i) for compressing the material flow G(i). Alternatively, the apparatus of the present invention preferably comprises n compressors C(i) arranged downstream of K(i) and upstream of D for compressing the material flow W(i).
[0115] For distillation column D, it is preferred that the column has 20-100, more preferably 30-80, and even more preferably 40-60 theoretical stages. Preferably, the inlet device for feeding stream W(i) or one or more of its combined streams into D is located between the bottom of D and the 15th theoretical stage, more preferably between the bottom of D and the 10th theoretical stage, and even more preferably between the bottom of D and the 8th theoretical stage. Preferably, the inlet device for feeding stream M into D is located at least 4 theoretical stages from the top of D, more preferably between the 4th and 20th theoretical stages from the top of D, and even more preferably between the 6th and 15th theoretical stages from the top of D.
[0116] Preferably, the apparatus of the present invention further includes at least one condensate tank for the liquid stream taken from V(4) and optionally V(5), and further includes means for feeding at least a portion of the liquid contained in the tank as a feed stream T(3) into the top of D. More preferably, the apparatus of the present invention further includes means for recompressing the top vapor obtained from D, the means more preferably including a compressor C(3) for compressing the feed stream T(1) taken from the top of D, means for feeding T(1) from the top of D into C(3), a reboiler V(6) for condensing the compressed feed stream, means for feeding the compressed feed stream from (C3) into V(6), and means for supplying the resulting liquid stream into the top of D. Preferably, the reboiler V(6) is a reboiler of D, more preferably an intermediate reboiler of D. Further preferred distillation column D is equipped with trays and / or packing, wherein in the case where reboiler V(6) is the reboiler of D, D is more preferably equipped with packing arranged above the intermediate reboiler of D and trays arranged below the intermediate reboiler of D.
[0117] In the context of this invention, it is also feasible for suitable reactive distillation columns K(i) to be essentially bubble cap tray, valve tray, and sieve tray columns. Particularly in the case of valve trays and sieve trays, the trays should be constructed to minimize raining-through of the liquid. Those skilled in the art are well aware of the required structural measures. Choosing particularly tight-closing valve types and thus particularly increasing the vapor velocity entering the tray openings to double the normally set value is achieved by reducing the number of valves. In the case of sieve trays, it is particularly useful to reduce the diameter of the openings in the tray and maintain or even increase the number of openings. It is also feasible to provide the column with either random packing elements or structured packing, with structured packing being superior to random packing elements from the perspective of uniform liquid distribution. In all sub-regions corresponding to more than 2% of the total column cross-section, the average ratio of liquid flow to vapor flow must not exceed 15%, preferably not more than 3%. Maintaining such a low liquid volume allows the capillary effect on the wire mesh to prevent local peaks in the liquid droplet density.
[0118] According to the invention, the apparatus preferably further includes at least one condensate tank for the condensate stream taken out from V(6), and more preferably further includes means for feeding at least a portion of the gas phase in the tank into V(4) and means for feeding at least a portion of the liquid phase in the tank into the condensate tank as defined above.
[0119] Furthermore, it is likely preferred that the apparatus further include means for separating alkali metal methoxide A(i)OMe from at least one feed stream P(i).
[0120] The number n of the reactive distillation column K(i) is preferably in the range of 2-10, more preferably in the range of 2-5, more preferably 2 or 3, and more preferably 2.
[0121] The present invention further relates to the use of the chemical production apparatus or method of the present invention in the simultaneous production of n mixtures P(i) comprising alkali metal ethanol salts and methanol, where n is an integer, n≥2 and i=1…n, wherein at least two of the mixtures P(i) comprise different alkali metal ethanol salts A(i)OMe, and / or at least two of the mixtures P(i) comprise the same alkali metal alkoxide A(i)OMe at different concentrations.
[0122] The present invention is further illustrated by the following set of embodiments and combinations of embodiments derived from the shown dependencies and retrospective references. It is particularly noteworthy that in the various instances where a range of embodiments is mentioned, for example with the term "the method of any one of embodiments 1-4," it is intended to explicitly disclose to a skilled person that each embodiment within that range is synonymous with "the method of any one of embodiments 1, 2, 3, and 4."
[0123] Furthermore, it should be clearly noted that the following set of embodiments is not the same as the claims that define the scope of protection, but rather represents appropriate components of the specification relating to the general and preferred aspects of the invention.
[0124] 1. An integrated method for simultaneously preparing n mixtures P(i) comprising alkali metal methoxides and methanol, comprising:
[0125] Provide n reactive distillation columns K(i);
[0126] Provide n aqueous liquid streams H(i), where each stream H(i) contains dissolved alkali metal hydroxide A(i)OH, and n is an integer, where n ≥ 2 and i = 1…n; and
[0127] Provide distillation column D;
[0128] The method further includes:
[0129] (a) Provide a feed stream G containing methanol;
[0130] (b) Divide the material flow G into n material flows G(i), each material flow G(i) having the same composition as G;
[0131] (c) Preparing the one or more alkali metal methanol salts, comprising:
[0132] Each feed stream G(i) is fed into the lower part of the corresponding reactive distillation column K(i), and an aqueous liquid stream H(i) containing dissolved alkali metal hydroxide A(i)OH is fed into the upper part of the reactive distillation column K(i); and
[0133] G(i) and H(i) are subjected to reactive distillation conditions in each K(i) to obtain n overhead feed streams W(i) containing methanol and water; and n streams containing alkali metal methanol salt A(i)OMe and methanol are obtained.
[0134] The bottom material flow P(i);
[0135] (d) Feed each feed stream W(i) into the lower part of the distillation column D, and feed the feed stream M containing methanol into
[0136] In distillation column D; and subjecting the n streams W(i) and M to distillation conditions in D to obtain the stream G as the top stream according to (a).
[0137] 2. The method of implementation scheme 1, wherein n is in the range of 2-10, preferably 2-5, more preferably 2 or 3, and even more preferably 2;
[0138] 3. The method of embodiment 1 or 2, wherein each alkali metal hydroxide A(i)OH is preferably selected from lithium hydroxide, sodium hydroxide and potassium hydroxide, more preferably from sodium hydroxide and potassium hydroxide.
[0139] 4. The method of any one of embodiments 1-3, wherein at least two alkali metal hydroxides A(i)OH are different from each other, wherein preferably, especially if n is 2 or 3, all alkali metal hydroxides A(i)OH are different from each other.
[0140] 5. The method of any one of embodiments 1-4, wherein the given liquid flow H(i) comprises an alkali metal hydroxide A(i)OH dissolved in water, methanol or a mixture of water and methanol, preferably dissolved in water.
[0141] 6. The method of any one of embodiments 1-5, being an integrated method for simultaneously preparing at least two, preferably two, mixtures P(i), wherein mixture P(1) comprises A(1)OMe, preferably sodium methoxide, and methanol, and mixture P(2) comprises A(2)OMe, preferably potassium methoxide, and methanol, the method comprising:
[0142] (a) Provide a feed stream G containing methanol;
[0143] (b) Divide the material flow G into at least two material flows G(1) and G(2), G(1) and G(2) having the same characteristics as G.
[0144] Composition;
[0145] (c.1) Preparation of A(1)OMe, including:
[0146] (c.1.1) Feed stream G(1) is fed into the lower part of reactive distillation column K(1), and liquid stream H(1), preferably aqueous liquid stream H(1), is fed into the upper part of reactive distillation column K(1), wherein H(1) contains dissolved A(1)OH, preferably sodium hydroxide;
[0147] (c.1.2) G(1) and H(1) are subjected to reactive distillation conditions in K(1) to obtain a top stream W(1) containing methanol and water; and a bottom stream P(1) containing A(1)OMe and methanol.
[0148] (c.2) Preparation of A(2)OMe, including:
[0149] (c.2.1) Feed stream G(2) is fed into the lower part of reactive distillation column K(2), wherein K(2) is arranged parallel to K(1), and liquid stream H(2), preferably aqueous liquid stream H(2), is fed into the upper part of reactive distillation column K(2), wherein H(2) contains dissolved A(2)OH, preferably potassium hydroxide;
[0150] (c.2.2) G(2) and H(2) are subjected to reactive distillation conditions in K(2) to obtain a top stream W(2) containing methanol and water; and a bottom stream P(2) containing A(2)OMe and methanol.
[0151] (d.1) Feed W(1) and W(2) into the lower part of the distillation column D, and feed the methanol-containing stream M into the lower part of the column D.
[0152] It enters distillation column D;
[0153] (d.2) subject W(1), W(2) and M to distillation conditions in D to obtain the feed stream G according to (a) as the overhead feed stream.
[0154] 7. The method of implementation 6, wherein W(1) and W(2) are supplied as gas streams into distillation column D, preferably at the bottom of distillation column D and the 15th theoretical stage, more preferably at the bottom of the column and the 10th theoretical stage, and more preferably at the position between the bottom of the column and the 8th theoretical stage.
[0155] 8. The method of any one of the embodiments 1-7, wherein the distillation column D has 20-100, preferably 30-80, and more preferably 40-60 theoretical stages.
[0156] 9. The method of any one of embodiments 1-8, wherein the distillation column D is operated at a top pressure in the range of 0.5-10 bar (abs), preferably 0.75-6 bar (abs), more preferably 1-5 bar (abs).
[0157] 10. The method of any one of embodiments 1-9, wherein 99-100% by weight, preferably 99.5-100% by weight, more preferably 99.9-100% by weight, of the feed stream M is composed of methanol and optionally, water, wherein the amount of water contained in the feed stream M is at most 2000 ppm by weight, more preferably at most 1500 ppm by weight, and more preferably at most 1000 ppm by weight.
[0158] 11. The method of any one of embodiments 1-10, wherein the feed stream M is fed into the upper part of D, preferably at least 4 theoretical stages from the top of D, more preferably between the 4th and 20th theoretical stages from the top of D, more preferably between the 6th and 15th theoretical stages from the top of D, preferably at the temperature of M in the range of ambient temperature to the boiling point of methanol at the tower pressure of D, more preferably at ambient temperature.
[0159] 12. The method of any one of embodiments 1-11, wherein the distillation column D is operated with a reflux ratio of at least 0.5:1, preferably in the range of 0.55:1-1.4:1, more preferably in the range of 0.6:1-1.4:1.
[0160] 13. The method of implementation scheme 12, wherein the distillation column D is operated without top vapor recompression.
[0161] 14. The method of implementation scheme 13, wherein achieving the reflux ratio includes taking the top feed stream T(2) from the distillation column except for G, passing the feed stream T(2) through the condenser V(4) to obtain the liquid stream T(3) and the waste gas stream T(2w), and feeding the liquid stream T(3) into the top of the distillation column D.
[0162] 15. The method of implementation scheme 13, wherein achieving the reflux ratio includes taking the top feed stream T(2) from the distillation column except for G, passing the feed stream T(2) through the condenser V(4) to obtain a liquid stream T(2l) and a gas stream T(2g); passing the gas stream T(2g) through the condenser V(5) to obtain a liquid stream T(2gl) and a waste gas stream T(2w); and merging the liquid stream T(2l) and (T2gl) to obtain a merged liquid stream, and feeding the latter as feed stream T(3) into the top of the distillation column D.
[0163] 16. The method of embodiment 14 or 15, wherein the waste gas stream T(2w) is basically composed of oxygen, nitrogen, carbon dioxide and methanol, wherein the amount of methanol in T(2w) is preferably in the range of 2-80% by weight, more preferably 10-30% by weight, based on the total weight of T(2w).
[0164] 17. The method of implementation scheme 12, wherein the distillation column is operated under top vapor recompression.
[0165] 18. The method of implementation scheme 17, wherein achieving the reflux ratio includes:
[0166] (i) Take the top feed stream T(2) from the distillation column D except for G, and pass the feed stream T(2) through the condenser.
[0167] V(4), to obtain liquid flow and waste gas flow T(2w);
[0168] (ii) In addition to G and T(2), another overhead stream T(1) is taken from distillation column D, and this stream T(2) is passed through compressor C(3). The compressed stream is then passed through reboiler V(6) to obtain a liquid stream, which...
[0169] The reboiler V(6) is preferably the reboiler of the distillation column D;
[0170] (iii) The liquid flow obtained according to (i) and (ii) is fed into the top of the distillation column D.
[0171] 19. The method of implementation scheme 17, wherein achieving the reflux ratio includes:
[0172] (i) Except for G, the top feed stream T(2) is taken from the distillation column D, and the feed stream T(2) is passed through the condenser V(4) to obtain liquid stream T(2l) and gas stream T(2g); the gas stream T(2g) is passed through the condenser V(5) to obtain liquid stream T(2gl) and waste gas stream T(2w); and the liquid stream T(2l) and (T2gl) are combined to obtain a combined...
[0173] The fluid flow T(2cl);
[0174] (ii) In addition to G and T(2), another overhead stream T(1) is taken from distillation column D, and this stream T(2) is passed through compressor C(3). The compressed stream is then passed through reboiler V(6) to obtain a liquid stream, which...
[0175] The reboiler V(6) is preferably the reboiler of the distillation column D;
[0176] (iii) The combined liquid stream obtained according to (i) and the liquid stream obtained according to (ii) are fed into the top of the distillation column D.
[0177] 20. The method of embodiment 18 or 19, wherein the waste gas stream T(2w) is basically composed of oxygen, nitrogen, carbon dioxide and methanol, wherein the amount of methanol in T(2w) is preferably in the range of 2-80% by weight, more preferably 10-30% by weight, based on the total weight of T(2w).
[0178] 21. The method of any one of embodiments 18-20, wherein (ii) further comprises feeding the liquid stream obtained from the reboiler V (6) into a condensate tank, wherein a gas stream T (1g) and a liquid stream T (1l) are taken out from the condensate tank, the gas stream T (1g) is fed into the condenser V (4) and the liquid stream T (1l) is fed into the liquid stream obtained according to (ii), wherein the liquid stream is preferably depressurized before being fed into the top of the distillation column D according to (iii).
[0179] 22. The method of any one of embodiments 18-21, wherein (iii) includes combining the liquid streams obtained according to (i) and (ii) to obtain liquid stream T(3) and feeding the liquid stream T(3) into the top of distillation column D.
[0180] 23. The method of any one of embodiments 18-22, wherein, according to (ii), the reboiler V (6) is an intermediate reboiler of distillation column D or a bottom reboiler of distillation column D, preferably an intermediate reboiler of distillation column D.
[0181] 24. The method of any one of embodiments 1-23, wherein the feed stream G provided according to (a) by distillation according to (d.2) comprises methanol and water, wherein preferably 99.95-100% by weight of G consists of methanol and water and wherein the water content of G is at most 200 ppm by weight, preferably at most 150 ppm by weight, more preferably at most 100 ppm by weight, and more preferably in the range of 5-100 ppm by weight, more preferably 10-100 ppm by weight, and more preferably 15-100 ppm by weight.
[0182] 25. The method of any one of implementation schemes 1-24, wherein according to (b), the material flow G is divided into two material flows G(1) and G(2), wherein the material flow G has a mass flow rate f(G), the material flow G(1) has a mass flow rate f(G(1)) and the material flow G(2) has a mass flow rate f(G(2)), wherein f(G) = f(G(1)) + f(G(2)).
[0183] 26. The method of any one of embodiments 1-25, wherein the division according to (b) includes feeding the material flow G into the diversion device S, the device preferably including a pipe fitting.
[0184] 27. The method of implementation scheme 25 or 26, wherein the ratios f(G(1)) / f(G) and f(G(2)) / f(G) are adjusted according to the required amount of A(1)OMe obtained according to (c.1.2) relative to the required amount of A(2)OMe obtained according to (c.2.2).
[0185] 28. The method of any one of embodiments 1-27, wherein prior to the division according to (b), the material flow G is passed through the compressor C, thereby achieving a pressure increase of G in the range of 0.1-0.8 bar (abs), preferably 0.15-0.6 bar (abs), more preferably 0.2-0.4 bar (abs).
[0186] 29. Method 28 of the embodiment, wherein the division according to (b) includes feeding a compressed material stream G into a diversion device S, the device preferably including a pipe joint and at least one control device to allow adjustment of the ratio f(G(1)) / f(G(2)) as defined in embodiment 25, the at least one control device being located downstream of the pipe joint, wherein at least one of these control devices is located in the material stream G(1) or in the material stream G(2) or in both the material streams G(1) and G(2), wherein the at least one control device preferably includes a control valve.
[0187] 30. The method of any one of embodiments 1-29, preferably any one of embodiments 1-27, wherein the feed stream G(1) is passed through the compressor C(1) before being fed into the reactive distillation column K(1), thereby achieving an increase in pressure of G(1) in the range of 0.1-0.8 bar (abs), preferably 0.15-0.6 bar (abs), more preferably 0.2-0.4 bar (abs).
[0188] 31. The method of any one of embodiments 1-30, preferably any one of embodiments 1-27, wherein before being fed into the reactive distillation column K(2), the feed stream G(2) is passed through the compressor C(2), thereby achieving a pressure increase of G(2) in the range of 0.1-0.8 bar (abs), preferably 0.15-0.6 bar (abs), more preferably 0.2-0.4 bar (abs).
[0189] 32. The method of any one of embodiments 1-31, wherein 99-100% by weight, more preferably 99.5-100% by weight, more preferably 99.9-100% by weight, of the feed stream H(1) is composed of water and A(1)OH, wherein preferably 37.5-58% by weight, more preferably 40-55% by weight, more preferably 42.5-52% by weight, of the feed stream H(1) is composed of A(1)OH.
[0190] 33. The method of any one of embodiments 1-32, wherein the feed stream H(1) is fed into the reactive distillation column K(1) at a temperature of H(1) in the range of ambient temperature to its boiling temperature, preferably 50-80°C.
[0191] 34. The method of any one of 1-33, wherein the feed stream H(1) is fed into the top of the reactive distillation column K(1), preferably into the first theoretical stage from the top.
[0192] 35. The method of any one of embodiments 1-34, wherein the reactive distillation column K(1) has 5-50, preferably 10-40, more preferably 15-30 theoretical stages, wherein the feed stream G(1) is fed into the reactive distillation column K(1) at the bottom of the preferred reactive distillation column K(1) and the fifth theoretical stage, more preferably the bottom of the column and the third theoretical stage, more preferably between the bottom of the column and the second theoretical stage.
[0193] 36. The method of any one of embodiments 1-35, wherein the reactive distillation column K(1) is operated at a top pressure in the range of 0.5-10 bar (abs), preferably 1-6 bar (abs), more preferably 1-5 bar (abs).
[0194] 37. The method of any one of 1-36, wherein the reactive distillation column K(1) is operated at a reflux ratio of 0:1.
[0195] 38. The method of any one of embodiments 1-37, wherein 99-100% by weight, preferably 99.5-100% by weight, more preferably 99.9-100% by weight, of the feed stream W(1) is composed of methanol and water, wherein preferably 1-10% by weight, more preferably 2-8% by weight, more preferably 5-6% by weight, of the feed stream W(1) is composed of water.
[0196] 39. The method of any one of embodiments 1-38, wherein 99-100% by weight, preferably 99.5-100% by weight, more preferably 99.9-100% by weight, of the feed stream P(1) is composed of A(1)OMe and methanol, wherein 10-50% by weight, more preferably 20-40% by weight, more preferably 25-35% by weight, of the feed stream P(1) is composed of A(1)OMe, and wherein at most 5000 ppm by weight, more preferably at most 2000 ppm by weight, more preferably at most 1000 ppm by weight, of the feed stream P(1) is composed of water.
[0197] 40. The method of any one of embodiments 1-39, wherein the reactive distillation column K(1) operates at a reboiler load that allows a specific concentration of A(1)OMe to be achieved in the feed stream P(1), preferably the concentration defined in embodiment 39.
[0198] 41. The method of any one of embodiments 1-40, wherein the top of the reactive distillation column K(1) is equipped with a droplet separation device D(1), preferably a demister, the method comprising separating droplets containing A(1)OH from the vapor stream in the top of K(1).
[0199] 42. The method of implementation scheme 41 includes at least temporarily spraying the demister, preferably with a feed stream M(1) containing methanol, said feed stream preferably being a branch of the overhead feed stream from the distillation column D or a fresh methanol feed stream.
[0200] 43. The method of any one of embodiments 1-42, wherein 99-100% by weight, more preferably 99.5-100% by weight, more preferably 99.9-100% by weight, of the feed stream H(2) is composed of water and A(2)OH, wherein preferably 30-55% by weight, more preferably 40-52.5% by weight, more preferably 45-50% by weight, of the feed stream H(2) is composed of A(2)OH.
[0201] 44. The method of any one of embodiments 1-43, wherein the feed stream H(2) is fed into the reactive distillation column K(2) at a temperature of H(2) in the range of ambient temperature to its boiling temperature, preferably 50-80°C.
[0202] 45. The method of any one of embodiments 1-44, wherein the feed stream H(2) is fed into the top of the reactive distillation column K(2), preferably into the first theoretical stage from the top.
[0203] 46. The method of any one of embodiments 1-45, wherein the reactive distillation column K(2) has 5-50, preferably 10-40, more preferably 15-30 theoretical stages, wherein the feed stream G(2) is fed into the reactive distillation column K(2) at the bottom of the preferred reactive distillation column K(2) and the fifth theoretical stage, more preferably the bottom of the column and the third theoretical stage, more preferably between the bottom of the column and the second theoretical stage.
[0204] 47. The method of any one of embodiments 1-46, wherein the reactive distillation column K(2) is operated at a top pressure in the range of 0.5-10 bar (abs), preferably 1-6 bar (abs), more preferably 1-5 bar (abs).
[0205] 48. The method of any one of 1-47, wherein the reactive distillation column K(2) is operated at a reflux ratio of 0:1.
[0206] 49. The method of any one of embodiments 1-48, wherein 99-100% by weight, preferably 99.5-100% by weight, more preferably 99.9-100% by weight, of the feed stream W(2) is composed of methanol and water, wherein preferably 1-15% by weight, more preferably 2-12% by weight, more preferably 6-10% by weight, of the feed stream W(2) is composed of water.
[0207] 50. The method of any one of embodiments 1-49, wherein 99-100% by weight, preferably 99.5-100% by weight, more preferably 99.9-100% by weight, of the feed stream P(2) is composed of A(2)OMe and methanol, wherein preferably 10-50% by weight, more preferably 20-40% by weight, more preferably 25-35% by weight, of the feed stream P(2) is composed of A(2)OMe, and wherein preferably up to 5000 ppm by weight, more preferably up to 2000 ppm by weight, more preferably up to 1000 ppm by weight, of the feed stream P(2) is composed of water.
[0208] 51. The method of any one of embodiments 1-50, wherein the reactive distillation column K(2) operates at a reboiler load that allows a specific concentration of A(2)OMe to be achieved in the feed stream P(2), preferably the concentration defined in embodiment 50.
[0209] 52. The method of any one of embodiments 1-51, wherein the top of the reactive distillation column K(2) is equipped with a droplet separation device D(2), preferably a demister, the method comprising separating droplets containing A(2)OH from the vapor stream in the top of K(2).
[0210] 53. The method of implementation scheme 52 includes at least temporarily spraying the demister, preferably with a feed stream M(2) containing methanol, said feed stream preferably being a branch of the overhead feed stream from the distillation column D or a fresh methanol feed stream.
[0211] 54. The method of any one of embodiments 1-53, wherein before being fed into the distillation column D, the feed stream W(1) is passed through the compressor C(1), thereby achieving an increase in pressure of W(1) in the range of 0.1-0.8 bar (abs), preferably 0.15-0.6 bar (abs), more preferably 0.2-0.4 bar (abs).
[0212] 55. The method of any one of embodiments 1-54, wherein before being fed into the distillation column D, the feed stream W(2) is passed through the compressor C(2), thereby achieving a pressure increase of W(2) in the range of 0.1-0.8 bar (abs), preferably 0.15-0.6 bar (abs), more preferably 0.2-0.4 bar (abs).
[0213] 56. The method of embodiment 54 or 55, wherein prior to the division according to (b), the material flow G is not allowed to pass through the compressor C, preferably not through the compressor C, thereby achieving a pressure increase of G in the range of 0.1-0.8 bar (abs), preferably 0.15-0.6 bar (abs), more preferably 0.2-0.4 bar (abs).
[0214] 57. The method of any one of embodiments 54-56, wherein the feed stream G(1) is not passed through the compressor C(1) before being fed into the reactive distillation column K(1), preferably not through the compressor C(1), thereby achieving a pressure increase of G(1) in the range of 0.1-0.8 bar (abs), preferably 0.15-0.6 bar (abs), more preferably 0.2-0.4 bar (abs).
[0215] 58. The method of any one of embodiments 54-57, wherein the feed stream G(2) is not passed through the compressor C(2) before being fed into the reactive distillation column K(2), preferably not through the compressor C(2), thereby achieving a pressure increase of G(2) in the range of 0.1-0.8 bar (abs), preferably 0.15-0.6 bar (abs), more preferably 0.2-0.4 bar (abs).
[0216] 59. The method of any one of embodiments 1-58 is an integrated method for simultaneously preparing two mixtures P(i), wherein mixture P(1) contains sodium methoxide as A(1)OMe and methanol and mixture P(2) contains potassium methoxide as A(2)OMe and methanol.
[0217] 60. The method of any one of embodiments 1-58, an integrated method for simultaneously preparing three mixtures P(1), P(2) and P(3), wherein mixture P(1) contains sodium methoxide as A(1)OMe and methanol, mixture P(2) contains potassium methoxide as A(2)OMe and methanol, and mixture P(3) contains lithium methoxide as A(3)OMe and methanol, the method comprising:
[0218] (a) Provide a feed stream G containing methanol;
[0219] (b) The material flow G is divided into three material flows G(1), G(2) and G(3), and G(1), G(2) and G(3) have
[0220] Same composition as G;
[0221] (c.1) Preparation of sodium methoxide, including:
[0222] (c.1.1) Feed stream G(1) is fed into the lower part of reactive distillation column K(1), and liquid stream H(1), preferably aqueous liquid stream H(1), is fed into the upper part of reactive distillation column K(1), wherein H(1) contains dissolved sodium hydroxide.
[0223] (c.1.2) G(1) and H(1) are subjected to reactive distillation conditions in K(1) to obtain a top stream W(1) containing methanol and water; and a bottom stream P(1) containing sodium methoxide and methanol.
[0224] (c.2) Preparation of potassium methoxide, including:
[0225] (c.2.1) Feed stream G(2) is fed into the lower part of reactive distillation column K(2), wherein K(2) is arranged parallel to K(1), and liquid stream H(2), preferably aqueous liquid stream H(2), is fed into the upper part of reactive distillation column K(2), wherein H(2) contains dissolved potassium hydroxide;
[0226] (c.2.2) G(2) and H(2) are subjected to reactive distillation conditions in K(2) to obtain a top stream W(2) containing methanol and water; and a bottom stream P(2) containing potassium methoxide and methanol.
[0227] (c.3) Preparation of lithium methoxide, including:
[0228] (c.3.1) Feed stream G(3) is fed into the lower part of reactive distillation column K(3), wherein K(3) is arranged parallel to K(1) and K(2) and liquid stream H(3), preferably aqueous liquid stream H(3), is fed into the upper part of reactive distillation column K(3), wherein H(3) contains dissolved lithium hydroxide;
[0229] (c.3.2) G(3) and H(3) are subjected to reactive distillation conditions in K(3) to obtain a top stream W(3) containing methanol and water; and a bottom stream P(3) containing lithium methoxide and methanol.
[0230] (d.1) Feed W(1), W(2) and W(3) into the lower part of distillation column D, and feed containing methanol into the column.
[0231] Flow M is fed into the upper part of distillation column D;
[0232] (d.2) Subject W(1), W(2), W(3) and M to distillation conditions in D, and obtain the overhead feed as the product.
[0233] According to (a), the material flow G.
[0234] 61. The method of any one of embodiments 1-60, wherein A(i)OMe is separated from methanol at least partially from at least one feed stream P(i), preferably to obtain solid A(i)OMe, more preferably crystalline A(i)OMe.
[0235] 62. A chemical production apparatus for implementing the method according to any one of embodiments 1-61, comprising:
[0236] - Distillation column D, including:
[0237] --An inlet device used to feed material flow M into D;
[0238] --At its lower part is an inlet for feeding the material flow W(i) or one or more of its combined material flows into D.
[0239] Device;
[0240] --An outlet device for removing material flow T(2) and G or their combined material flow from the top of D;
[0241] --At least one condenser, preferably condenser V(4) and optionally another condenser V(5) arranged downstream of V(4), having an inlet device for receiving the feed stream T(2) and having a means for taking
[0242] The outlet device for the condensate flow T(3) and the outlet device for the waste gas flow;
[0243] -- An inlet device for feeding the material flow T(3) into the top of D;
[0244] --Bottom reboiler;
[0245] - A diversion device S for dividing a material flow G into n material flows G(i);
[0246] - A device for feeding the material flow G into the diversion device S;
[0247] -n reactive distillation columns K(i), n≥2 and i=1…n; the reactive distillation columns K(i) are arranged in parallel, and each reactive distillation column K(i) includes:
[0248] --At its upper part, preferably at its top, is an inlet device for feeding the material flow H(i) into K(i);
[0249] --At its lower part is the inlet device for feeding the material flow G(i) into K(i);
[0250] --An outlet device for removing the material flow W(i) from the top of K(i);
[0251] --Bottom reboiler;
[0252] --An outlet device for removing the bottom flow from K(i);
[0253] --A flow divider for separating the material flow P(i) from the bottom material flow taken out from K(i);
[0254] - A device for feeding the feed stream G(i) into the reactive distillation column K(i);
[0255] - A device for feeding the feed stream W(i) into the distillation column D;
[0256] - One or more compressors C(i) for compressing material flow G and / or material flow G(i) and / or material flow W(i).
[0257] 63. The apparatus of embodiment 62, wherein at least one, preferably each reactive distillation column K(i), is equipped with a droplet separation device D(i) at the top, preferably a demister, the demister preferably including an inlet device for feeding a methanol-containing feed stream M(i) into the demister.
[0258] 64. The apparatus of embodiment 62 or 63, wherein each of the reactive distillation columns K(i) comprises 5 to 50, preferably 10 to 40, and more preferably 15 to 30 theoretical stages, independently of each other.
[0259] 65. The apparatus of any one of embodiments 62-64, wherein the means for feeding the feed stream G(i) into the reactive distillation column K(i) are independently located at the bottom of K(i) and the fifth theoretical stage, more preferably at the bottom of K(i) and the third theoretical stage, and more preferably at the position between the bottom of K(i) and the second theoretical stage.
[0260] 66. The apparatus of any one of embodiments 62-65, wherein the means for feeding the feed stream H(i) into the reactive distillation column K(i) is located at the top of K(i), preferably the uppermost theoretical stage.
[0261] 67. An apparatus according to any one of embodiments 62-66, wherein at least one, preferably each reactive distillation column K(i), does not include an apparatus operating at a reflux ratio greater than 0:1.
[0262] 68. An apparatus according to any one of embodiments 62-67, wherein each reactive distillation column K(i) is equipped with a tray.
[0263] 69. An apparatus according to any one of embodiments 62-68, comprising n compressors C(i) arranged upstream of K(i) for compressing the material flow G(i).
[0264] 70. An apparatus according to any one of embodiments 62-68, comprising n compressors C(i) arranged downstream of K(i) and upstream of D for compressing the material flow W(i).
[0265] 71. The apparatus of any one of embodiments 62-70, wherein the distillation column D has 20-100, preferably 30-80, and more preferably 40-60 theoretical stages.
[0266] 72. The apparatus of any one of embodiments 62-71, wherein the inlet device for supplying the material flow W(i) or one or more of its combined material flows into D is located at the bottom of D and the 15th theoretical stage, more preferably the bottom of D and the 10th theoretical stage, and even more preferably the bottom of D and the 8th theoretical stage.
[0267] 73. The apparatus of any one of embodiments 62-72, wherein the inlet device for feeding the material flow M into D is located at the top of D, preferably at least 4 theoretical stages from the top of D, more preferably between the 4th and 20th theoretical stages from the top of D, and even more preferably between the 6th and 15th theoretical stages from the top of D.
[0268] 74. The apparatus of any one of embodiments 62-73 further includes at least one condensate tank for extracting liquid streams from V(4) and optionally V(5) and further includes means for feeding at least a portion of the liquid contained in the tank as a feed stream T(3) into the top of D.
[0269] 75. The apparatus of any one of embodiments 62-74, further comprising means for recompressing the top vapor obtained from D, the means preferably comprising a compressor C(3) for compressing the feed stream T(1) taken from the top of D, means for feeding T(1) from the top of D into C(3), a reboiler V(6) for condensing the compressed feed stream, means for feeding the compressed feed stream from (C3) into V(6), and means for supplying the resulting liquid stream into the top of D.
[0270] 76. The apparatus of embodiment 75, wherein the reboiler V(6) is a reboiler of D, preferably an intermediate reboiler of D.
[0271] 77. The apparatus of any one of embodiments 62-76, wherein the distillation column is equipped with trays and / or packing, wherein, in the case of embodiment 77 depending on embodiment 76, D is equipped with packing arranged above the intermediate reboiler of D and trays arranged below the intermediate reboiler of D.
[0272] 78. The apparatus of embodiment 76 or 77 further includes at least one condensate tank for the condensate stream taken out from V(6), the apparatus preferably further includes means for feeding at least a portion of the gas phase in the tank into V(4) and means for feeding at least a portion of the liquid phase in the tank into the condensate tank according to embodiment 74.
[0273] 79. The apparatus of any one of embodiments 62-78, further comprising means for separating alkali metal methoxide A(i)OMe from at least one feed stream P(i).
[0274] 80. The apparatus of any one of embodiments 62-79, wherein n is in the range of 2-10, more preferably 2-5, more preferably 2 or 3, more preferably 2.
[0275] 81. Use of a chemical production apparatus according to any one of embodiments 62-80 or a method according to any one of embodiments 1-61 in the simultaneous production of n mixtures P(i) comprising alkali metal ethanol salts and methanol, where n is an integer, n≥2 and i=1…n, wherein at least two of the mixtures P(i) comprise different alkali metal ethanol salts A(i)OMe, and / or at least two of the mixtures P(i) comprise the same alkali metal alkoxide A(i)OMe at different concentrations.
[0276] The present invention comprises the following embodiments 1 and 2 and Figure 1-6 Further explanation. Example
[0277] Example 1: Simultaneous production of sodium methoxide and potassium methoxide in distillation column D without top vapor recompression
[0278] Figure 2 The process flow diagram shows the preparation of a mixture P(1) containing NaOMe and MeOH and a mixture P(2) containing KOMe and MeOH. For the operating conditions of distillation column D and reactive distillation columns K(1) and K(2), refer to Table 1a below. For the relative mass flow rates, refer to Table 1b below.
[0279] Table 1a Operating conditions of towers D, K(1) and K(2)
[0280]
[0281]
[0282] Table 1b shows the relationship between the mass flow rates f of different material flows.
[0283]
[0284] *)f(G)=f(G(1))+f(G(2))
[0285] P(1): 30% sodium methoxide in methanol, <1000ppm water.
[0286] P(2): 32% potassium methoxide in methanol, <1000ppm water.
[0287] The following section shows how to calculate the mass flow rate f of methanol contained in the feed stream M (methanol equilibrium, fresh methanol feed stream). MeOH (M). In this calculation, the water content of P(1) and P(2)—both less than 1000 ppm by weight—is negligible. According to this calculation, f MeOH (P(1)) is the mass flow rate of MeOH contained in the feed stream P(1), f MeOH(P(2)) is the mass flow rate of MeOH contained in the material flow P(2), f MeOH (water) is the mass flow rate of MeOH contained in the water stream and f MeOH (Waste gas) refers to the mass flow rate of MeOH contained in the waste gas stream:
[0288] f MeOH (M)=f MeOH (P(1))+f MeOH (P(2))+f MeOH (water) + f MeOH (Exhaust gas)
[0289] 1.1f MeOH (P(1))=[(1-c NaOME )*f(P(1))]+[(M MeOH / M NaOH *c NaOH )*f(H(1))]
[0290]
[0291] 1.2f MeOH (P(2))=[(1-c KOMe )*f(P(2))]+[(M MeOH / M KOH *c KOH )*f(H(2))]
[0292]
[0293] 1.3f MeOH (Water) = 0.001 * f(Water) (Maximum value)
[0294] 1.4f MeOH (Exhaust gas) = 0 (negligible)
[0295] The following shows how to calculate the mass flow rate, f(water), of the water contained in the feed stream (the bottom feed stream of D, the wastewater stream). In this calculation, the water content of P(1) and P(2)—both less than 1000 ppm by weight—is negligible.
[0296] 1.5f(water) = f H2O (H(1))+f H2O (H(2))+f H2O (M)-f H2O (Exhaust gas)
[0297] f H2O (H(1)) is the mass flow rate of water contained in the material flow H(1), f H2O (H(2)) is the mass flow rate of water contained in the material flow H(2) and fH2O (M) represents the mass flow rate of water contained in the material flow M:
[0298] 1.5.1f H2O (H(1))=[(1-c NaOH )*f(H(1))]+[(M H2O / M NaOH *c NaOH )*f(H(1))]
[0299]
[0300] 1.5.2f H2O (H(2))=[(1-c KOH )*f(H(2))]+[(M H2O / M KOH *c KOH )*f(H(2))]
[0301]
[0302]
[0303] 1.5.3f H2O (M) = 0.001 * f(M)
[0304] 1.5.4f H2O (Exhaust gas) = 0 (negligible)
[0305] Example 2: Simultaneous production of sodium methoxide and potassium methoxide in distillation column D with top vapor recompression
[0306] The use of vapor recompression significantly reduces the energy requirement for distillation in D. The heat flow with V(3) and V(6) can have a ratio of approximately 1:4. This means that the energy requirement is reduced by 20%. However, approximately 10% (depending on the pressure) of the energy transferred in V(6) is required as the energy source for the compressor C(3). In summary, there are significant energy savings through the use of vapor recompression.
[0307] Figure 5 The process flow diagram shows the preparation of a mixture P(1) containing NaOMe and MeOH and a mixture P(2) containing KOMe and MeOH. For the operating conditions of distillation column D and reactive distillation columns K(1) and K(2), refer to Table 2a below. For the relative mass flow rates, refer to Table 2b below.
[0308] Table 2a Operating conditions of towers D, K(1) and K(2)
[0309]
[0310] Table 2b shows the relationship between mass flow rates f for different material flows.
[0311]
[0312] *)f(G)=f(G(1))+f(G(2))
[0313] P(1): 30% sodium methoxide in methanol, <1000ppm water.
[0314] P(2): 32% potassium methoxide in methanol, <1000ppm water.
[0315] The following section shows how to calculate the mass flow rate f of methanol contained in the feed stream M (methanol equilibrium, fresh methanol feed stream). MeOH (M). In this calculation, the water content of P(1) and P(2)—both less than 1000 ppm by weight—is negligible. According to this calculation, f MeOH (P(1)) is the mass flow rate of MeOH contained in the feed stream P(1), f MeOH (P(2)) is the mass flow rate of MeOH contained in the material flow P(2), f MeOH (water) is the mass flow rate of MeOH contained in the water stream and f MeOH (Waste gas) refers to the mass flow rate of MeOH contained in the waste gas stream:
[0316] f MeOH (M)=f MeOH (P(1))+f MeOH (P(2))+f MeOH (water) + f MeOH (Exhaust gas)
[0317] 2.1f MeOH (P(1))=[(1-c NaOME )*f(P(1))]+[(M MeOH / M NaOH *c NaOH )*f(H(1))]
[0318]
[0319] 2.2f MeOH (P(2))=[(1-c KOMe )*f(P(2))]+[(M MeOH / M KOH *c KOH )*f(H(2))]
[0320]
[0321]
[0322] 2.3f MeOH (Water) = 0.001 * f(Water) (Maximum value)
[0323] 2.4f MeOH (Exhaust gas) = 0 (negligible)
[0324] The following shows how to calculate the mass flow rate, f(water), of the water contained in the feed stream (the bottom feed stream of D, the wastewater stream). In this calculation, the water content of P(1) and P(2)—both less than 1000 ppm by weight—is negligible.
[0325] 2.5f(water) = f H2O (H(1))+f H2O (H(2))+f H2O (M)-f H2O (Exhaust gas)
[0326] f H2O (H(1)) is the mass flow rate of water contained in the material flow H(1), f H2O (H(2)) is the mass flow rate of the water contained in H(2) and f H2O (M) represents the mass flow rate of water contained in the material flow M:
[0327] 2.5.1f H2O (H(1))=[(1-c NaOH )*f(H(1))]+[(M H2O / M NaOH *c NaOH )*f(H(1))]
[0328]
[0329] 2.5.2f H2O (H(2))=[(1-c KOH )*f(H(2))]+[(M H2O / M KOH *c KOH )*f(H(2))]
[0330]
[0331] 2.5.3f H2O (M) = 0.001 * f(M)
[0332] 2.5.4f H2O (Exhaust gas) = 0 (negligible) Attached Figure Description
[0333] Figure 1This diagram illustrates the method of the present invention, wherein the distillation column D operates without top vapor recompression. Specifically, a fresh methanol feed stream M is fed into the upper part of the distillation column D. A gas stream T(2)—an anhydrous methanol feed stream—is taken from the top of the distillation column D and passed through a condenser V(4), where it is compressed by a compressor V(4) to obtain a waste gas stream T(2w) and a liquid stream T(3), which consists essentially of inert components and methanol. The liquid stream T(3) is returned to the top of the column D. A portion of the bottom stream taken from the column D is fed into the bottom reboiler V(3) of D to dispose of the remaining portion of the bottom stream, which consists essentially of water. Furthermore, an anhydrous methanol gas stream G, in addition to T(2), is taken from the top of the column D. This gas stream G, having a flow rate f(G), is split into two streams G(1) and G(2), both having the same composition as G. Stream G(1) has a flow rate f(G(1)) and stream G(2) has a flow rate f(G(2)), where f(G(1)) + f(G(2)) = f(G). Stream G(1) is then passed through compressor C(1), and the compressed stream G(1) is fed into the lower part of reactive distillation column K(1), where an aqueous stream H(1) containing dissolved alkali metal hydroxide A(1)OH is fed into the upper part of K(1). A portion of the bottom stream from column K(1) is fed into the reboiler V(1) of K(1), and the remaining portion of the bottom stream is a mixture P(1) containing alkali metal methoxide A(1)OMe and methanol. A gas stream W(1) consisting primarily of methanol and water is drawn from the top of column K(1) which operates without reflux, and W(1) is fed into the lower part of distillation column D. The feed stream G(2) is then passed through compressor C(2), and the compressed feed stream G(2) is then fed into the lower part of reactive distillation column K(2), where an aqueous stream H(2) containing dissolved alkali metal hydroxide A(2)OH is fed into the upper part of K(2). A portion of the bottom stream taken from column K(2) is fed into the reboiler V(2) of K(2), and the remaining portion of the bottom stream is a mixture P(2) containing alkali metal methoxide A(2)OMe and methanol. A gas stream W(2) consisting essentially of methanol and water is taken from the top of column K(2) which operates without reflux, and W(2) is fed together with W(1) into the lower part of distillation column D.
[0334] Figure 2 Display according to Figure 1 A schematic overview of the diagram, wherein droplet separation devices D(1) and D(2), preferably demisters, are located at the top of reactive distillation towers K(1) and K(2), and feed streams M(1) and M(2) are used for at least temporary spraying.
[0335] Figure 3 Display according to Figure 2The diagram outlines the process where compressors C(1) and C(2) are not located upstream of K(1) and K(2) to compress G(1) and G(2), but are located downstream of K(1) and K(2) to compress W(1) and W(2) before W(1) and W(2) are fed into D.
[0336] Figure 4 This provides a graphical overview of the method of the present invention, wherein... Figure 1 Compared to the previous method, distillation column D operates under top vapor recompression. Regarding the top vapor recompression, anhydrous methanol overhead stream is taken from distillation column D except for G and T(2). This stream T(1) is passed through compressor C(3), and then the compressed stream T(1) is passed through intermediate reboiler V(6) of column D. The compressed and condensed stream T(1) thus obtained from V(6) is then fed into a first condensate tank. The inert component contained in T(1) is taken out from the first condensate tank as stream T(1g) via a control valve (not shown) and fed into condenser V(4), in which the overhead stream T(2) is also fed. The remaining portions T(1)-T(1l) are depressurized to a second condensate tank. Another stream T(2gl) obtained from condenser V(5) is fed into the second condensate tank, and streams T(2g) and T(2l) obtained from V(4) are fed into V(5). In addition, the feed stream T(2l) obtained from V(4) is fed into the second condensate tank. The liquid stream T(3) is taken out from the second condensate tank and fed into the top of the tower D.
[0337] Figure 5 Display according to Figure 4 A schematic overview of the diagram, wherein droplet separation devices D(1) and D(2), preferably demisters, are located at the top of reactive distillation towers K(1) and K(2), and feed streams M(1) and M(2) are used for at least temporary spraying.
[0338] Figure 6 Display according to Figure 5 The diagram outlines the process where compressors C(1) and C(2) are not located upstream of K(1) and K(2) to compress G(1) and G(2), but are located downstream of K(1) and K(2) to compress W(1) and W(2) before W(1) and W(2) are fed into D.
[0339] References
[0340] -US 2002 / 0183566 A1
[0341] -US 2008 / 0296786 A1
[0342] -WO 2013 / 168113 A1
Claims
1. An integrated method for simultaneously preparing n mixtures P(i) comprising alkali metal methoxides and methanol, comprising: Provide n reactive distillation columns K(i); Provide n aqueous liquid flows H(i), where each aqueous liquid flow H(i) contains dissolved alkali metal hydroxide A(i)OH, where n is an integer, n ≥ 2 and i = 1…n; as well as Provide distillation column D; The method further includes: (a) Provide a feed stream G containing methanol; (b) Divide the material flow G into n material flows G(i), each material flow G(i) having the same composition as G; (c) Preparing one or more alkali metal methanol salts, comprising: Each feed stream G(i) is fed into the lower part of the corresponding reactive distillation column K(i), and an aqueous liquid stream H(i) containing dissolved alkali metal hydroxide A(i)OH is fed into the upper part of the reactive distillation column K(i); and G(i) and H(i) are subjected to reactive distillation conditions in each K(i) to obtain n overhead streams W(i) containing methanol and water; and n bottom streams P(i) containing alkali metal methanol salt A(i)OMe and methanol. (d) Each stream W(i) is fed into the lower part of the distillation column D, and a stream M containing methanol is fed into the distillation column D; and the n streams W(i) and M are subjected to distillation conditions in D to obtain the stream G according to (a) as the top stream. The distillation column D operates at a reflux ratio of at least 0.5:1, and the distillation column D operates with top vapor recompression, wherein, in order to achieve the said reflux ratio, the method includes: (i) Take the top feed stream T(2) from the distillation column D except for G, and pass the feed stream T(2) through the condenser V(4) to obtain liquid stream and waste gas stream T(2w); (ii) Take another top stream T(1) from the distillation column D in addition to G and T(2), pass the stream T(1) through the compressor C(3), and pass the compressed stream through the reboiler V(6) to obtain a liquid stream, wherein the reboiler V(6) is the intermediate reboiler of the distillation column D; (iii) The liquid flow obtained according to (i) and (ii) is fed into the top of the distillation column D; or (i) Take the top feed stream T(2) from the distillation column D except for G, and pass the feed stream T(2) through the condenser V(4) to obtain liquid stream T(2l) and gas stream T(2g); pass the gas stream T(2g) through the condenser V(5) to obtain liquid stream T(2gl) and waste gas stream T(2w); and combine liquid stream T(2l) and T(2gl) to obtain combined liquid stream T(2cl); (ii) Take another top stream T(1) from the distillation column D in addition to G and T(2), pass the stream T(1) through the compressor C(3), and pass the compressed stream through the reboiler V(6) to obtain a liquid stream, wherein the reboiler V(6) is an intermediate reboiler of the distillation column D; (iii) The combined liquid stream obtained according to (i) and the liquid stream obtained according to (ii) are fed into the top of the distillation column D.
2. The method of claim 1, wherein n is in the range of 2-10.
3. The method of claim 1, wherein n is in the range of 2-5.
4. The method of claim 1, wherein n is 2 or 3.
5. The method of claim 1, wherein each alkali metal hydroxide A(i)OH is selected from lithium hydroxide, sodium hydroxide and potassium hydroxide, and wherein a given aqueous stream H(i) contains an alkali metal hydroxide A(i)OH dissolved in water, methanol or a mixture containing water and methanol.
6. The method of claim 2, wherein each alkali metal hydroxide A(i)OH is selected from lithium hydroxide, sodium hydroxide and potassium hydroxide, and wherein a given aqueous stream H(i) contains an alkali metal hydroxide A(i)OH dissolved in water, methanol or a mixture containing water and methanol.
7. The method of claim 3, wherein each alkali metal hydroxide A(i)OH is selected from lithium hydroxide, sodium hydroxide and potassium hydroxide, and wherein a given aqueous stream H(i) contains an alkali metal hydroxide A(i)OH dissolved in water, methanol or a mixture containing water and methanol.
8. The method of claim 4, wherein each alkali metal hydroxide A(i)OH is selected from lithium hydroxide, sodium hydroxide and potassium hydroxide, and wherein a given aqueous stream H(i) contains an alkali metal hydroxide A(i)OH dissolved in water, methanol or a mixture containing water and methanol.
9. The method of any one of claims 5-8, wherein each alkali metal hydroxide A(i)OH is selected from sodium hydroxide and potassium hydroxide.
10. The method of any one of claims 1-8, comprising an integrated method for simultaneously preparing at least two mixtures P(i), wherein mixture P(1) comprises A(1)OMe and methanol, and mixture P(2) comprises A(2)OMe and methanol, the method comprising: (a) Provide a feed stream G containing methanol; (b) Divide the material flow G into at least two material flows G(1) and G(2), G(1) and G(2) having the same composition as G; (c.1) Preparation of A(1)OMe, including: (c.1.1) Feed stream G(1) into the lower part of reactive distillation column K(1) and feed stream H(1) containing dissolved A(1)OH into the upper part of reactive distillation column K(1); (c.1.2) G(1) and H(1) are subjected to reactive distillation conditions in K(1) to obtain a top stream W(1) containing methanol and water; and a bottom stream P(1) containing A(1)OMe and methanol. (c.2) Preparation of A(2)OMe, including: (c.2.1) Feed stream G(2) into the lower part of reactive distillation column K(2), wherein K(2) is arranged parallel to K(1), and aqueous liquid stream H(2) containing dissolved A(2)OH is fed into the upper part of reactive distillation column K(2); (c.2.2) G(2) and H(2) are subjected to reactive distillation conditions in K(2) to obtain a top stream W(2) containing methanol and water; and a bottom stream P(2) containing A(2)OMe and methanol. (d.1) Feed W(1) and W(2) into the lower part of distillation column D, and feed M containing methanol into distillation column D; (d.2) subject W(1), W(2) and M to distillation conditions in D to obtain the feed stream G according to (a) as the overhead feed stream.
11. The method of claim 9, an integrated method for simultaneously preparing at least two mixtures P(i), wherein mixture P(1) comprises A(1)OMe and methanol, and mixture P(2) comprises A(2)OMe and methanol, the method comprising: (a) Provide a feed stream G containing methanol; (b) Divide the material flow G into at least two material flows G(1) and G(2), G(1) and G(2) having the same composition as G; (c.1) Preparation of A(1)OMe, including: (c.1.1) Feed stream G(1) into the lower part of reactive distillation column K(1) and feed stream H(1) containing dissolved A(1)OH into the upper part of reactive distillation column K(1); (c.1.2) G(1) and H(1) are subjected to reactive distillation conditions in K(1) to obtain a top stream W(1) containing methanol and water; and a bottom stream P(1) containing A(1)OMe and methanol. (c.2) Preparation of A(2)OMe, including: (c.2.1) Feed stream G(2) into the lower part of reactive distillation column K(2), wherein K(2) is arranged parallel to K(1), and aqueous liquid stream H(2) containing dissolved A(2)OH is fed into the upper part of reactive distillation column K(2); (c.2.2) G(2) and H(2) are subjected to reactive distillation conditions in K(2) to obtain a top stream W(2) containing methanol and water; and a bottom stream P(2) containing A(2)OMe and methanol. (d.1) Feed W(1) and W(2) into the lower part of distillation column D, and feed M containing methanol into distillation column D; (d.2) subject W(1), W(2) and M to distillation conditions in D to obtain the feed stream G according to (a) as the overhead feed stream.
12. The method of claim 11 is an integrated method for simultaneously preparing two mixtures P(i).
13. The method of claim 12, wherein A(1)OMe is sodium methoxide.
14. The method of claim 13, wherein A(2)OMe is potassium methoxide.
15. The method of claim 14, wherein A(1)OH is sodium hydroxide.
16. The method of claim 15, wherein A(2)OH is potassium hydroxide.
17. The method of claim 10, wherein W(1) and W(2) are supplied as gas streams into distillation column D.
18. The method of any one of claims 11-16, wherein W(1) and W(2) are supplied as gas streams into distillation column D.
19. The method of claim 18, wherein W(1) and W(2) are supplied as gas streams into the distillation column D at a position between the bottom of the distillation column D and the 15th theoretical stage.
20. The method of claim 19, wherein W(1) and W(2) are supplied as gas streams into the distillation column D at a position between the bottom of the distillation column D and the 10th theoretical stage.
21. The method of claim 20, wherein W(1) and W(2) are supplied as gas streams into the distillation column D at a position between the bottom of the distillation column D and the 8th theoretical stage.
22. The method of any one of claims 1-8, wherein 99-100% by weight of the feed stream M consists of methanol and optionally water, wherein the amount of water contained in the feed stream M is at most 2000 ppm by weight.
23. The method of any one of claims 19-21, wherein 99-100% by weight of the feed stream M consists of methanol and optionally water, wherein the amount of water contained in the feed stream M is at most 2000 ppm by weight.
24. The method of claim 23, wherein 99.5-100% by weight of the feed stream M consists of methanol and optionally water.
25. The method of claim 24, wherein 99.9-100% by weight of the feed stream M consists of methanol and optionally water.
26. The method of claim 25, wherein the amount of water contained in the feed stream M is at most 1500 ppm by weight.
27. The method of claim 26, wherein the amount of water contained in the feed stream M is at most 1000 ppm by weight.
28. The method of claim 27, wherein the material flow M is fed into the upper part of D.
29. The method of claim 28, wherein the material flow M is fed into the upper part of D at least 4 theoretical stages away from the top of D.
30. The method of claim 29, wherein the material flow M is supplied to the upper part of D between the 4th and 20th theoretical stages from the top of D.
31. The method of claim 30, wherein the material flow M is supplied to the upper part of D between the 6th and 15th theoretical stages from the top of D.
32. The method of claim 31, wherein the feed stream M is fed into the upper part of D at a temperature of M within the range of ambient temperature to the boiling point of methanol at the tower pressure of D.
33. The method of claim 32, wherein the feeding of the material stream M into the upper part of D is carried out at ambient temperature.
34. The method of any one of claims 1-8, wherein the distillation column D is operated at a reflux ratio in the range of 0.55:1 to 1.4:
1.
35. The method of any one of claims 24-33, wherein the distillation column D is operated at a reflux ratio in the range of 0.55:1 to 1.4:
1.
36. The method of claim 35, wherein the distillation column D is operated at a reflux ratio in the range of 0.6:1 to 1.4:
1.
37. The method of any one of claims 1-8, wherein the feed stream G provided according to (a) by distillation according to (d.2) comprises methanol and water and wherein the water content of G is at most 200 ppm by weight.
38. The method of claim 36, wherein the feed stream G provided according to (a) by distillation according to (d.2) comprises methanol and water and wherein the water content of G is at most 200 ppm by weight.
39. The method of claim 38, wherein 99.95-100% by weight of G is composed of methanol and water.
40. The method of claim 39, wherein the water content of G is at most 150 ppm by weight.
41. The method of claim 40, wherein the water content of G is at most 100 ppm by weight.
42. The method of claim 41, wherein the water content is in the range of 5-100 ppm by weight.
43. The method of claim 42, wherein the water content is in the range of 10-100 ppm by weight.
44. The method of claim 43, wherein the water content is in the range of 15-100 ppm by weight.
45. The method of any one of claims 1-8, wherein, according to (b), the material flow G is divided into two material flows G(1) and G(2).
46. The method of any one of claims 39-44, wherein, according to (b), the material flow G is divided into two material flows G(1) and G(2).
47. The method of any one of claims 1-8, wherein the feed stream G(1) is passed through compressor C(1) before being fed into the reactive distillation column K(1), thereby achieving an increase in the absolute pressure of G(1) in the range of 0.1-0.8 bar; And / or, Before being fed into the reactive distillation column K(2), the feed stream G(2) is passed through the compressor C(2), thereby increasing the absolute pressure of G(2) in the range of 0.1-0.8 bar.
48. The method of claim 46, wherein the feed stream G(1) is passed through compressor C(1) before being fed into the reactive distillation column K(1), thereby achieving an increase in the absolute pressure of G(1) in the range of 0.1-0.8 bar; And / or, Before being fed into the reactive distillation column K(2), the feed stream G(2) is passed through the compressor C(2), thereby increasing the absolute pressure of G(2) in the range of 0.1-0.8 bar.
49. The method of claim 48, wherein the feed stream G(1) is passed through the compressor C(1) before being fed into the reactive distillation column K(1), thereby achieving an increase in the absolute pressure of G(1) in the range of 0.15-0.6 bar.
50. The method of claim 49, wherein the feed stream G(1) is passed through the compressor C(1) before being fed into the reactive distillation column K(1), thereby achieving an increase in the absolute pressure of G(1) in the range of 0.2-0.4 bar.
51. The method of claim 50, wherein the feed stream G(2) is passed through compressor C(2) before being fed into the reactive distillation column K(2), thereby achieving an increase in the absolute pressure of G(2) in the range of 0.15-0.6 bar.
52. The method of claim 51, wherein the feed stream G(2) is passed through the compressor C(2) before being fed into the reactive distillation column K(2), thereby achieving an increase in the absolute pressure of G(2) in the range of 0.2-0.4 bar.
53. The method of any one of claims 1-8, wherein before being fed into the distillation column D, the feed stream W(1) is passed through the compressor C(1) by an increase in absolute pressure of W(1) in the range of 0.1-0.8 bar; and / or Before being fed into distillation column D, the feed stream W(2) is passed through compressor C(2), thereby increasing the absolute pressure of W(2) in the range of 0.1-0.8 bar.
54. The method of claim 46, wherein before being fed into the distillation column D, the feed stream W(1) is passed through the compressor C(1) by an increase in absolute pressure of W(1) in the range of 0.1-0.8 bar; and / or Before being fed into distillation column D, the feed stream W(2) is passed through compressor C(2), thereby increasing the absolute pressure of W(2) in the range of 0.1-0.8 bar.
55. The method of claim 54, wherein before being fed into the distillation column D, the feed stream W(1) is passed through the compressor C(1) by an increase in absolute pressure of W(1) in the range of 0.15-0.6 bar.
56. The method of claim 55, wherein before being fed into the distillation column D, the feed stream W(1) is passed through the compressor C(1) to increase the absolute pressure of W(1) in the range of 0.2-0.4 bar.
57. The method of claim 56, wherein before being fed into the distillation column D, the feed stream W(2) is passed through the compressor C(2), thereby achieving an increase in the absolute pressure of W(2) in the range of 0.15-0.6 bar.
58. The method of claim 57, wherein before being fed into the distillation column D, the feed stream W(2) is passed through the compressor C(2), thereby achieving an increase in the absolute pressure of W(2) in the range of 0.2-0.4 bar.
59. A chemical production apparatus for implementing the method according to any one of claims 1-58, comprising: - Distillation column D, including: --An inlet device used to feed material flow M into D; --At its lower part is an inlet device for feeding the material flow W(i) or one or more of its combined material flows into D; --An outlet device for removing material flow T(2) and G or their combined material flow from the top of D; --At least one condenser having an inlet device for receiving a feed stream T(2) and an outlet device for removing the condensed feed stream T(3) and removing the waste gas stream; -- An inlet device for feeding the material flow T(3) into the top of D; --Bottom reboiler; - A diversion device S for dividing a material flow G into n material flows G(i); - A device for feeding the material flow G into the diversion device S; -n reactive distillation columns K(i), n≥2 and i=1…n; the reactive distillation columns K(i) are arranged in parallel, and each reactive distillation column K(i) includes: --The inlet device at its upper part is used to supply the aqueous liquid flow H(i) into K(i); --At its lower part is the inlet device for feeding the material flow G(i) into K(i); --An outlet device for removing the material flow W(i) from the top of K(i); --Bottom reboiler; --An outlet device for removing the bottom flow from K(i); --A flow divider for separating the material flow P(i) from the bottom material flow taken out from K(i); - A device for feeding the feed stream G(i) into the reactive distillation column K(i); - A device for feeding the feed stream W(i) into the distillation column D; - One or more compressors C(i) for compressing material flow G and / or material flow G(i) and / or material flow W(i).
60. The apparatus of claim 59, wherein at least one condenser is a condenser V(4) and optionally, another condenser V(5) is arranged downstream of V(4).
61. The apparatus of claim 60, wherein each reactive distillation column K(i) includes an inlet device at its top for feeding an aqueous liquid stream H(i) into K(i).
62. The apparatus of claim 59, comprising n compressors C(i) arranged upstream of K(i) for compressing the material flow G(i) or comprising n compressors C(i) arranged downstream of K(i) and upstream of D for compressing the material flow W(i).
63. The apparatus of claim 60, comprising n compressors C(i) arranged upstream of K(i) for compressing the material flow G(i) or comprising n compressors C(i) arranged downstream of K(i) and upstream of D for compressing the material flow W(i).
64. The apparatus of claim 61, comprising n compressors C(i) arranged upstream of K(i) for compressing the material flow G(i) or comprising n compressors C(i) arranged downstream of K(i) and upstream of D for compressing the material flow W(i).
65. The apparatus of any one of claims 59-64, wherein the inlet device for feeding the feed stream W(i) or one or more of their combined feed streams into D is located between the bottom of D and the 15th theoretical stage; and / or The inlet device for feeding the material flow M into D is located at the top of D.
66. The apparatus of claim 65, wherein the inlet device for feeding the stream W(i) or one or more of its combined streams into D is located between the bottom of D and the 10th theoretical stage.
67. The apparatus of claim 66, wherein the inlet device for feeding the material stream W(i) or one or more of its combined material streams into D is located between the bottom of D and the 8th theoretical stage.
68. The apparatus of claim 67, wherein the inlet device for feeding the material flow M into D is located at the top of D at least 4 theoretical stages away from the top of D.
69. The apparatus of claim 68, wherein the inlet device for feeding the material flow M into D is located at the top of D, between the 4th and 20th theoretical stages from the top of D.
70. The apparatus of claim 69, wherein the inlet device for feeding the material flow M into D is located at the top of D, between the 6th and 15th theoretical stages from the top of D.
71. Use of the chemical production apparatus according to any one of claims 59-70 or the method according to any one of claims 1-58 in the simultaneous production of n mixtures P(i) comprising an alkali metal ethanol salt A(i)OMe and methanol, where n is an integer, n≥2 and i=1…n, wherein at least two of the mixtures P(i) comprise different alkali metal ethanol salts A(i)OMe and / or at least two of the mixtures P(i) comprise the same alkali metal alkoxide salt A(i)OMe at different concentrations.
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