Device and process for preparing metal organic compounds

Abstract

The present disclosure relates to a device and process for preparing metal organic compounds. The device is a multi-layer tray structure, and the whole tower includes three parts: the top of the tower, the middle of the tower and the bottom of the tower. The top of the tower includes a condensing coil and a gas outlet, and the middle of the tower includes: more than two trays and a feed port corresponding to each tray, and the bottom of the tower includes an overflow port, a bottom outlet and a flushing port. The device disclosed in the present disclosure is aimed at the preparation and production of metal organic compounds. The existing kettle technology has the disadvantages of low heat exchange efficiency, difficult to control reaction temperature, easy to cause material rushing, slow dripping rate, and long reaction time. The structure of layered feeding and multi-tray heat exchange is adopted to achieve effective temperature control, prevent material rushing, and stabilize production. The whole set of equipment is easy to operate and control, has a high conversion rate, and significant economic benefits.

Description

Technical Field

[0001] The present disclosure relates to the field of organic synthesis production, and in particular to a device for preparing metal organic compounds and a process for preparing metal organic compounds using the device. Background Art

[0002] Organometallic compounds are an important class of chemical reagents, widely used in organic synthetic chemistry and the pharmaceutical industry, such as Grignard reagents, alkyl lithium, etc. Alkyl lithium is used as an anionic polymer initiator and hydrocarbonating agent to prepare low-cis polybutadiene rubber, isoprene rubber, thermosetting resins and coatings. Grignard reagents are the most important multifunctional reagents that can synthesize hydrocarbons, alcohols, ketones, aldehydes, carboxylic acids and metal organic compounds.

[0003] However, this type of metal organic compound is very active in nature and reacts violently with air and moisture. It needs to be synthesized in the absence of oxygen and water and under the protection of inert gas. At the same time, their production process is also very exothermic, and a large amount of flammable and explosive raw materials in the reaction are easily flushed in the kettle.

[0004] At present, the production of this type of active metal organic compound mainly includes two processes: single-pot batch production and multi-pot series continuous production. The cooling of the single-pot is mainly realized by the medium heat exchange in the jacket. However, the heat exchange area of ​​the jacket is limited, and the reaction temperature is difficult to control, so the raw material is added dropwise, which is slow and has a long reaction time. CN107537423, CN106674257 and CN111138461 have developed a continuous production process of multi-pot series, and each pot is connected by an overflow port, which alleviates the problem of material flushing to a certain extent and increases the heat exchange area. However, the overall heat transfer efficiency of the kettle process is low, the flux is low, and the production is unstable, which makes it unsuitable for the large-scale preparation and production of this type of active organic metal, and there are also potential safety hazards. Summary of the invention

[0005] The present invention provides a device for preparing metal organic compounds and a process for preparing metal organic compounds using the device. The present invention aims to solve the problems of insufficient cooling, difficult temperature control, easy material impaction, etc. in the traditional autoclave process of metal organic compounds, reduce the potential safety hazards in the production process, and improve the production efficiency of metal organic compounds.

[0006] The technical solution of the present disclosure is as follows:

[0007] A device for preparing metal organic compounds, which is a multi-layer tray structure, the whole tower includes three parts: the tower top, the tower middle and the tower bottom: wherein,

[0008] The tower top includes a condensing coil and a gas outlet, wherein:

[0009] The condensing coil is arranged inside the tower top, and is used to cool the organic vapor rising to the tower top in the device, condense it and return it to the first layer of tower tray, thereby controlling the temperature of the tower top;

[0010] The gas outlet is arranged at the top of the tower to discharge uncondensed organic vapor or non-condensable gas;

[0011] The tower comprises: more than two trays and a feed port corresponding to each tray, wherein:

[0012] The tower trays are arranged in sequence from top to bottom in the tower, and are used to evenly pile up metal reaction raw materials thereon, such as magnesium chips required for Grignard reagent reaction, metal lithium particles required for alkyl lithium synthesis, etc.; an inlet overflow weir and an outlet overflow weir are respectively arranged on both sides of each tower tray; the inlet overflow weir is slightly higher than the outlet overflow weir, and is used to prevent the raw materials from directly rushing into the tower tray; the outlet overflow weir is used to ensure the liquid holding capacity on the tower tray; the setting positions of the inlet overflow weir and the outlet overflow weir of the lower tower tray are opposite to the setting positions of the inlet overflow weir and the outlet overflow weir of the adjacent upper tower tray;

[0013] Each tray has a number of slots with caps on them, which are passages for the organic vapor and non-condensable gas in the device to rise; the height of the slot wall is not lower than the inlet overflow weir of the tray to ensure that the liquid will not short-circuit from the slot to the next tray;

[0014] A cooling coil is welded under the bottom of each tray, which is used to cool the reaction liquid on the tray and condense organic vapor;

[0015] A downcomer is arranged between the outlet overflow weir of the upper tower tray and the inlet overflow weir of the adjacent lower tower tray, and the downcomer cooperates with the inlet overflow weir of the lower tower tray to form a liquid seal;

[0016] The feed port corresponding to each tray is used to add reaction raw materials, wherein the feed port corresponding to the top tray extends from the tower wall to the outside of the inlet overflow weir and is not higher than the inlet overflow weir, and the feed ports corresponding to other trays extend from the tower wall into the middle and lower part of the downcomer;

[0017] The tower kettle includes an overflow port, a tower bottom outlet and a flushing port, wherein:

[0018] The overflow port is used to overflow the clear liquid after the reaction;

[0019] The flushing port is used to introduce solvent to flush the bottom residue of the kettle and discharge it from the bottom outlet of the tower.

[0020] Preferably, the number of the tower trays is 2-6. The number of the tower trays can be determined according to the reaction type and reaction speed.

[0021] Preferably, the grooves of adjacent trays are arranged in a staggered manner, so that the organic vapor rises smoothly through the channels in the grooves to prevent material impact; at the same time, the rising organic vapor can be condensed when encountering the cooling coil of the upper tray and return to the tray along the cap.

[0022] The size and number of the grooves on the tray depend on the amount of gas in the specific reaction. Preferably, the total area of ​​the grooves accounts for 10-35% of the tray area. The shapes of the grooves on the tray and their caps are not particularly limited, as long as they can achieve the corresponding functions. Preferably, the grooves on the tray can be parallel strip grooves or structures with the same function; the corresponding caps can be herringbone or arched caps or other structures with the same function.

[0023] Preferably, the cooling coil welded below the bottom of the tray can be a semicircular series coil half tube or a triangular series coil half tube. The coil heat exchange area is as sufficient as possible, which is used to control the reaction temperature of the reaction liquid on the tray and also provide cooling capacity for the condensation of organic vapor.

[0024] In addition, when the synthesis of metal organic compounds is very exothermic, independent cooling coils can be added between the tower plates to better control the tower temperature.

[0025] The present disclosure also provides a process for preparing a metal organic compound using the above-mentioned device, the process comprising:

[0026] 1) While the whole tower is being replaced with inert gas and protected, the reactant solution is allowed to enter the tower through the feed port of the uppermost tray;

[0027] 2) the reactant solution passes through the inlet overflow weir of the tower tray in step 1) and contacts with the uniformly scattered metal raw materials on the tower tray to react, and the reaction liquid flows to the lower outlet overflow weir;

[0028] 3) The reaction is highly exothermic, and a cooling medium is introduced into the cooling coil of the tower tray to cool the temperature to a predetermined reaction temperature, so as to reduce solvent vaporization or escape of gaseous reactants;

[0029] 4) The solvent and other gases vaporized in step 3), such as protective gas argon or N2, rise to the top of the tower or the upper tower tray through the grooves on the tower tray, are cooled by the cooling coils on the top of the tower or the upper tower tray, partially condensed, slide along the cap and fall into the tower tray to continue to participate in the reaction; finally, the uncondensed steam and non-condensable gas leave the tower from the gas outlet at the top of the tower;

[0030] 5) The reaction liquid in step 2) flows out of the tower tray along the outlet overflow weir and enters the downcomer;

[0031] 6) In step 5), the downcomer and the inlet overflow weir of the lower tower tray form a liquid seal, thereby preventing gas from entering the downcomer;

[0032] 7) The fresh reactant solution enters the downcomer in step 6) from the feed port of the next tray, mixes with the upper layer of the reaction solution, and then passes over the inlet overflow weir to enter the next tray for reaction;

[0033] 8) Keep the concentration of liquid phase raw materials on each tray not too high to avoid excessive reaction and exceeding the heat exchange capacity of the cooling coil, and repeat steps 2)-7) until the reaction liquid flows into the kettle;

[0034] 9) The reaction liquid in step 8) carries some solid residues and is allowed to settle in the reactor, the settled clear liquid continuously flows out from the overflow port, and the sludge-like solid residues accumulate at the bottom;

[0035] 10) When the solid residue accumulates to a certain extent, close the overflow port in step 9), open the bottom outlet to let the slurry flow out, and open the flushing pipe to flush the bottom of the kettle until the clear liquid is discharged.

[0036] Preferably, in step 1), the reactant solution includes but is not limited to ether solution or tetrahydrofuran solution of halogenated hydrocarbon (halogenated alkane or halogenated aromatic hydrocarbon) in the synthesis of Grignard reagent; cyclohexane, n-hexane or white oil solution of halogenated hydrocarbon in the synthesis of alkyl lithium, etc.

[0037] Preferably, in step 2), the metal raw materials include but are not limited to magnesium chips required for Grignard reagent reaction and metal lithium particles required for alkyl lithium synthesis;

[0038] Preferably, in step 3), the cooling medium includes but is not limited to circulating cooling water, chilled brine, etc.

[0039] Preferably, the device can be operated at normal pressure or at pressurized pressure.

[0040] Beneficial Effects

[0041] The device disclosed in the present invention is aimed at the preparation and production of metal organic compounds. The existing kettle technology has the disadvantages of low heat exchange efficiency, difficult to control reaction temperature, easy to produce materials, slow dripping rate, long reaction time, etc. The structure of layered feeding and multi-tray heat exchange is adopted to achieve effective temperature control, prevent material from being washed out, and stabilize production. The whole set of equipment is easy to operate and control, has a high conversion rate, and significant economic benefits. BRIEF DESCRIPTION OF THE DRAWINGS

[0042] Figure 1 It is a schematic structural diagram of an embodiment of an apparatus for preparing metal organic compounds according to the present disclosure.

[0043] Figure 2 This is a schematic diagram of the tray structure installed inside a conventional distillation tower.

[0044] Figure 3The present invention is a perspective view showing a schematic arrangement of components on a tray of an apparatus for preparing a metal organic compound according to an embodiment of the present invention.

[0045] Figure 4 For viewing from below Figure 3 A perspective view of the device.

[0046] Reference numerals

[0047] 1-tower top, 2-tower middle, 3-tower bottom; 11-condensing coil, 12-gas outlet, 21-feed port, 22-strip groove, 23-herringbone cap, 24-cooling coil, 25-inlet overflow weir, 26-outlet overflow weir, 27-downcomer, 31-overflow port, 32-flushing pipe, 33-tower bottom outlet. DETAILED DESCRIPTION

[0048] The specific embodiments of the present disclosure are described in detail below with reference to the accompanying drawings, but are not intended to limit the present disclosure.

[0049] It should be understood that various modifications may be made to the embodiments disclosed herein. Therefore, the following description should not be considered as limiting, but merely as an example of an embodiment. Other modifications within the scope and spirit of the present disclosure will occur to those skilled in the art.

[0050] The accompanying drawings, which are incorporated in and constitute a part of the specification, illustrate embodiments of the present disclosure and, together with the general description of the present disclosure given above and the detailed description of the embodiments given below, serve to explain the principles of the present disclosure.

[0051] These and other characteristics of the present disclosure will become apparent from the following description of a preferred form of embodiment given as a non-limiting example, with reference to the accompanying drawings.

[0052] It should also be understood that, although the present disclosure has been described with reference to some specific examples, those skilled in the art will be able to realize many other equivalent forms of the present disclosure that have the features described in the claims and are therefore within the scope of protection defined thereby.

[0053] The above and other aspects, features and advantages of the present disclosure will become more apparent from the following detailed description when taken in conjunction with the accompanying drawings.

[0054] This specification may use the phrases "in one embodiment," "in another embodiment," "in a further embodiment," or "in other embodiments," all of which may refer to one or more of the same or different embodiments according to the present disclosure.

[0055] According to one embodiment of the present disclosure, a device for preparing a metal organic compound is provided, such as Figure 1As shown, it is a multi-layer tray structure, and the entire tower mainly includes three parts: tower top 1, tower middle 2 and tower bottom 3.

[0056] The tower top 1 mainly includes a condensing coil 11 and a gas outlet 12. The condensing coil 11 is mainly used to cool the organic vapor rising from the device to the tower top, condense it and return it to the first layer of the tower plate; the gas outlet 12 is mainly used to discharge uncondensed organic vapor and non-condensable gas. After the uncondensed organic vapor flows out of the device, it can be recovered by heat exchange, for example, through a heat exchanger.

[0057] The tower 2 mainly includes multi-layer trays ( Figure 1 There are 3 layers in the tower, which are arranged in sequence from top to bottom in the tower) and a feed port 21 corresponding to each tray. The number of trays can be determined according to the reaction type and reaction speed, for example, it can be 2-6 layers.

[0058] Metal reaction raw materials are evenly scattered on the tray, such as magnesium chips required for Grignard reagent reaction, metal lithium particles required for alkyl lithium synthesis, etc., but not limited thereto.

[0059] The tray is provided with a strip groove 22, and a herringbone cap 23 is installed on the groove, which is a channel for the organic vapor in the device to rise. The height of the groove wall is not lower than the inlet overflow weir described below to ensure that the liquid will not short-circuit from the groove to the next tray. Preferably, the number and size of the strip grooves 22 and the caps 23 on the tray are determined according to the amount of gas in the specific reaction. Preferably, the total area of ​​the grooves accounts for 10-35% of the tray area, such as 15%, 20%, 25%, 30%, etc. In addition, the strip grooves 22 and the herringbone caps 23 on the tray can also be replaced by structures with the same function, for example: the herringbone cap can be replaced by an arch cap, and the strip grooves 22 and the herringbone caps 23 can be replaced by cylindrical openings and conical caps. In this way, the organic vapor can rise and pass smoothly to prevent the material from rushing on the tray; at the same time, the organic vapor condensed by the cooling coil returns to the tray along the cap. Preferably, the slots of adjacent trays are arranged in a staggered manner, so that the organic vapor rises smoothly through the channels in the slots to prevent material impact; at the same time, the rising organic vapor encounters the cooling coil of the upper tray and can be condensed and return to the tray along the cap.

[0060] A cooling coil 24 is welded to the bottom of each tray to cool the reaction liquid on the tray and also to condense the rising organic vapor.

[0061] The shape of the cooling coil 24 below the bottom of the tray is not particularly limited, for example, a semicircular series coil half tube or a triangular series coil half tube can be selected. The coil heat exchange area is as sufficient as possible, which is used to control the reaction temperature of the reaction liquid on the tray and also provide cooling capacity for the condensation of organic vapor. When the synthesis of metal organic compounds is very exothermic, an independent cooling coil can be added under each layer of the tray to better control the tower temperature of each layer.

[0062] An inlet overflow weir 25 and an outlet overflow weir 26 are respectively arranged on both sides of each tray, wherein the inlet overflow weir and the outlet overflow weir of the lower tray are arranged at opposite positions to those of the upper tray, that is, the lower tray and the upper tray are arranged with the inlet overflow weir and the outlet overflow weir in a staggered manner. The inlet overflow weir 25 is slightly higher than the outlet overflow weir 26, and is used to prevent the raw material from directly rushing into the tray; the outlet overflow weir 26 is used to ensure the liquid holding capacity on the tray.

[0063] A large excess of metal raw materials can be piled up on the trays of each layer, and the pile height can exceed the inlet overflow weir 25. In this case, the metal raw materials are greatly excessive, so that continuous production can be maintained for a period of time without the need to add metal raw materials.

[0064] A downcomer 27 is provided between the outlet overflow weir of the upper tray and the inlet overflow weir of the adjacent lower tray. The downcomer 27 and the inlet overflow weir 25 of the lower tray cooperate to form a liquid seal, which can prevent organic vapor and non-condensable gas from entering the downcomer 27. The feed port 21 is used to add reaction raw materials, wherein the feed port 21 corresponding to the top tray extends from the tower wall to the outside of the inlet overflow weir 25 and is not higher than the inlet overflow weir 25, and the feed ports 21 corresponding to other trays extend from the tower wall into the lower middle part of the downcomer 27.

[0065] Figure 2 The schematic diagram of the conventional tray structure set inside the conventional distillation tower is shown, including the tray, overflow weir and downcomer. In the conventional tray structure, multiple holes are opened on the tray. When the gas and liquid react, the gas and liquid are in favorable contact, and then react. As the gas continues to rise through the holes, the low-boiling point substances in the liquid phase are lifted to the top of the tower with the gas, while the liquid gradually falls and the content of high-boiling point components becomes higher and higher, so as to achieve the purpose of distillation. Since the general distillation tower uses the principle of gas-liquid reaction, the conventional tray structure cannot contain cooling equipment, such as cooling coils, which will cause a serious reduction in distillation efficiency.

[0066] Figure 3A stereoscopic diagram showing a schematic arrangement of the structure on a tower plate according to an embodiment of the present invention is shown, wherein strip grooves 22 and a herringbone cap 23 are provided on the tower plate, an inlet overflow weir 25 and an outlet overflow weir 26 are provided on both sides of the tower plate, and a downcomer 27 is provided on the side of the outlet overflow weir 26. Figure 4 For viewing from below Figure 3 A three-dimensional diagram of the device, showing the cooling coil 24 welded below the bottom surface of the tower plate, the inlet overflow weir 25 and the downcomer 27. In the present invention, since the boiling point of the reaction solvent tetrahydrofuran is relatively low, and the synthesis process of the organometallic compound is a process that generates a lot of heat, the contact between the reaction solvent and the reaction liquid should be avoided as much as possible. At present, the production of such active metal organic compounds mainly includes single-kettle batch production and multi-kettle series continuous production. However, the cooling of a single kettle is mainly achieved by heat exchange of the medium in the jacket. However, the heat exchange area of ​​the jacket is limited, and the reaction temperature is not easy to control. Therefore, the raw materials are added dropwise, which is slow and the reaction time is long. According to Figure 3 In the tower tray structure shown in one embodiment of the present invention, strip grooves are opened on the tower tray surface, groove walls and caps are arranged on the strip grooves, and cooling coils are welded under the tower tray surface, so as to prevent the contact between the gas phase (main solvent tetrahydrofuran) and the liquid phase and realize precise control of the temperature of the reaction liquid phase, thereby realizing tower continuous production.

[0067] A reactive metal feed port may be added to each layer of the tower tray. For example, the reactive metal feed port may extend from the tower wall between the inlet and outlet overflow weirs 25 and 26 of each layer of the tower tray to be used for adding metal raw materials to the tower tray in real time. Since the metal raw materials often contain oxides or other impurities, there are many sludge-like residues after the reaction, which are deposited in the structure inside the tower and easily cause poor flow, so it is recommended to clean and flush them thoroughly periodically.

[0068] The tower kettle 3 mainly includes an overflow port 31, a tower bottom outlet 33 and a flushing port 32. The overflow port 31 is used to overflow the clear liquid after the reaction; the flushing port 32 is used to pass the solvent in, flush the bottom residue of the kettle and discharge it from the tower bottom outlet 33.

[0069] The horizontal line in the bottom of the tower 3 indicates that there is reacting liquid in the bottom of the tower.

[0070] The device can be operated at normal pressure or at pressurized pressure.

[0071] Reference below Figure 1 The process of preparing active metal organic compounds using the device according to the present disclosure is specifically described:

[0072] 1) Under the condition of inert gas replacement and protection throughout the tower, the reactant solution is allowed to enter the tower through the feed port 21 of the uppermost tray,

[0073] 2) The inlet overflow weir 25 of the tower tray in step 1) contacts the uniformly scattered metal raw materials on the tower tray and reacts quickly, while the reaction liquid flows to the lower outlet overflow weir 26;

[0074] 3) The reaction releases a large amount of heat, and a cooling medium is introduced into the cooling coil 24 of the tower tray to quickly cool the temperature to a predetermined reaction temperature, thereby preventing a large amount of solvent from being vaporized or the solubility of gaseous reactants from being reduced and escaping, thereby effectively solving the problem of material rushing in the autoclave process;

[0075] 4) The uncondensed gas in step 3) (including vaporized solvent and other gases, such as protective gas argon and N2) rises to the upper tower plate or the tower top through the strip groove 22, is cooled by the cooling coil of the upper tower plate or the tower top, and partially condenses and slides down the cap 23 into the tower plate to continue to participate in the reaction; finally, the uncondensed steam and non-condensable gas leave the tower from the tower top gas outlet 12 and can be collected downstream;

[0076] 5) The reaction liquid obtained in step 2) flows out of the tower tray along the outlet overflow weir 26 and enters the downcomer 27;

[0077] 6) In step 5), the downcomer 27 and the inlet overflow weir of the lower tray form a liquid seal, thereby preventing gas (including organic vapor and non-condensable gas) from entering the downcomer;

[0078] 7) The fresh reactant solution enters the downcomer 27 in step 6) from the feed port of the next tray, mixes with the upper layer of the reaction solution (preferably fully mixed), and then passes over the inlet overflow weir to enter the next tray for reaction;

[0079] 8) Keep the concentration of liquid phase raw materials in each tray not too high to avoid excessive reaction and exceeding the heat exchange capacity of the cooling coil, and repeat steps 2)-7) until the reaction liquid flows into the reactor 2;

[0080] 9) The reaction liquid in step 8) carries some solid residue and settles in the reactor 2, and may also continue to react with a small amount of metal chips in the residue. The settled clear liquid continues to flow out from the overflow port 31, while the sludge-like solid residue accumulates at the bottom;

[0081] 10) When the amount of residue reaches a certain level, close the overflow port 31 in step 9), open the bottom outlet 33 to let the slurry flow out, and open the flushing pipe 32 to flush the bottom of the kettle until the clear liquid is discharged.

[0082] In step 1), the reactant solution includes but is not limited to ether solution or tetrahydrofuran solution of halogenated hydrocarbon (halogenated alkane or halogenated aromatic hydrocarbon) in the synthesis of Grignard reagent; cyclohexane, n-hexane or white oil solution of halogenated hydrocarbon in the synthesis of alkyl lithium, etc.

[0083] In step 2), the metal raw materials include but are not limited to magnesium chips required for Grignard reagent reaction, metal lithium particles required for alkyl lithium synthesis, etc.

[0084] In step 3), the cooling medium includes but is not limited to circulating cooling water, chilled brine, etc.

[0085] Example 1

[0086] Continuous Synthesis of n-Butylmagnesium Chloride Grignard Reagent

[0087] First, the reaction is initiated in the reactor: under argon protection, 5kg of magnesium chips, 1.3kg of 1-chlorobutane, and 15L of tetrahydrofuran are added to a 100L reactor, stirred, heated to 90°C, and 300g of dibromoethane is added for initiation; after successful initiation, the temperature is maintained at 90°C, and 18kg of 1-chlorobutane and 45L of tetrahydrofuran are continuously added dropwise, and after the addition is completed, the temperature is kept for 3-5 hours. The reaction clear liquid is used as the initiator.

[0088] use Figure 1 The device shown. Under the protection of argon in the tower, a tetrahydrofuran solution of 1-chlorobutane with a mass concentration of about 15% and a small amount of the above-prepared reaction clear liquid initiator are added to the feed port of each tower plate respectively, and 1-chlorobutane reacts with magnesium chips on the tower plate and releases heat; at the same time, the circulating cooling water flow rate of each tower plate cooling coil is adjusted to fully cool and exchange heat, and the reaction temperature of each tower plate is kept not more than 95°C. The feed amount and circulating cooling water amount of each tower plate are controlled respectively, so that the reaction liquid on each tower plate is kept slightly boiling and condensate is refluxed, the total feed amount is kept controlled at 20-30kg / h, and the tower top pressure is less than 0.3MPa. After the clear liquid flows out of the overflow port at the bottom of the kettle, sampling and analysis are performed, and the conversion rate of 1-chlorobutane is greater than 90%.

[0089] Example 2

[0090] Continuous Synthesis of n-Butyl Lithium

[0091] use Figure 1 The device shown. Under the protection of inert gas argon, 20-30% mass concentration of 1-chlorobutane cyclohexane solution is added to the feed port of each tower plate respectively, and 1-chlorobutane reacts with the prepared metal lithium particles on the tower plate and releases heat; at the same time, the 7-degree chilled water flow of each tower plate cooling coil is adjusted for cooling and heat exchange, and the reaction temperature of each tower plate is kept not more than 60°C. The feed amount and circulating cooling water amount of each tower plate are controlled respectively, so that the reaction liquid on each tower plate is kept slightly boiling and condensate is refluxed, the total feed amount is kept controlled at 20-30kg / h, and the tower top pressure is less than 0.3MPa. After the clear liquid flows out of the overflow port at the bottom of the kettle, sampling and analysis are performed, and the conversion rate of 1-chlorobutane is greater than 76%.

[0092] The above embodiments are only exemplary embodiments of the present disclosure and are not intended to limit the present disclosure. The protection scope of the present disclosure is defined by the claims. Those skilled in the art may make various modifications or equivalent substitutions to the present disclosure within the essence and protection scope of the present disclosure, and such modifications or equivalent substitutions shall also be deemed to fall within the protection scope of the present disclosure.

Claims

1. A device for preparing metal organic compounds, characterized in that: The device is a multi-layer tray structure, and the whole tower includes three parts: the tower top, the tower middle and the tower bottom, wherein: The tower top includes a condensing coil and a gas outlet, wherein: The condensing coil is arranged inside the tower top, and is used to cool the organic vapor rising to the tower top in the device, condense it and return it to the first layer of tower tray, thereby controlling the temperature of the tower top; The gas outlet is arranged at the top of the tower to discharge uncondensed organic vapor or non-condensable gas; The tower comprises: more than two trays and a feed port corresponding to each tray, wherein: The tower trays are arranged in sequence from top to bottom in the tower for uniformly piling the metal reaction raw materials thereon; An inlet overflow weir and an outlet overflow weir are respectively arranged on both sides of each tray; the inlet overflow weir is slightly higher than the outlet overflow weir to prevent the raw material from directly rushing into the tray; the outlet overflow weir is used to ensure the liquid holding capacity on the tray; the inlet overflow weir and the outlet overflow weir of the lower tray are arranged at positions opposite to those of the inlet overflow weir and the outlet overflow weir of the adjacent upper tray; Each tray has a plurality of grooves, which are capped and serve as channels for the organic vapor and non-condensable gas in the device to rise; the height of the groove wall is not lower than the inlet overflow weir of the tray to ensure that the liquid does not short-circuit from the groove to the next tray; wherein the total area of ​​the grooves on the tray accounts for 15-35% of the tray area; A cooling coil is welded under the bottom of each tray, which is used to cool the reaction liquid on the tray and condense organic vapor; A downcomer is arranged between the outlet overflow weir of the upper tower tray and the inlet overflow weir of the adjacent lower tower tray, and the downcomer cooperates with the inlet overflow weir of the lower tower tray to form a liquid seal; The feed port corresponding to each tray is used to add reaction raw materials, wherein the feed port corresponding to the top tray extends from the tower wall to the outside of the inlet overflow weir and is not higher than the inlet overflow weir, and the feed ports corresponding to other trays extend from the tower wall into the middle and lower part of the downcomer; The tower kettle comprises an overflow port, a tower bottom outlet and a flushing port, wherein: The overflow port is used to overflow the clear liquid after the reaction; The flushing port is used to introduce solvent to flush the bottom residue of the kettle and discharge it from the bottom outlet of the tower.

2. The device according to claim 1, characterized in that The number of the tower plates is 2-6 layers, and the grooves of adjacent tower plates are arranged in a staggered manner.

3. The device according to claim 1, characterized in that The total area of ​​the slots on the tray accounts for 20-35% of the tray area.

4. The device according to claim 1, characterized in that The grooves on the tower plate are parallel strip grooves; the cap is a herringbone or arched cap.

5. The device according to claim 1, characterized in that The cooling coil below the bottom of the tower tray has a cross section of a semicircular series coil half pipe or a triangular series coil half pipe; and / or Independent cooling coils are added between the tower plates.

6. A process for preparing a metal organic compound using the device according to any one of claims 1 to 5, characterized in that: The process comprises: 1) While the whole tower is being replaced with inert gas and protected, the reactant solution is allowed to enter the tower through the feed port of the uppermost tray; 2) the reactant solution passes through the inlet overflow weir of the tower tray in step 1) and contacts with the uniformly scattered metal raw materials on the tower tray to react, and the reaction liquid flows to the lower outlet overflow weir; 3) The reaction is highly exothermic, and a cooling medium is introduced into the cooling coil of the tower tray to cool the temperature to a predetermined reaction temperature, so as to reduce solvent vaporization or escape of gaseous reactants; 4) The solvent and other gases vaporized in step 3) rise to the top of the tower or the upper tower tray through the grooves on the tower tray, are cooled by the cooling coils on the top of the tower or the upper tower tray, and are partially condensed and slide down the cap into the tower tray to continue to participate in the reaction; finally, the uncondensed steam and non-condensable gas leave the tower from the gas outlet at the top of the tower; 5) The reaction liquid in step 2) flows out of the tower tray along the outlet overflow weir and enters the downcomer; 6) In step 5), the downcomer and the inlet overflow weir of the lower tray form a liquid seal, thereby preventing gas from entering the downcomer; 7) The fresh reactant solution enters the downcomer in step 6) from the feed port of the next tray, mixes with the upper layer of the reaction solution, and then passes over the inlet overflow weir to enter the next tray for reaction; 8) Keep the concentration of liquid phase raw materials in each tray not too high to avoid excessive reaction and exceeding the heat exchange capacity of the cooling coil, and repeat steps 2)-7) until the reaction liquid flows into the kettle; 9) The reaction liquid in step 8) carries some solid residues and is allowed to settle in the reactor, the settled clear liquid continuously flows out from the overflow port, and the sludge-like solid residues accumulate at the bottom; 10) When the solid residue accumulates to a certain extent, close the overflow port in step 9), open the bottom outlet to let the slurry flow out, and open the flushing pipe to flush the bottom of the kettle until the clear liquid is discharged.

7. The process according to claim 6, characterized in that In step 1), the reactant solution is an ether solution or a tetrahydrofuran solution of a halogenated hydrocarbon in the synthesis of a Grignard reagent, or a cyclohexane, n-hexane or white oil solution of a halogenated hydrocarbon in the synthesis of an alkyl lithium.

8. The process according to claim 6, characterized in that In step 2), the metal raw material is magnesium chips required for Grignard reagent reaction or metal lithium particles required for alkyl lithium synthesis.

9. The process according to claim 6, characterized in that In step 3), the cooling medium is selected from circulating cooling water and chilled brine.

10. The process according to claim 6, characterized in that The device operates at normal pressure or pressurized pressure.

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