CN111187164B - 6-carbonyl-8-chloro ethyl caprylate synthesis device and method for synthesizing 6-carbonyl-8-chloro ethyl caprylate by using same - Google Patents
6-carbonyl-8-chloro ethyl caprylate synthesis device and method for synthesizing 6-carbonyl-8-chloro ethyl caprylate by using same Download PDFInfo
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Abstract
A6-carbonyl-8-chlorine ethyl caprylate synthesis device and a method for synthesizing 6-carbonyl-8-chlorine ethyl caprylate by the device comprise the following steps: introducing 6-chloro-6-oxoethyl hexanoate, dichloroethane and anhydrous aluminum trichloride which are reaction raw materials into a complexing liquid preparation kettle to obtain a complexing liquid; conveying ethylene to an inlet of an ethylene compressor, conveying the ethylene to an ethylene buffer tank from an opening of the ethylene buffer tank through an outlet pipeline of the ethylene compressor, and conveying the ethylene to a premixer of a reaction mechanism through an outlet pipeline of the ethylene buffer tank to obtain a reaction material to be synthesized; and leading the reaction material to be synthesized in the premixer into the static mixer from the inlet end of the static mixer, leading the reaction material to be synthesized into the heat exchanger from the inlet end of the heat exchanger through the outlet end pipeline of the static mixer, leading the reaction material to be synthesized into the hydrolysis kettle through the outlet end pipeline of the heat exchanger, and obtaining a finished product through layering and distillation. The preparation efficiency is improved, the consistency and stability of the product quality under the continuous flow reaction are ensured, the yield is improved, and the preparation method is energy-saving, environment-friendly and safe.
Description
Technical Field
The invention belongs to the technical field of lipoic acid intermediate synthesis devices, and particularly relates to a 6-carbonyl-8-chloro ethyl caprylate synthesis device and a method for synthesizing 6-carbonyl-8-chloro ethyl caprylate by using the device.
Background
The above-mentioned apparatus for synthesizing ethyl 6-carbonyl-8-chlorooctanoate is substantially a continuous flow synthesis apparatus for ethyl 6-carbonyl-8-chlorooctanoate (the same applies hereinafter), and accordingly, the above-mentioned method for synthesizing ethyl 6-carbonyl-8-chlorooctanoate is substantially a continuous flow synthesis method for ethyl 6-carbonyl-8-chlorooctanoate (the same applies hereinafter).
The english name of ethyl 6-carbonyl-8-chlorooctanoate is: ethyl 8-chloro-6-oxoctanoate, molecular formula: c 10 H 17 O 3 Cl; the molecular weight is: 220.69, is a chemical reaction intermediate, used for synthesizing 6,8-ethyl dichlorooctoate, and the 6,8-ethyl dichlorooctoate is an indispensable important intermediate for synthesizing lipoic acid.
The lipoic acid is a substance which can eliminate aging and pathogenic diseases and is similar to vitamins, can remove free radicals of a matrix, promotes the matrix to synthesize vitamin C by using glucose, can effectively remove melanin, can assist coenzyme to carry out physiological metabolism favorable for the immunity of an organism, is a universal antioxidant medicine, and is widely applied to prevention and treatment of heart diseases, diabetes and senile dementia.
In recent years, with the increasing attention of people to resources, environment and the like, the call for sustainable development, green chemistry, environmental friendliness and the like is rising, so that more severe requirements on energy conservation, emission reduction, consumption reduction and high efficiency are provided in the research, development and production of chemical medicines.
As mentioned above, ethyl 6-carbonyl-8-chlorooctanoate is an important pharmaceutical intermediate in the production of lipoic acid. The chemical structure is shown as the following formula:
the current main method for producing 6-carbonyl-8-chloro ethyl caprylate is as follows: in a reaction kettle, 6-chloro-6-oxoethyl hexanoate is used as a raw material, aluminum trichloride is used as a catalytic action, ethylene gas is introduced for alkylation reaction, and the reaction is carried out in a gas-liquid two-phase environment, and the reaction process needs 2 times of excess ethylene, so that the problems of low production efficiency, unstable product quality and large potential safety hazard of excess ethylene are caused, and the requirements of modern industrial production are not met. However, if the 6-carbonyl-8-chlorooctanoic acid ethyl ester is produced on the basis of meeting the requirements of high yield, low energy consumption, stability and safety and environment protection, reasonable equipment configuration inevitably plays a key role, and the technical scheme to be described below is generated under the background.
Disclosure of Invention
The invention aims to provide a 6-carbonyl-8-chloro ethyl caprylate synthesizing device which is beneficial to meeting the continuous synthesis requirement, providing a foundation for improving the preparation efficiency, ensuring the consistency and stability of the quality of the prepared product, obviously improving the yield, reducing the energy consumption and the emission, embodying the green and environmental protection, and conveniently embodying the safety so as to avoid hidden danger.
The invention also aims to provide a method for synthesizing 6-carbonyl-8-chloro ethyl caprylate by using the 6-carbonyl-8-chloro ethyl caprylate synthesis device, which has the advantages of short process steps, capability of guaranteeing the consistency and stability of the quality, high yield, low energy consumption, less emission, environmental protection and safety, and can be comprehensively embodied.
The invention has the primary task that a 6-carbonyl-8-chloro ethyl caprylate synthesizer comprises a complexing liquid supply mechanism, an ethylene gas supply mechanism and a reaction mechanism, wherein the complexing liquid supply mechanism comprises a complexing liquid preparation kettle, a complexing liquid temporary storage kettle, a complexing liquid metering pump, a damping buffer, a complexing liquid conveying pipeline one-way valve and a mixed liquid conveying pump; the ethylene gas supply mechanism comprises an ethylene compressor, an ethylene buffer tank and an ethylene buffer tank outlet pipeline one-way valve, wherein an ethylene compressor inlet of the ethylene compressor is connected with an ethylene gas supply source pipeline through an ethylene compressor inlet pipeline, an ethylene compressor outlet of the ethylene compressor is connected with an ethylene buffer tank inlet of the ethylene buffer tank through an ethylene compressor outlet pipeline, an ethylene buffer tank outlet of the ethylene buffer tank is connected with the reaction mechanism through an ethylene buffer tank outlet pipeline, and the ethylene buffer tank outlet pipeline one-way valve is connected to an ethylene buffer tank outlet pipeline; the reaction mechanism comprises a premixer, a static mixer, a heat exchanger and a hydrolysis kettle, the premixer is connected with the inlet end of the static mixer, the complex liquid metering pump conveying pipeline and the ethylene buffer tank outlet pipeline are connected with the premixer, the outlet end of the static mixer is connected with the heat exchanger inlet end of the static mixer outlet end pipeline heat exchanger, and the heat exchanger outlet end of the heat exchanger is connected with the hydrolysis kettle through the heat exchanger outlet end pipeline.
In a specific embodiment of the present invention, a complexing liquid preparation kettle discharge port conveying pipe control valve and a complexing liquid preparation kettle discharge port conveying pipe check valve are arranged on the pipeline of the complexing liquid preparation kettle discharge port conveying pipe, and the position of the complexing liquid preparation kettle discharge port conveying pipe check valve on the pipeline of the complexing liquid preparation kettle discharge port conveying pipe is located between the complexing liquid preparation kettle discharge port conveying pipe control valve and the mixed liquid conveying pump inlet of the mixed liquid conveying pump.
In another specific embodiment of the present invention, the damping buffer is a pulse diaphragm type damping buffer with a pressure gauge and used for reducing pulses caused by the complexing liquid metering pump, and a damping buffer connecting pipe check valve is arranged on a pipe of a damping buffer connecting pipe connected with the complexing liquid metering pump conveying pipe of the damping buffer; and a pressure display device and a safety valve are arranged at a discharge port of the complexing liquid metering pump.
In another specific embodiment of the present invention, a hydrolysis kettle inlet and a hydrolysis kettle tail gas outlet are formed at the top of the hydrolysis kettle, a hydrolysis kettle inlet valve is disposed at one end of the heat exchanger outlet end pipeline, which is connected with the hydrolysis kettle inlet, a hydrolysis kettle tail gas outlet is connected with the hydrolysis kettle tail gas outlet, and a tail gas outlet valve is disposed on the hydrolysis kettle tail gas outlet.
In yet another embodiment of the present invention, the static mixer is an SV-type static mixer.
Another object of the present invention is to provide a method for synthesizing ethyl 6-carbonyl-8-chlorooctanoate from an apparatus for synthesizing ethyl 6-carbonyl-8-chlorooctanoate, comprising the steps of:
a) Preparing complex liquid, firstly introducing 6-chloro-6-oxoethyl hexanoate and dichloroethane as reaction raw materials into a complex liquid preparation kettle from a complex liquid preparation kettle feed inlet at the upper part of a complex liquid preparation kettle of a complex liquid supply mechanism through a pipeline, then introducing anhydrous aluminum trichloride into the complex liquid preparation kettle from a complex liquid preparation kettle feed inlet through a pipeline to obtain the complex liquid, then introducing the complex liquid into a mixed liquid conveying pump from a mixed liquid conveying pump inlet through a complex liquid preparation kettle discharge outlet conveying pipe between a complex liquid preparation kettle discharge outlet connected to the bottom of the complex liquid preparation kettle and a mixed liquid conveying pump inlet of the mixed liquid conveying pump, introducing a mixed liquid conveying pump outlet of a mixed liquid conveying pump into the mixed liquid temporary storage kettle from a mixed liquid temporary storage kettle feeding port at the top of the mixed liquid temporary storage kettle through a mixed liquid conveying pump outlet pipeline, introducing the mixed liquid temporary storage kettle into a mixed liquid metering pump liquid inlet of a mixed liquid metering pump through a mixed liquid temporary storage kettle discharging port pipeline connected with a mixed liquid temporary storage kettle discharging port at the bottom of the mixed liquid temporary storage kettle, and conveying the mixed liquid temporary storage kettle into a premixer of a reaction mechanism through a mixed liquid metering pump conveying pipeline, wherein a damping buffer and a mixed liquid conveying pipeline check valve are respectively connected to the mixed liquid metering pump conveying pipeline, and the position of the mixed liquid conveying pipeline check valve on the mixed liquid metering pump conveying pipeline is positioned between the damping buffer and the premixer of the reaction mechanism;
b) Preparing a reaction material to be synthesized, conveying ethylene to an inlet of an ethylene compressor of the ethylene compressor by an inlet pipeline of the ethylene compressor, which is connected with an ethylene gas supply source pipeline and is also connected with an inlet of the ethylene compressor of an ethylene gas supply mechanism, conveying the ethylene to an ethylene buffer tank from an opening of the ethylene buffer tank by an outlet pipeline of the ethylene compressor, which is connected with an outlet of the ethylene compressor, and conveying the ethylene to a premixer of the reaction mechanism by an outlet pipeline of the ethylene buffer tank, which is connected with a check valve of the outlet pipeline of the ethylene buffer tank, so as to obtain the reaction material to be synthesized;
c) And D), synthesizing a finished product, namely leading the reaction material to be synthesized in the premixer in the step B) into a static mixer from the inlet end of the static mixer, leading the reaction material to be synthesized into a heat exchanger from the inlet end of the heat exchanger through a pipeline at the outlet end of the static mixer connected with the outlet end of the static mixer, leading the reaction material to be synthesized into a hydrolysis kettle through a pipeline at the outlet end of the heat exchanger connected with the outlet end of the heat exchanger, and obtaining the 6-carbonyl-8-chloro ethyl caprylate through layering and distillation.
In still another embodiment of the present invention, the mol ratio of ethyl 6-chloro-6-oxohexanoate, anhydrous aluminum trichloride and dichloroethane in the step A) is 1: 1.6-2.5: 8-10; the flow rate of the complexing liquid is 9000-11000ml/min; the pressure of the damping buffer is 0.3-0.7MPa.
In a more specific embodiment of the present invention, the pressure of the ethylene gas in step B) is 0.15 to 0.25MPa greater than the pressure of the damping buffer in step A), and the flow rate of the ethylene gas is 14 to 18L/min; the temperature of the jacket water bath of the static mixer in the step C) is 65-78 ℃, and the retention time of the materials in the static mixer is 15-60s.
In a further specific embodiment of the invention, the temperature of the reaction material to be synthesized after heat exchange by the heat exchanger in step C) is 0 to 25 ℃; the hydrolysis temperature of the hydrolysis kettle is 0-25 ℃.
In a still more specific embodiment of the present invention, the static mixer described in step C) is formed with a hole therein, the hole being a spiral-up hole, and the static mixer is formed by connecting four tubes each having a diameter of DN25mm and a length of 1000mm in series.
The technical scheme provided by the invention has the technical effects that: because the complexing liquid supply mechanism and the ethylene gas supply mechanism are simultaneously connected with the reaction mechanism, the kettle type intermittent reaction in the prior art can be changed into continuous flow reaction, basic guarantee is provided for improving the preparation efficiency, the consistency and the stability of the product quality under the continuous flow reaction can be guaranteed, the yield can be improved, the energy and the cost can be saved, and the emission is reduced, so that the green, environment-friendly and safe effects are realized; the preparation method can introduce raw materials of 6-chloro-6-oxoethyl hexanoate, dichloroethane and anhydrous aluminum trichloride into a complexing liquid preparation kettle to obtain complexing liquid, and then sequentially convey the complexing liquid temporary storage kettle and a complexing liquid metering pump to a reaction mechanism, and further introduce ethylene gas into the reaction mechanism sequentially through an ethylene compressor and a static mixer, so that the 6-chloro-6-oxoethyl hexanoate and ethylene can continuously perform gas-liquid two-phase reaction, the molar ratio consumed by the reaction of the ethylene and the 6-chloro-6-oxoethyl hexanoate can be reduced from 2.4: 1 to 1.3: 1, and the technical effect of the 6-carbonyl-8-chloroethyl octanoate synthesis device can be comprehensively embodied.
Drawings
FIG. 1 is a schematic diagram of a 6-carbonyl-8-ethyl chlorooctanoate synthesis apparatus according to the present invention.
Detailed Description
Example 1:
the method for synthesizing the ethyl 6-carbonyl-8-chlorooctoate by using the synthesis device of the ethyl 6-carbonyl-8-chlorooctoate shown in figure 1 comprises the following steps:
a) Preparing a complexing liquid, firstly, respectively introducing 6-chloro-6-oxoethyl hexanoate and dichloroethane as reaction raw materials into a complexing liquid preparation kettle 11 through respective pipelines, namely a 6-chloro-6-oxoethyl hexanoate conveying pipeline matched with a valve and a dichloroethane conveying pipeline also matched with a valve from a complexing liquid preparation kettle feed port 111 at the upper part of a complexing liquid preparation kettle 11 of a structural system of a complexing liquid supply mechanism 1, as shown in figure 1, the complexing liquid preparation kettle 11 has two sets with completely identical structures so as to fully ensure the uninterrupted conveying of 6-chloro-6-oxoethyl hexanoate and dichloroethane mixture, specifically, when the material in one complexing liquid preparation kettle is used up, starting another material in the complexing liquid preparation kettle, and the complexing liquid preparation kettle which is used up is in a feeding state of the 6-chloro-6-oxoethyl hexanoate conveying pipeline and the dichloroethane conveying pipeline, closing the valve when the mixing kettle is full, so that the complexing liquid is temporarily stored in the complexing liquid preparation kettle and continuously pumped back to a complexing liquid preparation kettle, then introducing the complexing liquid which is not used up into a mixing liquid preparation kettle from a feed port of the compounding kettle through a feeding liquid preparation kettle 12 and conveying pipeline 16, and a mixing liquid conveying kettle from a mixing liquid preparation kettle through a mixing liquid conveying pipeline 161, and a mixing liquid conveying pipeline 12, a complexing liquid temporary storage kettle discharge port pipe 1221 connected to a complexing liquid temporary storage kettle discharge port 122 at the bottom of a complexing liquid temporary storage kettle 12 is led to a complexing liquid metering pump inlet of a complexing liquid metering pump 13, the complexing liquid metering pump inlet is conveyed to a premixer 31 of a reaction mechanism 3 through a complexing liquid metering pump conveying pipe 131, wherein a damping buffer 14 and a complexing liquid conveying pipe check valve 15 are connected to the complexing liquid metering pump conveying pipe 131 respectively, the position of the complexing liquid conveying pipe check valve 15 on the complexing liquid metering pump conveying pipe 131 is located between the damping buffer 14 and the premixer 31 of the reaction mechanism 3, in the present embodiment, the mol ratio of ethyl 6-chloro-6-oxohexanoate, anhydrous aluminum trichloride and dichloroethane is 1: 1.83: 9.5, the flow rate of the complexing liquid is 9000ml/min, the pressure of the damping buffer 14 is 0.5MPa, as shown in fig. 1, a complexing liquid conveying pipe for preparing complexing liquid is provided with a complexing liquid conveying pipe 1121 on a complexing liquid temporary storage kettle delivery pipe 1121, a pulse check valve for controlling the position of the complexing liquid conveying pipe 131 and a complexing liquid conveying pipe is provided on the complexing liquid conveying pipe 1121 for preparing a complexing liquid, and a complexing liquid conveying pipe 12, and a pulse buffer conveying pipe 12 is provided with a damping buffer delivery port for preparing a damping buffer 12, and a damping buffer delivery pipe 12 is provided with a damping buffer delivery port for preparing a damping buffer delivery control a damping buffer delivery pipe 12, and a damping buffer delivery pipe 1121 connecting pipe 12, and a damping buffer delivery port for preparing a damping buffer delivery pipe 12, and a damping buffer delivery pipe 12 is provided on a damping buffer delivery pipe 12, and a pressure display device 132 (such as a pressure gauge) and a safety valve 133 are provided at the position of the outlet of the complexing liquid metering pump 13;
b) Preparing a reactant to be synthesized, delivering ethylene, i.e. ethylene gas, to the ethylene compressor inlet 211 of the ethylene compressor 21 through an ethylene compressor inlet pipe 2111 connected to an ethylene gas supply source, e.g. an ethylene gas storage tank pipe, and also connected to the ethylene compressor inlet 211 of the ethylene compressor 21 of the structural system of the ethylene gas supply mechanism 2, delivering the ethylene, i.e. ethylene gas, to the ethylene buffer tank 22 from an ethylene buffer tank port 221 through an ethylene compressor outlet pipe 2121 connected to an ethylene compressor outlet 212 of the ethylene compressor 21, and delivering the ethylene to the premixer 31 of the reaction mechanism 3 through an ethylene buffer tank outlet pipe 2221 connected to an ethylene buffer tank outlet 222 of the ethylene buffer tank 22, to obtain the reactant to be synthesized, wherein an ethylene buffer tank outlet pipe check valve 23 is connected to the ethylene buffer tank outlet pipe 2221, as can be known from the description of the present step and the description of step a): the material entering the premixer 31 in the step A) is in a liquid phase, while the material entering the premixer 31 in the step B) is in a gas phase, and the reaction material to be synthesized is formed by the gas-liquid two-phase material, wherein the pressure of the ethylene gas in the step is controlled to be 0.5MPa, the pressure of the damping buffer 14 is 0.35MPa, namely the pressure of the ethylene gas is 0.15MPa greater than the pressure of the damping buffer 14 in the step A), and the flow rate of the ethylene gas in the step is 16L/min;
c) Synthesizing a finished product, namely leading the reaction material to be synthesized in the premixer 31 in the step B) into the static mixer 32 from the inlet end of the static mixer 32, leading the reaction material to be synthesized into the heat exchanger 33 from the inlet end of the heat exchanger through a pipeline 321 at the outlet end of the static mixer connected with the outlet end of the static mixer 32, leading the reaction material to be synthesized into the hydrolysis kettle 34 through a pipeline 331 at the outlet end of the heat exchanger connected with the outlet end of the heat exchanger 33, layering and distilling to obtain the finished product, namely the 6-carbonyl-8-ethyl chlorooctoate, wherein the gas-phase analysis purity of the 6-carbonyl-8-ethyl chlorooctoate is 97.69%, the unreacted raw material is 1.93%, and the impurity is 0.37%, the water bath temperature of a jacket of the static mixer 32 in the step is 70 ℃, the retention time of the material in the static mixer 32 is controlled to be 40s, the temperature of the reaction material to be synthesized after heat exchange by the heat exchanger 33 is 5 ℃, the hydrolysis temperature of the hydrolysis kettle 34 is 0 ℃, a pore passage is formed inside the static mixer 32, the pore passage is a spiral rising pore passage, the static mixer 32 is formed by connecting four pipes with the pipe diameters of DN25mm and the lengths of 1000mm in series, as shown in fig. 1, a hydrolysis kettle material inlet 341 and a hydrolysis kettle tail gas outlet 342 are formed at the top of the hydrolysis kettle 34, a hydrolysis kettle material inlet valve 3311 is arranged at one end of the heat exchanger outlet end pipeline 331 matched and connected with the hydrolysis kettle material inlet 341, a hydrolysis kettle tail gas outlet pipe 3421 is matched and connected with the hydrolysis kettle tail gas outlet 342, and a tail gas outlet valve 34211 is arranged on the hydrolysis kettle tail gas outlet pipe 3421.
Example 2:
only changing the mol ratio of the 6-chloro-6-oxoethyl hexanoate, the anhydrous aluminum trichloride and the dichloroethane in the step A) to 1: 1.6: 10, changing the flow of the complexing liquid to 11000L/min, and changing the pressure of the damping buffer 14 to 0.7MPa; only changing the pressure of the ethylene gas in the step B) to 0.8MPa, changing the pressure of the damping buffer 14 to 0.6MPa, wherein the pressure of the ethylene gas is 0.2MPa higher than the pressure of the damping buffer 14, and changing the flow rate of the ethylene gas to 14L/min; only the jacket water bath temperature of the static mixer 32 in the step C) was changed to 65 ℃, the residence time of the material in the static mixer 32 was changed to 60s, the temperature of the reaction material to be synthesized after heat exchange by the heat exchanger 33 was changed to 25 ℃, the hydrolysis temperature of the hydrolysis kettle 34 was changed to 10 ℃, the gas phase analytical purity of ethyl 6-carbonyl-8-chlorooctanoate was 96.07%, the unreacted raw material was 3.48%, and the impurities were 0.44%, and the rest was the same as described in example 1.
Example 3:
only changing the mol ratio of the 6-chloro-6-oxoethyl hexanoate, the anhydrous aluminum trichloride and the dichloroethane in the step A) to 1: 2.5: 8, changing the flow of the complexing liquid to 10000L/min, and changing the pressure of the damping buffer 14 to 0.3MPa; only changing the pressure of the ethylene gas in the step B) to 0.9MPa, changing the pressure of the damping buffer 14 to 0.65MPa, wherein the pressure of the ethylene gas is 0.25MPa greater than the pressure of the damping buffer 14, and changing the flow rate of the ethylene gas to 18L/min; only the jacket water bath temperature of the static mixer 32 in the step C) was changed to 78 ℃, the residence time of the material in the static mixer 32 was changed to 15s, the temperature of the reaction material to be synthesized after heat exchange by the heat exchanger 33 was changed to 10 ℃, the hydrolysis temperature of the hydrolysis kettle 34 was changed to 25 ℃, the gas phase analytical purity of ethyl 6-carbonyl-8-chlorooctanoate was 96.43%, the unreacted raw material was 4.22%, and the impurities were 0.6%, and the rest was the same as described in example 1.
Claims (6)
1. A method for synthesizing 6-carbonyl-8-chloro ethyl caprylate is characterized by comprising the following steps: a) Preparing complexing liquid, firstly introducing 6-chloro-6-oxoethyl hexanoate and dichloroethane as reaction raw materials into a complexing liquid preparation kettle (11) from a complexing liquid preparation kettle feed port (111) at the upper part of a complexing liquid preparation kettle (11) of a complexing liquid supply mechanism (1) through a pipeline, then introducing anhydrous aluminum trichloride into the complexing liquid preparation kettle (11) from the complexing liquid preparation kettle feed port (111) through a pipeline to obtain complexing liquid, then introducing the complexing liquid into a mixed liquid conveying pump (16) from a mixed liquid inlet of the mixed liquid preparation kettle through a complexing liquid preparation kettle discharge port conveying pipe (1121) connected between a complexing liquid preparation kettle discharge port (112) at the bottom of the complexing liquid preparation kettle (11) and a mixed liquid conveying pump inlet of the mixed liquid conveying pump (16), introducing the mixed liquid into the complexing liquid conveying pump (16) from a mixed liquid inlet of the mixed liquid conveying pump through a mixed liquid conveying pump inlet (121) at the top of the complexing liquid preparation kettle through a mixed liquid conveying pump feed port (161) connected with the mixed liquid conveying pump discharge port of the mixed liquid conveying pump (16) from a complexing liquid kettle feed port (121) at the top of the complexing liquid temporary storage kettle (12) through a mixing liquid conveying pump pipeline (122) to a metering pump through a metering pump mechanism (13) connected with the bottom of the complexing liquid mixing kettle (1) through a metering pump of the complexing liquid conveying mechanism, and a metering pump (13) through a metering pump, and a metering pump connected with the complexing liquid conveying pump (31) at the bottom of the complexing liquid mixing kettle (13) through a metering pump of the complexing liquid mixing kettle, wherein, a damping buffer (14) and a complexing liquid conveying pipeline one-way valve (15) are respectively connected on the complexing liquid metering pump conveying pipeline (131), and the position of the complexing liquid conveying pipeline one-way valve (15) on the complexing liquid metering pump conveying pipeline (131) is positioned between the damping buffer (14) and the premixer (31) of the reaction mechanism (3);
b) Preparing a reaction material to be synthesized, delivering ethylene to an ethylene compressor inlet (211) of an ethylene compressor (21) by an ethylene compressor inlet pipeline (2111) connected with an ethylene gas supply source pipeline and simultaneously connected with an ethylene compressor inlet (211) of an ethylene compressor (21) of an ethylene gas supply mechanism (2), delivering the ethylene to an ethylene buffer tank (22) from an ethylene buffer tank port (221) through an ethylene compressor outlet pipeline (2121) connected with an ethylene compressor outlet (212) of the ethylene compressor (21), and delivering the ethylene to a premixer (31) of a reaction mechanism (3) through an ethylene buffer tank outlet pipeline (2221) connected with an ethylene buffer tank outlet (222) of the ethylene buffer tank (22), wherein an ethylene buffer tank outlet pipeline one-way valve (23) is connected to the ethylene buffer tank outlet pipeline (2221) to obtain the reaction material to be synthesized;
c) Synthesizing a finished product, namely leading the reaction material to be synthesized in the premixer (31) in the step B) into the static mixer (32) from the inlet end of the static mixer (32), leading the reaction material to be synthesized into the heat exchanger (33) from the inlet end of the heat exchanger (33) through a static mixer outlet end pipeline (321) connected with the outlet end of the static mixer (32), leading the reaction material to be synthesized into the hydrolysis kettle (34) through a heat exchanger outlet end pipeline (331) connected with the heat exchanger outlet end of the heat exchanger (33), and obtaining the 6-carbonyl-8-chlorooctanoic acid ethyl ester through layering and distillation;
the mol ratio of the 6-chloro-6-oxoethyl hexanoate, the anhydrous aluminum trichloride and the dichloroethane in the step A) is 1: 1.6-2.5: 8-10; the flow rate of the complexing liquid is 9000-11000ml/min; the pressure of the damping buffer (14) is 0.3-0.7MPa;
the pressure of the ethylene gas in the step B) is 0.15-0.25MPa greater than that of the damping buffer (14) in the step A), and the flow rate of the ethylene gas is 14-18L/min; the temperature of the jacket water bath of the static mixer (32) in the step C) is 65-78 ℃, and the retention time of the materials in the static mixer (32) is 15-60s;
the temperature of the reaction material to be synthesized after heat exchange of the heat exchanger (33) in the step C) is 0-25 ℃; the hydrolysis temperature of the hydrolysis kettle (34) is 0-25 ℃;
a pore canal is formed inside the static mixer (32) in the step C), the pore canal is a spiral ascending pore canal, and the static mixer (32) is formed by connecting four pipes with the pipe diameter of DN25mm and the length of 1000mm in series.
2. An apparatus for carrying out the method according to claim 1, characterized by comprising a complexing liquid supply means (1), an ethylene gas supply means (2) and a reaction means (3), wherein the complexing liquid supply means (1) comprises a complexing liquid preparation tank (11), a complexing liquid temporary storage tank (12), a complexing liquid metering pump (13), a damping buffer (14), a complexing liquid delivery line check valve (15) and a mixed liquid delivery pump (16), wherein a complexing liquid preparation tank feed port (111) is provided in the upper part of the complexing liquid preparation tank (11), and a complexing liquid preparation tank discharge port (112) is formed in the bottom of the complexing liquid preparation tank (11), the complexing liquid preparation tank discharge port (112) is connected to a mixed liquid delivery pump inlet of the mixed liquid delivery pump (16) through a complexing liquid preparation tank discharge port delivery pipe (1121), and the mixed liquid delivery pump feed port of the mixed liquid delivery pump (16) is connected to a mixed liquid delivery pump inlet of the top temporary storage tank (121) of the complexing liquid temporary storage tank (12) through a mixed liquid delivery pipe (161), and the mixed liquid delivery pump outlet of the mixed liquid delivery pump (121) is connected to a mixed liquid metering pump inlet of the mixed liquid preparation tank (13) through a complexing liquid delivery pipe (131), and the mixed liquid metering pump (13) of the bottom of the complexing liquid preparation tank (13), the damping buffer (14) and the complexing liquid conveying pipeline one-way valve (15) are connected to a complexing liquid metering pump conveying pipeline (131), wherein the position of the complexing liquid conveying pipeline one-way valve (15) on the complexing liquid metering pump conveying pipeline (131) is positioned between the damping buffer (14) and the reaction mechanism (3); the ethylene gas supply mechanism (2) comprises an ethylene compressor (21), an ethylene buffer tank (22) and an ethylene buffer tank outlet pipeline one-way valve (23), wherein an ethylene compressor inlet (211) of the ethylene compressor (21) is connected with an ethylene gas supply source pipeline through an ethylene compressor inlet pipeline (2111), an ethylene compressor outlet (212) of the ethylene compressor (21) is connected with an ethylene buffer tank port (221) of the ethylene buffer tank (22) through an ethylene compressor outlet pipeline (2121), an ethylene buffer tank outlet (222) of the ethylene buffer tank (22) is connected with the reaction mechanism (3) through an ethylene buffer tank outlet pipeline (2221), and the ethylene buffer tank outlet pipeline one-way valve (23) is connected to the ethylene buffer tank outlet pipeline (2221); the reaction mechanism (3) comprises a premixer (31), a static mixer (32), a heat exchanger (33) and a hydrolysis kettle (34), wherein the premixer (31) is connected with the inlet end of the static mixer (32), the complex liquid metering pump conveying pipeline (131) and the ethylene buffer tank outlet pipeline (2221) are connected with the premixer (31), the outlet end of the static mixer (32) is connected with the heat exchanger inlet end of the heat exchanger (33) through the static mixer outlet end pipeline (321), and the heat exchanger outlet end of the heat exchanger (33) is connected with the hydrolysis kettle (34) through the heat exchanger outlet end pipeline (331).
3. The apparatus according to claim 2, wherein a complex liquid preparation kettle discharge port delivery pipe control valve (11211) and a complex liquid preparation kettle discharge port delivery pipe check valve (11212) are disposed on the pipeline of the complex liquid preparation kettle discharge port delivery pipe (1121), and the position of the complex liquid preparation kettle discharge port delivery pipe check valve (11212) on the pipeline of the complex liquid preparation kettle discharge port delivery pipe (1121) is located between the complex liquid preparation kettle discharge port delivery pipe control valve (11211) and the mixed liquid delivery pump inlet of the mixed liquid delivery pump (16).
4. The device according to claim 2, characterized in that the damping buffer (14) is a pulse diaphragm type damping buffer with a pressure gauge for reducing the pulse caused by the complexing liquid metering pump (13), and a damping buffer connecting pipe check valve (1411) is arranged on the damping buffer connecting pipe (141) of the damping buffer (14) connected with the complexing liquid metering pump conveying pipe (131); and a pressure display device (132) and a safety valve (133) are arranged at the discharge hole of the complexing liquid metering pump (13).
5. The device according to claim 2, wherein a hydrolysis vessel inlet (341) and a hydrolysis vessel tail gas outlet (342) are formed at the top of the hydrolysis vessel (34), a hydrolysis vessel inlet valve (3311) is disposed at one end of the heat exchanger outlet pipeline (331) connected to the hydrolysis vessel inlet (341), a hydrolysis vessel tail gas outlet (3421) is connected to the hydrolysis vessel tail gas outlet (342), and a tail gas outlet valve (34211) is disposed on the hydrolysis vessel tail gas outlet (3421).
6. The apparatus of claim 2 wherein said static mixer is an SV type static mixer.
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| CN108774209A (en) * | 2018-08-03 | 2018-11-09 | 苏州富士莱医药股份有限公司 | A method of lipoic acid ethyl ester is prepared using tubular reactor |
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| CN108774209A (en) * | 2018-08-03 | 2018-11-09 | 苏州富士莱医药股份有限公司 | A method of lipoic acid ethyl ester is prepared using tubular reactor |
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