CN217450115U - Production system of 8-chloro-6-oxo-ethyl octanoate - Google Patents
Production system of 8-chloro-6-oxo-ethyl octanoate Download PDFInfo
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- CN217450115U CN217450115U CN202221516037.6U CN202221516037U CN217450115U CN 217450115 U CN217450115 U CN 217450115U CN 202221516037 U CN202221516037 U CN 202221516037U CN 217450115 U CN217450115 U CN 217450115U
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Abstract
The utility model discloses a production system of 8-chlorine-6-oxo octanoic acid ethyl ester, including first microchannel reactor, second microchannel reactor and the third microchannel reactor of establishing ties in proper order, second microchannel reactor and third microchannel reactor are all placed in ultrasonic device, and wherein, be equipped with the feed inlet on the first microchannel reactor, this feed inlet links to each other with adipic acid monoethyl ester head tank and thionyl chloride head tank respectively, are equipped with the raw materials import on the second microchannel reactor, and this raw materials import links to each other with the aluminium trichloride head tank, is equipped with the air inlet on the third microchannel reactor, the air inlet links to each other with the ethylene storage tank. The production system has the advantages of high degree of mechanization, rapidness, high efficiency, environmental protection, economy, practicality, simple operation, low cost, higher yield and the like.
Description
Technical Field
The utility model provides a production system of 8-chlorine-6-oxo octanoic acid ethyl ester specifically provides a system based on microchannel ultrasonic technology produces 8-chlorine-6-oxo octanoic acid ethyl ester.
Background
The 8-chloro-6-oxo ethyl caprylate is an upstream product of the 6, 8-dichloro ethyl caprylate, the 6, 8-dichloro ethyl caprylate is an important organic intermediate for synthesizing the lipoic acid, and the lipoic acid is called as a universal antioxidant, is widely used for treating and preventing various diseases such as heart disease, diabetes, Alzheimer's disease and the like, and has wide market prospects in China and in China.
Currently, ethyl 8-chloro-6-oxooctanoate is generally obtained by Friedel-crafts reaction of an acid chloride and ethylene in the presence of aluminum chloride. The Friedel-Crafts reaction is a general name of Friedel-Crafts alkylation (Friedel-Crafts alkylation) and Friedel-Crafts acylation (Friede-Crafts acylation), and is called Friedel-Crafts reaction or FC reaction for short. In the traditional Friedel-crafts reaction operation, the needed acyl chloride needs to be prepared as before, the temperature needs to be strictly controlled, and the operation is complex; when ethylene gas is introduced in the Friedel-crafts reaction, inevitable waste gas is discharged, and the ethylene gas is difficult to recover. In addition, the problem of heterogeneous mixing is always the reaction difficulty of the reaction, and the traditional bubbling mode is far from achieving sufficient mixing effect. Therefore, the heterogeneous reaction also becomes a hot spot to be solved in the flow chemistry process.
Furthermore, all reagents such as acyl chloride and aluminum trichloride used in the friedel-crafts reaction need to be operated under strict anhydrous conditions, which is a difficult operation difficulty for the traditional kettle type process, and the instability of the reagents causes the problems of poor reproducibility, low yield, low purity and the like of the reactions.
SUMMERY OF THE UTILITY MODEL
To the loaded down with trivial details of operation that present 8-chlorine-6-oxo octanoic acid ethyl ester production process exists, reaction conditions are harsh, degree of mechanization low grade is not enough, the utility model provides a production system of 8-chlorine-6-oxo octanoic acid ethyl ester, this production system introduce microchannel reactor and ultrasonic device, utilize microchannel ultrasonic technology to produce 8-chlorine-6-oxo octanoic acid ethyl ester, this production system can realize the reaction fast under the lower temperature, have that degree of mechanization is high, quick high efficiency, easy operation, advantage such as with low costs.
The utility model discloses specific technical scheme as follows:
the production system of the 8-chloro-6-oxo ethyl octanoate comprises a first micro-channel reactor, a second micro-channel reactor and a third micro-channel reactor which are sequentially connected in series, wherein the second micro-channel reactor and the third micro-channel reactor are both placed in an ultrasonic device, a feed inlet is formed in the first micro-channel reactor and is respectively connected with a monoethyl adipate raw material tank and a thionyl chloride raw material tank, a raw material inlet is formed in the second micro-channel reactor and is connected with an aluminum trichloride raw material tank, an air inlet is formed in the third micro-channel reactor and is connected with an ethylene storage tank.
Furthermore, the microchannel reactor has two functions, one is to fully mix the raw materials, and the other is to perform partial reaction during the mixing process of the raw materials. The raw materials enter the microchannel reactor, so that the raw materials can be quickly and automatically mixed, and the defects of long charging time, complex operation and the like of the traditional batch type kettle reactor are overcome. The first microchannel reactor, the second microchannel reactor and the third microchannel reactor can be various types of microchannel reactors, preferably plate microchannel reactors, and more preferably clamping plate microchannel reactors. The sandwich-type microchannel reactor is provided with a heat exchange channel connected with a cooling circulator, wherein the heat exchange channel is internally provided with a cooling liquid which circularly flows, and the cooling liquid can be cold ethanol and the like.
Furthermore, the first microchannel reactor, the second microchannel reactor and the third microchannel reactor are all provided with a feeding hole and a discharging hole, and the number of the feeding holes can be one or two or more. The discharge port of the first microchannel reactor is connected with the feed port of the second microchannel reactor, and the discharge port of the second microchannel reactor is connected with the feed port of the third microchannel reactor.
Further, the microchannel structures in the first microchannel reactor and the second microchannel reactor may be in different shapes such as a tubular structure, a Y-shaped structure, a heart-shaped structure, an M-shaped structure, a clip-shaped structure, and the like.
Furthermore, in the third microchannel reactor, the upper microchannel structure is a Y-shaped structure, a heart-shaped structure, an M-shaped structure or a square-shaped structure, and the lower microchannel structure is a column array structure. The structure is more beneficial to the good contact and reaction of gas, solid and liquid phases, and improves the reaction efficiency and the conversion rate of raw materials.
Further, the third microchannel reactor is also provided with a gas outlet, and the gas outlet is connected with the gas absorption kettle and used for receiving redundant gas in the reaction.
Furthermore, the third microchannel reactor is vertically installed, the air inlet is arranged at the bottom of the third microchannel reactor, and the air outlet is arranged at the top of the third microchannel reactor. The top of the third microchannel reactor is also provided with a feed inlet, and the feed inlet is connected with the second microchannel reactor. The arrangement mode has the advantages that gas is introduced from the lower part, dispersed through the column array type micro-channels, liquid is introduced from the upper part, falls under the action of gravity, and is dispersed through the upper micro-channels, finally, a mixed state of micro gas flow and micro liquid drops is formed, the contact is more thorough, and the reaction efficiency and the conversion rate of raw materials are improved. After the reaction is finished, the liquid flows out from the lower part, and the gas flows out from the upper gas path and is absorbed by the gas absorption tank.
Furthermore, a discharge port is also arranged on the third microchannel reactor and is connected with the material receiving kettle.
Furthermore, in the column array part of the third microchannel reactor, the diameter of the array micropores is 1.5-2.5mm, and the density of the micropores is 20-30/cm 2 The gas is dispersed into a micro gas flow after entering from the lower part, is connected with the upper micro channel, fully contacts and reacts with the liquid in the upper micro channel, and is finally discharged from the upper part.
Furthermore, the second microchannel reactor and the third microchannel reactor are arranged in the ultrasonic device, can be arranged in one ultrasonic device, and can also be arranged in two ultrasonic devices, and the size of the ultrasonic devices can be adjusted according to requirements.
Furthermore, the monoethyl adipate solution is contained in the monoethyl adipate raw material tank, the thionyl chloride solution is contained in the thionyl chloride raw material tank, and the thionyl chloride solution is used for preparation at present. The ethyl adipate raw material tank is connected with the first microchannel reactor through a pipeline, a first infusion pump is arranged on the pipeline, the thionyl chloride raw material tank is connected with the first microchannel reactor through a pipeline, and a second infusion pump is arranged on the pipeline. The raw materials in the two raw material tanks are pumped into the first microchannel reactor by an infusion pump. And the adipic acid monoethyl ester raw material tank and the thionyl chloride raw material tank are respectively connected with a feed inlet of the first microchannel reactor.
Further, what hold in the aluminium trichloride feed tank is aluminium trichloride solution, is equipped with agitating unit in the aluminium trichloride feed tank to guarantee that the material is dispersed evenly in the feed tank.
Furthermore, a heat-preservation jacket is arranged on the aluminum trichloride raw material tank, and cooling liquid is arranged in the jacket to ensure that the temperature of the material is within the range of 0-10 ℃.
Furthermore, a third infusion pump is arranged on a pipeline connecting the aluminum trichloride raw material tank and the second microchannel reactor. Pumping the aluminum trichloride solution into a second microchannel reactor by a third infusion pump.
Further, a gas flowmeter is arranged on a pipeline connecting the ethylene storage tank and the third microchannel reactor.
The utility model discloses utilize the high-efficient mass transfer heat transfer principle of microchannel technique, go into the intensive mixing in the microchannel reactor with the reaction raw materials earlier pump, then react under the ultrasonic action in getting into subsequent microchannel reactor in succession, the reaction liquid flows out in the microchannel reactor in succession, the reaction liquid of outflow gets into to connect and stores in the material cauldron. The utility model discloses production system compares with traditional batch type cauldron formula reaction and has that degree of mechanization is high, high efficiency, green, economical and practical, easy operation, with low costs, advantage such as productivity is higher.
Drawings
FIG. 1 is a schematic structural diagram of a production system of ethyl 8-chloro-6-oxooctanoate according to the present invention.
In the figure, 1, a raw material tank of monoethyl adipate, 2, a raw material tank of thionyl chloride, 3, a first infusion pump, 4, a second infusion pump, 5, a first micro-channel reactor, 6, a raw material tank of aluminum trichloride, 7, a third infusion pump, 8, a second micro-channel reactor, 9, an ethylene storage tank, 10, a gas flowmeter, 11, a third micro-channel reactor, 12, a gas absorption kettle and 13, a material receiving kettle.
Detailed Description
The present invention will be described in detail below with reference to the accompanying drawings and specific embodiments. The following description is exemplary only, and is not intended to limit the scope thereof.
Example 1
The production system of ethyl 8-chloro-6-oxo-octanoate shown in fig. 1 comprises a first microchannel reactor, a second microchannel reactor and a third microchannel reactor which are sequentially connected in series, wherein the first microchannel reactor is provided with two feed inlets and a discharge outlet, the second microchannel reactor is provided with a feed inlet, a raw material inlet and a discharge outlet, the top of the third microchannel reactor is provided with a feed inlet and an air outlet, and the bottom of the third microchannel reactor is provided with an air inlet and a discharge outlet. This production system still includes adipic acid monoethyl ester head tank 1 and thionyl chloride head tank 2, adipic acid monoethyl ester head tank and thionyl chloride head tank link to each other through the feed inlet of pipeline with first microchannel reactor 5 respectively, are equipped with first transfer pump 3 on the pipeline that adipic acid monoethyl ester head tank and first microchannel reactor link to each other, are equipped with second transfer pump 4 on the pipeline that thionyl chloride head tank and first microchannel reactor link to each other. The discharge port of the first microchannel reactor 5 is connected with the feed port of the second microchannel reactor 8, the raw material inlet of the second microchannel reactor is connected with the aluminum trichloride raw material tank 6, the second microchannel reactor 8 is arranged in the ultrasonic device, the discharge port of the second microchannel reactor is connected with the feed port of the third microchannel reactor 11, the third microchannel reactor is also arranged in the ultrasonic device, the third microchannel reactor is vertically installed, the gas outlet of the third microchannel reactor is connected with the gas absorption kettle 12, the gas inlet of the third microchannel reactor is connected with the ethylene storage tank 9, and the discharge port of the third microchannel reactor is connected with the material receiving kettle 13.
Furthermore, the first microchannel reactor and the second microchannel reactor are sandwich-type microchannel reactors with heat exchange channels, the texture of the reaction plate, i.e. the microchannel structure, is in a 'return' shape, the heat exchange channels are arranged in the sandwich-type microchannel reactors, and cooling liquid which flows circularly is arranged in the heat exchange channels, and can be cold ethanol and the like. In addition to the microchannel reactor of the microchannel structure, the first microchannel reactor and the second microchannel reactor may also adopt other microchannel structures, such as a tubular structure, a heart-shaped structure, an M-shaped structure, a Y-shaped structure, and the like.
Furthermore, the third microchannel reactor is a clamping plate type microchannel reactor, the upper microchannel structure of the third microchannel reactor is of a 'return' type, and the lower microchannel structure of the third microchannel reactor is of a column type array structure, wherein the column type array structure refers to that a plurality of columnar microchannels are arranged in an array type. The micro-channel structure above the micro-channel structure can be a heart-shaped structure, an M-shaped structure and a Y-shaped structure besides the 'return' structure.
Furthermore, in the column array part of the third microchannel reactor, the diameter of the array micropores is 1.5-2.5mm, and the density of the micropores is 20-30/cm 2 And the gas enters the column-type array microchannel from the lower part and is dispersed into a micro gas flow, so that the full contact reaction with the liquid is facilitated.
Furthermore, the aluminum trichloride raw material tank is provided with a heat-insulating jacket, and cooling liquid is arranged in the jacket and is cold ethanol and the like. Still be equipped with agitating unit in the aluminium trichloride head tank. And a third material conveying pump 7 is arranged on a pipeline connecting the aluminum trichloride raw material tank and the second micro-channel reactor.
Further, a gas flowmeter 10 is arranged on a pipeline connecting the ethylene storage tank and the second microchannel reactor, is used for controlling the flow rate, and is connected with a one-way valve to protect the gas flowmeter.
Further, the gas absorption kettle can be externally connected with circulating water to ensure the gas absorption efficiency.
The use mode of the production system is as follows:
1. adding an organic solvent solution of monoethyl adipate into a raw material tank of monoethyl adipate, and adding an organic solvent solution of thionyl chloride into a raw material tank of thionyl chloride, wherein the organic solvent can be dichloromethane, dichloroethane, toluene and the like.
2. Pumping the adipic acid monoethyl ester solution and the thionyl chloride solution into a first microchannel reactor according to a certain flow rate, and keeping the equivalent ratio of the oxalic acid monoethyl ester to the thionyl chloride at 1: 1.2-1.5, the temperature of the microchannel reactor is 45-65 ℃, and the retention time of the material is 8-12 min.
3. The material enters a second microchannel reactor of the ultrasonic device, the ultrasonic device is started, the temperature of the reactor is kept between 0 and 10 ℃, and the retention time of the material in the second microchannel reactor is kept between 5 and 10 minutes through the control of the flow rate of the material and the like.
4. The material enters a third microchannel reactor arranged in an ultrasonic device from the top, the ultrasonic device is started, the temperature of the reactor is kept at 25-35 ℃, meanwhile, ethylene gas is introduced from the bottom of the third microchannel reactor, the flow rate of the ethylene gas is controlled to be 150-200 ml/min through a gas flow meter, and the retention time of the material in the third microchannel reactor is kept to be 5-10 min through the control of the flow rate of the material and the like.
5. The material continuously flows out of the micro-channel ultrasonic reactor and continuously flows into the material receiving kettle. And quenching the materials in the material receiving kettle by ice water, separating liquid, extracting an organic phase by dichloromethane, washing with salt, drying, purifying by column chromatography and the like to obtain a white solid, namely the ethyl 8-chloro-6-oxooctoate product.
According to the production system, a delivery pump is used for inputting a monoethyl adipate solution and a thionyl chloride solution into a first micro-channel reactor at a low temperature, nucleophilic substitution is carried out in a pipeline to generate an acyl chloride intermediate, the acyl chloride intermediate and an organic solvent turbid solution of aluminum trichloride are mixed in a second micro-channel reactor, and a mixed solution after mixing is continuously subjected to Friedel-crafts alkylation reaction with ethylene gas introduced from the lower end in a third micro-channel reactor. After the reaction is finished, the reaction solution is post-treated to obtain the product of 8-chloro-6-oxo-ethyl octanoate. The production system utilizes the combination of the high-efficiency mass and heat transfer principle of the microchannel technology and the ultrasonic reaction technology to accelerate the gas-liquid mixing effect, and the whole production process is quick and efficient, green, economical and practical, and has good industrial application prospect.
Claims (10)
1. A production system of 8-chloro-6-oxo-ethyl octanoate is characterized in that: including first microchannel reactor, second microchannel reactor and the third microchannel reactor of establishing ties in proper order, second microchannel reactor and third microchannel reactor are all placed in ultrasonic device, and wherein, be equipped with the feed inlet on the first microchannel reactor, this feed inlet links to each other with adipic acid monoethyl ester head tank and thionyl chloride head tank respectively, are equipped with the raw materials import on the second microchannel reactor, and this raw materials import links to each other with aluminium trichloride head tank, is equipped with the air inlet on the third microchannel reactor, the air inlet links to each other with the ethylene storage tank.
2. The production system of claim 1, wherein: the first microchannel reactor, the second microchannel reactor and the third microchannel reactor are plate microchannel reactors.
3. The production system according to claim 1 or 2, wherein: the microchannel structures in the first microchannel reactor and the second microchannel reactor are tubular structures, Y-shaped structures, heart-shaped structures, M-shaped structures or clip-shaped structures.
4. The production system of claim 1, wherein: in the third microchannel reactor, the upper microchannel structure is a Y-shaped structure, a heart-shaped structure, an M-shaped structure or a clip-shaped structure, and the lower microchannel structure is a columnar array structure.
5. The production system of claim 4, wherein: in the column array part of the third microchannel reactor, the diameter of the array micropores is 1.5-2.5mm, and the density of the micropores is 20-30/cm 2 。
6. The production system according to claim 1, 4 or 5, wherein: the third microchannel reactor is vertically mounted.
7. The production system of claim 6, wherein: and the top of the third microchannel reactor is provided with a gas outlet, and the gas outlet is connected with the gas absorption kettle.
8. The production system of claim 6, wherein: and a discharge port is arranged at the bottom of the third microchannel reactor and is connected with the material receiving kettle.
9. The production system of claim 6, wherein: the gas inlet is arranged at the bottom of the third microchannel reactor.
10. The production system of claim 1, wherein: the discharge port of the first microchannel reactor is connected with the feed port of the second microchannel reactor, the discharge port of the second microchannel reactor is connected with the feed port of the third microchannel reactor, and the feed port of the third microchannel reactor is positioned at the top of the third microchannel reactor.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202221516037.6U CN217450115U (en) | 2022-06-17 | 2022-06-17 | Production system of 8-chloro-6-oxo-ethyl octanoate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN202221516037.6U CN217450115U (en) | 2022-06-17 | 2022-06-17 | Production system of 8-chloro-6-oxo-ethyl octanoate |
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| CN217450115U true CN217450115U (en) | 2022-09-20 |
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| CN202221516037.6U Active CN217450115U (en) | 2022-06-17 | 2022-06-17 | Production system of 8-chloro-6-oxo-ethyl octanoate |
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- 2022-06-17 CN CN202221516037.6U patent/CN217450115U/en active Active
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