CN212833557U - Continuous esterification device - Google Patents

Continuous esterification device Download PDF

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Publication number
CN212833557U
CN212833557U CN202021433088.3U CN202021433088U CN212833557U CN 212833557 U CN212833557 U CN 212833557U CN 202021433088 U CN202021433088 U CN 202021433088U CN 212833557 U CN212833557 U CN 212833557U
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pipeline
communicated
permeable membrane
dehydrator
reaction
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张影
宋香哲
张国栋
王立新
温明军
李娟�
李成果
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Hebei Chengxin Jiutian Pharmaceutical Chemical Co ltd
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Hebei Chengxin Jiutian Pharmaceutical Chemical Co ltd
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Abstract

The utility model provides a continuous esterification device, belonging to the technical field of esterification production, comprising a mixing tank, a heater, a catalytic reaction tower and a permeable membrane dehydrator; adding the materials in the mixing tank into a heater through a power pump; the catalytic reaction tower is provided with a plurality of reaction layers; resin catalysts are arranged in each reaction layer; the reaction layer is provided with an inlet and an outlet, and the inlet of the reaction layer at the lowest layer is communicated with the heater; the number of the permeable membrane dehydrator is multiple, and the permeable membrane dehydrator corresponds to each reaction layer one by one; the permeable membrane dehydrator is provided with a second feeding hole and a second discharging hole; the second feed inlet is communicated with the outlet of the corresponding catalytic reaction tower, and the discharge outlet is communicated with the inlet of the catalytic reaction tower which is adjacent and positioned above. The utility model provides a device esterifies in succession, the esterification reaction and the osmotic membrane dehydrator dewatering operation on a plurality of reaction layers that go on in succession have accomplished continuous production of esterifying, and esterification reaction and dewatering operation go on side by side, have improved production efficiency.

Description

Continuous esterification device
Technical Field
The utility model belongs to the technical field of the production of esterifying, more specifically say, relate to a device esterifies in succession.
Background
Cyanoacetic acid ester is an important organic synthesis intermediate for organic synthesis, medicines, pesticides and dyes, and the esterification reaction of cyanoacetic acid and alcohol is carried out under the catalytic action of concentrated sulfuric acid in the traditional production process. In the esterification process, the generated water needs to be continuously distilled out to ensure that the esterification reaction is completely carried out. In the process of water distillation, a large amount of low-boiling-point alcohol is inevitably distilled out, and then the alcohol is recovered by adopting a rectification mode, so that the steps of esterification reaction are increased, the continuity is poor, and the efficiency is low.
SUMMERY OF THE UTILITY MODEL
An object of the utility model is to provide a device esterifies in succession to the continuity of the esterification reaction who exists among the solution prior art is relatively poor, and the lower technical problem of efficiency.
In order to achieve the above object, the utility model adopts the following technical scheme: provided is a continuous esterification apparatus comprising:
the mixing tank is provided with a first feeding hole and a first discharging hole;
the heater is communicated with the mixing tank; the materials in the mixing tank are added into a heater through a power pump;
the catalytic reaction tower is provided with a plurality of reaction layers arranged from bottom to top; resin catalysts are arranged in each reaction layer; the reaction layer is provided with an inlet and an outlet, and the inlet of the reaction layer at the lowest layer is communicated with the heater;
the number of the permeable membrane dehydrator is multiple, and the permeable membrane dehydrator corresponds to each reaction layer one by one; the permeable membrane dehydrator is provided with a second feeding hole and a second discharging hole; the second feed inlet is communicated with the corresponding outlet of the catalytic reaction tower, and the discharge outlet is communicated with the inlet of the catalytic reaction tower which is adjacent and positioned above the discharge outlet.
As another embodiment of the present application, a first pipeline and a second pipeline which are respectively communicated with the second feed port and the second discharge port are arranged on the permeable membrane dehydrator; a third pipeline is arranged between the first pipeline and the second pipeline; be equipped with first valve on the first pipeline, be equipped with the second valve on the second pipeline, just the second valve is located the third pipeline with between the discharge gate, be equipped with the third valve on the third pipeline.
As another embodiment of the present application, a fourth pipeline is disposed on the heater, a fifth pipeline is disposed at an inlet of the catalytic reaction tower, the fourth pipeline and the fifth pipeline are connected by a tee joint, and a sixth pipeline for adding resin to the catalytic reaction tower is further disposed on the tee joint; and a fourth valve is arranged on the fourth pipeline, and a fifth valve is arranged on the sixth pipeline.
As another embodiment of the present application, the continuous esterification apparatus further comprises:
and the negative pressure water collecting device is communicated with each osmotic membrane dehydrator and is used for collecting the water in the osmotic membrane dehydrator.
As another embodiment of this application, the osmotic membrane dehydrator is provided with a water outlet, and the negative pressure water collecting device includes:
the connecting pipe is positioned on one side of the plurality of permeable membrane dehydrator and is communicated with the plurality of water outlets;
the upper end of the condenser is communicated with the connecting pipe and is used for liquefying water vapor;
the water collecting tank is communicated with the lower end of the condenser and is used for storing water;
and the negative pressure machine is connected with the water collecting tank and is used for forming negative pressure in the water collecting tank.
As another embodiment of the application, the second discharge hole of the permeable membrane dehydrator positioned at the uppermost position is connected with a storage tank.
As another embodiment of the application, a stirring device is further arranged on the mixing tank.
As another embodiment of the present application, the catalytic reaction tower is made of enamel.
The utility model provides a device esterifies in succession has the beneficial effect that: compared with the prior art, the utility model discloses continuous esterification device, add cyanoacetic acid and mellow wine in proportion from first feed inlet to the mixing tank in forming mixed liquid during the use, and heat in going into the heater by the power pump, then in the reaction layer of lower extreme in the import entering catalytic reaction tower, carry out esterification reaction with the help of resin catalyst and generate water and cyanoacetate, then get into to the penetrating film dehydrator dewatering that corresponds through export and second feed inlet again, remaining cyanoacetate wears out the second discharge gate and carries out esterification reaction again in the reaction layer of top and get into the penetrating film dehydrator dewatering that corresponds, esterification reaction and the penetrating film dehydrator dewatering operation through a plurality of reaction layers that go on in succession, continuous esterification production has been accomplished, and esterification reaction and dewatering operation are gone on side by side, and the production efficiency is improved.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings required for the embodiments or the prior art descriptions will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings without creative efforts.
Fig. 1 is a schematic structural diagram of a continuous esterification apparatus provided in an embodiment of the present invention;
fig. 2 is an enlarged view of a point a in fig. 1.
Wherein, in the figures, the respective reference numerals:
1. a mixing tank; 11. a first feed port; 12. a first discharge port; 13. a stirring device; 2. a heater; 21. a power pump; 22. a fourth conduit; 221. a fourth valve; 23. a sixth pipeline; 231. a fifth valve; 3. a catalytic reaction tower; 31. a reaction layer; 311. an inlet; 312. an outlet; 32. a fifth pipeline; 4. A permeable membrane dehydrator; 41. a second feed port; 42. a second discharge port; 43. a first conduit; 431. a first valve; 44. a second conduit; 441. a second valve; 45. a third pipeline; 451. a third valve; 46. A water outlet; 5. a negative pressure water collecting device; 51. a connecting pipe; 52. a condenser; 53. a water collection tank; 54. a negative pressure machine.
Detailed Description
In order to make the technical problem, technical solution and advantageous effects to be solved by the present invention more clearly understood, the following description is given in conjunction with the accompanying drawings and embodiments to illustrate the present invention in further detail. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Referring to fig. 1 and fig. 2, the continuous esterification apparatus provided by the present invention will now be described. A continuous esterification device comprises a mixing tank 1, a heater 2, a catalytic reaction tower 3 and a permeable membrane dehydrator 4, wherein the mixing tank 1 is provided with a first feeding hole 11 and a first discharging hole 12; the heater 2 is communicated with the mixing tank 1; the materials in the mixing tank 1 are added into the heater 2 through the power pump 21; the catalytic reaction tower 3 is provided with a plurality of reaction layers 31 arranged from bottom to top; resin catalysts are arranged in each reaction layer 31; the reaction layer 31 is provided with an inlet 311 and an outlet 312, and the inlet 311 of the reaction layer 31 at the lowest layer is communicated with the heater 2; the number of the permeable membrane dehydrator 4 is multiple, and the permeable membrane dehydrator corresponds to each reaction layer 31 one by one; the permeable membrane dehydrator 4 is provided with a second feeding hole 41 and a second discharging hole 42; the second feed port 41 is communicated with the outlet 312 of the corresponding catalytic reaction tower 3, and the discharge port is communicated with the inlet 311 of the adjacent and upper catalytic reaction tower 3.
The utility model provides a continuous esterification device, compared with the prior art, during the use with cyanoacetic acid and mellow wine according to the proportion from first feed inlet 11 add to form the mixed liquid in compounding jar 1, and pump the mixed liquid out first discharge gate 12 and heat in going into heater 2 by power pump 21, then in the reaction layer 31 of bottom in the import 311 gets into catalytic reaction tower 3, carry out esterification reaction with the help of resin catalyst and generate water and cyanoacetic acid ester, then get into through export 312 and second feed inlet 41 and remove water in the osmotic membrane dehydrator 4 that corresponds, remaining cyanoacetic acid ester wears out second discharge gate 42 and carries out esterification reaction again in getting into the reaction layer 31 of top and getting into the dehydration in the osmotic membrane dehydrator 4 that corresponds, esterification reaction and the dehydration operation of osmotic membrane dehydrator 4 through a plurality of reaction layers 31 that go on in succession, continuous esterification production has been accomplished, and the esterification reaction and the dewatering operation are carried out in parallel, so that the production efficiency is improved.
The first feed port 11 is provided in plural for feeding plural different reactants at the same time. The resin catalyst adopts strong acid ion exchange resin to replace concentrated sulfuric acid for catalysis, so that side reactions are less, corrosion of strong acid to equipment is avoided, and the burden of separation and purification of each subsequent reaction layer 31 is reduced; cyanoacetate and excessive alcohol generated by the esterification reaction and the water removal reaction are discharged into the storage tank from the second discharge port 42 of the permeable membrane dehydrator 4 at the uppermost end. The permeable membrane dehydrator 4 is adopted, so that the problems of large alcohol loss in the traditional evaporation dehydration and impurity residue in the entrainer water are avoided.
The reaction layer 31 is provided with four layers, and the number of the corresponding permeable membrane dehydrator 4 is also four. The molar ratio of cyanoacetic acid to alcohol is 1: 1.2-1: 1.5, and the heater 2 is heated to 60-90 ℃ to heat the mixed solution of cyanoacetic acid and alcohol.
Referring to fig. 1 and fig. 2, as a specific embodiment of the continuous esterification apparatus provided by the present invention, a first pipeline 43 and a second pipeline 44 are disposed on the permeable membrane dehydrator 4 and respectively communicated with the second feeding port 41 and the second discharging port 42; a third pipeline 45 is arranged between the first pipeline 43 and the second pipeline 44; a first valve 431 is arranged on the first pipeline 43, a second valve 441 is arranged on the second pipeline 44, and the second valve 441 is positioned between the third pipeline 45 and the discharge port, and the third pipeline 45 is provided with a third valve 451, when the continuous esterification system is used, the first valves 431 and the second valves 441 on the plurality of osmotic membrane dehydrators 4 are opened, the corresponding third valves 451 are closed, cyanoacetate and water generated after the esterification reaction enter the first pipeline 43 from the outlet 312 of the reaction layer 31, pass through the first valves 431 and the second feed inlets 41 and then enter the corresponding osmotic membrane dehydrators 4, and are dehydrated by the osmotic membrane dehydrators 4, and the cyanoacetate and the solution pass through a second discharge hole 42 on the permeable membrane dehydrator 4, pass through a second pipeline 44 and a second valve 441, enter the adjacent upper reaction layer 31 to continue the esterification reaction, and further perform the operations of esterification reaction and permeation dehydration step by step. When it is necessary to add the resin catalyst to each reaction layer 31, each of the first valve 431 and the second valve 441 is closed, the plurality of reaction layers 31 are communicated with each other through the third valve 451, and the resin catalyst is replenished to the catalytic reaction tower 3. Furthermore, the terms "first", "second", "third" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Thus, features defined as "first", "second", "third" may explicitly or implicitly include one or more of the features. In the description of the present invention, "a plurality" means two or more unless specifically limited otherwise.
Referring to fig. 1 and 2, as a specific embodiment of the continuous esterification apparatus provided by the present invention, a fourth pipeline 22 is disposed on the heater 2, a fifth pipeline 32 is disposed at an inlet 311 of the catalytic reaction tower 3, the fourth pipeline 22 and the fifth pipeline 32 are connected by a tee, and a sixth pipeline 23 for adding resin to the catalytic reaction tower 3 is further disposed on the tee; a fourth valve 221 is arranged on the fourth pipeline 22, and a fifth valve 231 is arranged on the sixth pipeline 23; the fourth pipeline 22, the fifth pipeline 32 and the sixth pipeline 23 are communicated through a tee joint, when the esterification reaction is performed, the fourth valve 221 on the fourth pipeline 22 is opened, the fifth valve 231 on the sixth pipeline 23 is closed, and the cyanoacetic acid and the alcohol heated by the heater 2 enter the first reaction layer 31 in the catalytic reaction tower 3 through the fourth pipeline 22, the fourth valve 221 and the fifth pipeline 32, so that the stability and the accuracy of the flow of the cyanoacetic acid and the alcohol are ensured. When resin catalyst needs to be added into each reaction layer 31 in the catalytic reaction tower 3, the fourth valve 221 and the first valves 431 and the second valves 441 are closed, the fifth valve 231 and the third valves 451 are opened, resin catalyst is added from one end of the sixth pipeline 23 far away from the tee joint, the resin catalyst enters the reaction layer 31 through the fifth valve 231, the fifth pipeline 32 and the inlet 311 of the first reaction layer 31, and the resin catalyst enters the adjacent upper reaction layer 31 along the first pipeline 43, the third pipeline 45 and the second pipeline 44 and avoids the permeable membrane dehydrator 4 due to the closing of the first valve 431 and the second valves 441, so that the resin catalyst can be directly and simply added into the catalytic reaction tower 3. The waste liquid and waste water generated during the addition of the resin catalyst is discharged from the outlet 312 of the uppermost reaction layer 31 without passing through the permeable membrane dehydrator 4, and the outlet 312 similarly discharges a solution after many times of esterification in the esterification reaction. Furthermore, the terms "fourth", "fifth", "sixth" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Thus, features defined as "fourth", "fifth", "sixth" may explicitly or implicitly include one or more of such features. In the description of the present invention, "a plurality" means two or more unless specifically limited otherwise.
Please refer to fig. 1 and fig. 2, as a specific embodiment of the continuous esterification apparatus provided by the present invention, the continuous esterification apparatus further includes a negative pressure water collecting device 5, the negative pressure water collecting device 5 is communicated with each osmotic membrane dehydrator 4 for collecting the water in the osmotic membrane dehydrator 4, cyanoacetate and water generated by the esterification reaction pass through the second feed port 41 to enter the osmotic membrane dehydrator 4, the negative pressure water collecting device 5 is started, a negative pressure is formed behind the membrane of the osmotic membrane dehydrator 4, the water generated by the esterification reaction is collected through the membrane by permeation, such a way not only can collect the water generated by the esterification reaction, but also can accelerate the water permeation by the pressure difference generated by the negative pressure. The pressure range generated by the negative pressure water collecting device 5 is-0.08-0.095 Mpa.
Referring to fig. 1 and fig. 2, as a specific embodiment of the continuous esterification apparatus provided by the present invention, a water outlet 46 is provided on the permeable membrane dehydrator 4, the negative pressure water collecting apparatus 5 includes a connecting pipe 51, a condenser 52, a water collecting tank 53 and a negative pressure device, the connecting pipe 51 is located at one side of the plurality of permeable membrane dehydrator 4 and is communicated with the plurality of water outlets 46; the upper end of the condenser 52 is communicated with the connecting pipe 51 and is used for liquefying water vapor; the water collection tank 53 is communicated with the lower end of the condenser 52 and used for storing water; the negative pressure machine 54 is connected with the water collecting tank 53 for forming negative pressure in the water collecting tank 53, and after the negative pressure machine 54 is started, the water collecting tank 53, the condenser 52, the connecting pipe 51 and the membrane rear side of the osmotic membrane dehydrator 4 form negative pressure, so that the water in the osmotic membrane dehydrator 4 is vaporized through the osmotic membrane, then passes through the connecting pipe 51 and enters the condenser 52, and the water is liquefied by the condenser 52 to form water flow which is stored in the water collecting tank 53. The connecting pipe 51 is vertically arranged, and the water outlets 46 of the plurality of osmotic membrane dehydrator 4 are all communicated with the connecting pipe 51.
Referring to fig. 1 and 2, as a specific embodiment of the continuous esterification apparatus of the present invention, the second discharge port 42 of the uppermost osmotic membrane dehydrator 4 is connected to a storage tank, and after the esterification reaction in the plurality of reaction layers 31 and the dehydration operation in the plurality of osmotic membrane dehydrators 4, cyanoacetate and excessive alcohol generated by the reaction flow out from the second discharge port 42 of the uppermost osmotic membrane dehydrator 4 and are stored in the storage tank.
Please refer to fig. 1 and fig. 2, as a specific embodiment of the continuous esterification apparatus provided by the present invention, the mixing tank 1 is further provided with a stirring device 13, the upper end surface of the mixing tank 1 is provided with a motor, an output shaft of the motor is connected with a stirring shaft extending into the mixing tank 1, after the cyanoacetic acid and the alcohol are added into the mixing tank 1, the motor is started to drive the stirring shaft to stir in the mixing tank 1, so as to accelerate the uniform mixing of the cyanoacetic acid and the alcohol.
Referring to fig. 1 and 2, as a specific embodiment of the continuous esterification apparatus provided by the present invention, the catalytic reaction tower 3 is made of enamel, the catalytic reaction tower 3 made of enamel can withstand high temperature and high pressure conditions, and the enamel is resistant to chemical corrosion, especially sulfuric acid and hydrochloric acid, so as to ensure that the whole esterification process is performed stably. The diameter of the catalytic reaction tower 3 is 800mm, and the resin packing height in each reaction layer 31 is 2 m.
The above description is only exemplary of the present invention and should not be construed as limiting the present invention, and any modifications, equivalents and improvements made within the spirit and principles of the present invention are intended to be included within the scope of the present invention.

Claims (8)

1. Continuous esterification device, its characterized in that includes:
the mixing tank is provided with a first feeding hole and a first discharging hole;
the heater is communicated with the mixing tank; the materials in the mixing tank are added into a heater through a power pump;
the catalytic reaction tower is provided with a plurality of reaction layers arranged from bottom to top; resin catalysts are arranged in each reaction layer; the reaction layer is provided with an inlet and an outlet, and the inlet of the reaction layer at the lowest layer is communicated with the heater;
the number of the permeable membrane dehydrator is multiple, and the permeable membrane dehydrator corresponds to each reaction layer one by one; the permeable membrane dehydrator is provided with a second feeding hole and a second discharging hole; the second feed inlet is communicated with the corresponding outlet of the catalytic reaction tower, and the discharge outlet is communicated with the inlet of the catalytic reaction tower which is adjacent and positioned above the discharge outlet.
2. The continuous esterification apparatus according to claim 1, wherein the permeable membrane dehydrator is provided with a first pipe and a second pipe respectively communicated with the second feed port and the second discharge port; a third pipeline is arranged between the first pipeline and the second pipeline; be equipped with first valve on the first pipeline, be equipped with the second valve on the second pipeline, just the second valve is located the third pipeline with between the discharge gate, be equipped with the third valve on the third pipeline.
3. The continuous esterification apparatus according to claim 2, wherein the heater is provided with a fourth pipeline, the inlet of the catalytic reaction tower is provided with a fifth pipeline, the fourth pipeline and the fifth pipeline are connected by a tee joint, and the tee joint is further provided with a sixth pipeline for adding resin into the catalytic reaction tower; and a fourth valve is arranged on the fourth pipeline, and a fifth valve is arranged on the sixth pipeline.
4. The continuous esterification apparatus of claim 1, further comprising:
and the negative pressure water collecting device is communicated with each osmotic membrane dehydrator and is used for collecting the water in the osmotic membrane dehydrator.
5. The continuous esterification apparatus as claimed in claim 4, wherein said permeable membrane dehydrator is provided with a water outlet, and said negative pressure water collecting device comprises:
the connecting pipe is positioned on one side of the plurality of permeable membrane dehydrator and is communicated with the plurality of water outlets;
the upper end of the condenser is communicated with the connecting pipe and is used for liquefying water vapor;
the water collecting tank is communicated with the lower end of the condenser and is used for storing water;
and the negative pressure machine is connected with the water collecting tank and is used for forming negative pressure in the water collecting tank.
6. The continuous esterification apparatus according to claim 1, wherein the second discharge port of the permeable membrane dehydrator positioned uppermost is connected to a storage tank.
7. The continuous esterification apparatus of claim 1, wherein the mixing tank is further provided with an agitation device.
8. The continuous esterification apparatus according to claim 1, wherein the catalytic reaction tower is made of enamel.
CN202021433088.3U 2020-07-20 2020-07-20 Continuous esterification device Active CN212833557U (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202021433088.3U CN212833557U (en) 2020-07-20 2020-07-20 Continuous esterification device

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202021433088.3U CN212833557U (en) 2020-07-20 2020-07-20 Continuous esterification device

Publications (1)

Publication Number Publication Date
CN212833557U true CN212833557U (en) 2021-03-30

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Application Number Title Priority Date Filing Date
CN202021433088.3U Active CN212833557U (en) 2020-07-20 2020-07-20 Continuous esterification device

Country Status (1)

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CN (1) CN212833557U (en)

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