CN208667550U - A kind of continuous esterification, the rectifier unit of monoxone formicester - Google Patents

A kind of continuous esterification, the rectifier unit of monoxone formicester Download PDF

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Publication number
CN208667550U
CN208667550U CN201821319911.0U CN201821319911U CN208667550U CN 208667550 U CN208667550 U CN 208667550U CN 201821319911 U CN201821319911 U CN 201821319911U CN 208667550 U CN208667550 U CN 208667550U
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esterification
connect
condenser
monoxone
formicester
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CN201821319911.0U
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张荣楠
张亦林
李贺存
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Tai'an Hanwei Group Co Ltd
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Tai'an Hanwei Group Co Ltd
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Abstract

The utility model discloses continuous esterification, the rectifier units of a kind of monoxone formicester, including sequentially connected raw material to prepare kettle, reaction kettle of the esterification, first rectifying column, the first condenser, ester separator, water phase receiving tank, methyl esters receiving tank, Second distillation column, methyl dichloroacetate finished pot, methyl chloroacetate finished pot and the second condenser;The raw material is prepared kettle and is connect by the first delivery pump with reaction kettle of the esterification;The reaction kettle of the esterification is connect with its feed inlet of first rectifying column;Its top of the first rectifying column is connect with the first condenser, and it forms closed loop with reaction kettle of the esterification by the first condenser and connect;Its bottom of the first rectifying column is connect with ester separator;Continuous esterification, the rectifier unit of the monoxone formicester of the utility model can efficiently separate methanol, methyl chloroacetate and water, and yield and purity are higher, and can reduce energy consumption, and then realize the production of methyl chloroacetate continuous esterification, rectifying.

Description

A kind of continuous esterification, the rectifier unit of monoxone formicester
Technical field
The utility model relates to continuous esterification, the rectifier units of a kind of monoxone formicester, belong to chemical equipment technical field.
Background technique
Methyl chloroacetate is important organic synthesis raw material, is the important intermediate of synthetic pesticide, medicine, in Chemical Manufacture In can be used as the raw materials of the products such as organic solvent or adhesive, surfactant;Methyl chloroacetate is most simple and easy at present Synthetic method be monoxone and methanol esterification method, methanol and chloroacetic mixed liquor are continuously added in reaction kettle of the esterification, steamed Ester output, water, methanol mixture, obtain methyl chloroacetate through ester separator, but there are three problems for this method: 1) methanol There are situation be lauched with methyl chloroacetate be layered it is unobvious;2) contain methanol and methyl chloroacetate in water phase, processing is very tired It is difficult;3) utilization rate of methanol is lower;Therefore, in order to solve problem above, it would be highly desirable to design the continuous of the new monoxone formicester of one kind Esterification, rectifier unit.
Utility model content
In order to solve the above problems, the utility model proposes a kind of continuous esterification, the rectifier unit of monoxone formicester, can Methanol, methyl chloroacetate and water are efficiently separated, yield and purity are higher, and can reduce energy consumption, and then realize that methyl chloroacetate connects Continue the production of esterification, rectifying.
Continuous esterification, the rectifier unit of the monoxone formicester of the utility model, including sequentially connected raw material prepare kettle, ester Change reaction kettle, first rectifying column, the first condenser, ester separator, water phase receiving tank, methyl esters receiving tank, Second distillation column, two Methyl chloroacetate finished pot, methyl chloroacetate finished pot and the second condenser;The raw material prepare kettle by the first delivery pump with Reaction kettle of the esterification connection;The reaction kettle of the esterification is connect with its feed inlet of first rectifying column;The first rectifying column its top with The connection of first condenser, and it forms closed loop with reaction kettle of the esterification by the first condenser and connect;Its bottom of the first rectifying column Portion is connect with ester separator;Its separation delivery outlet of the ester separator connects with water phase receiving tank and methyl esters receiving tank respectively It connects;By the second delivery pump, its feed inlet is connect the methyl esters receiving tank with Second distillation column;Its bottom of the Second distillation column It is connect by third delivery pump with methyl dichloroacetate finished pot;Its top of the Second distillation column is connected to through the second condenser Methyl chloroacetate finished pot.
Further, the first rectifying column and Second distillation column are enamel packed tower, and its top is mounted on Temperature measuring equipment.
Further, the ester separator is the ester separator for coming with condenser.
Further, its tower top temperature of the first rectifying column is 64 ~ 66 DEG C;The esterification temperature in the kettle be 95 ~ 100 DEG C, monoxone and methanol are carried out being mixed to form mixed liquor according to the molar ratio of 1:1;Mixed liquor is dropped evenly into ester Change in reaction kettle, the reaction temperature for controlling reaction kettle of the esterification is 95 ~ 100 DEG C, adjusts condensation methanol eddy ratio, controls the first rectifying Column overhead temperatures are 64 ~ 66 DEG C.
Further, its tower top temperature of the Second distillation column is 80 ~ 85 DEG C, and interior vacuum degree is -0.09Mpa.
Compared with prior art, continuous esterification, the rectifier unit of the monoxone formicester of the utility model, Methanol, water, methyl chloroacetate steam by first rectifying column separate, water and methyl chloroacetate (high boiling component) are cooled to band Then the ester separator of condenser is separated, methanol (low boiling component) is cooled back to esterification by the first condenser completely Reaction kettle greatly improves use ratio of methanol;The methyl esters isolated directly enters Second distillation column by side port and carries out continuous fine It evaporates, obtains methyl dichloroacetate and methyl chloroacetate finished product.
Detailed description of the invention
Fig. 1 is the production equipment schematic diagram of the utility model.
Each component mark in attached drawing are as follows: 1- raw material prepares kettle, 2- reaction kettle of the esterification, the first condenser of 3-, the first rectifying of 4- Tower, 5- ester separator, 6- methyl esters receiving tank, 7- water phase receiving tank, 8- Second distillation column, the second condenser of 9-, bis- chloroethene of 10- Sour methyl esters finished pot, 11- methyl chloroacetate finished pot, the first delivery pump of 12-, the second delivery pump of 13-, 14- third delivery pump.
Specific embodiment
Continuous esterification, the rectifier unit of monoxone formicester as shown in Figure 1, including sequentially connected raw material prepare kettle 1, ester Change reaction kettle 2, first rectifying column 4, the first condenser 3, ester separator 5, water phase receiving tank 7, the 6, second essence of methyl esters receiving tank Evaporate tower 8, methyl dichloroacetate finished pot 10, methyl chloroacetate finished pot 11 and the second condenser 9;It is logical that the raw material prepares kettle 1 The first delivery pump 12 is crossed to connect with reaction kettle of the esterification 2;Its feed inlet is connect the reaction kettle of the esterification 2 with first rectifying column 4;It is described Its top of first rectifying column 4 is connect with the first condenser 3, and it forms closed loop with reaction kettle of the esterification 2 by the first condenser 3 and connects It connects;Described its bottom of first rectifying column 4 is connect with ester separator 5;The ester separator 5 its separate delivery outlet respectively with water The closed cans that connects 7 and methyl esters receiving tank 6 connect;The methyl esters receiving tank 6 passes through its charging of the second delivery pump 13 and Second distillation column 8 Mouth connection;Described its bottom of Second distillation column 8 is connect by third delivery pump 14 with methyl dichloroacetate finished pot 10;Described Its top of two rectifying columns 8 is connected to methyl chloroacetate finished pot 11 through the second condenser 9.
The first rectifying column 4 and Second distillation column 8 are enamel packed tower, and its top is mounted on thermometric dress It sets.
The ester separator 5 is the ester separator for coming with condenser.
Described its tower top temperature of first rectifying column 4 is 64 ~ 66 DEG C;Temperature is 95 ~ 100 DEG C in the reaction kettle of the esterification 2.
Described its tower top temperature of Second distillation column 8 is 80 ~ 85 DEG C, and interior vacuum degree is -0.09Mpa.
Continuous esterification, the rectifier unit of the monoxone formicester of the utility model, methanol, water, methyl chloroacetate steam warp First rectifying column separation is crossed, water and methyl chloroacetate (high boiling component) are cooled to the ester separator with condenser and then carry out Separation, methanol (low boiling component) are cooled back to reaction kettle of the esterification by the first condenser completely, greatly improve methanol benefit With rate;And without the interference of methanol, methyl chloroacetate is enough preferably separated with water energy;The methyl esters isolated is directly by side port Into Second distillation column carry out continuous rectification, control Second distillation column tower top temperature be 80 ~ 85 DEG C, vacuum degree control be- 0.09Mpa obtains methyl dichloroacetate and methyl chloroacetate finished product.
Above-described embodiment is only the better embodiment of the utility model, therefore all according to the utility model patent application range The equivalent change or modification that the structure, feature and principle is done, is included in the scope of the utility model patent application.

Claims (5)

1. a kind of continuous esterification, the rectifier unit of monoxone formicester, it is characterised in that: including sequentially connected raw material prepare kettle, Reaction kettle of the esterification, first rectifying column, the first condenser, ester separator, water phase receiving tank, methyl esters receiving tank, Second distillation column, Methyl dichloroacetate finished pot, methyl chloroacetate finished pot and the second condenser;The raw material prepares kettle and passes through the first delivery pump It is connect with reaction kettle of the esterification;The reaction kettle of the esterification is connect with its feed inlet of first rectifying column;Its top of the first rectifying column It is connect with the first condenser, and it forms closed loop with reaction kettle of the esterification by the first condenser and connect;The first rectifying column its Bottom is connect with ester separator;Its separation delivery outlet of the ester separator connects with water phase receiving tank and methyl esters receiving tank respectively It connects;By the second delivery pump, its feed inlet is connect the methyl esters receiving tank with Second distillation column;Its bottom of the Second distillation column It is connect by third delivery pump with methyl dichloroacetate finished pot;Its top of the Second distillation column is connected to through the second condenser Methyl chloroacetate finished pot.
2. continuous esterification, the rectifier unit of monoxone formicester according to claim 1, it is characterised in that: first essence It evaporates tower and Second distillation column is enamel packed tower, and its top is mounted on temperature measuring equipment.
3. continuous esterification, the rectifier unit of monoxone formicester according to claim 1, it is characterised in that: the ester moisture It is the ester separator for coming with condenser from device.
4. continuous esterification, the rectifier unit of monoxone formicester according to claim 1, it is characterised in that: first essence Evaporating its tower top temperature of tower is 64 ~ 66 DEG C;The esterification temperature in the kettle is 95 ~ 100 DEG C.
5. continuous esterification, the rectifier unit of monoxone formicester according to claim 1, it is characterised in that: second essence Evaporating its tower top temperature of tower is 80 ~ 85 DEG C, and interior vacuum degree is -0.09Mpa.
CN201821319911.0U 2018-08-16 2018-08-16 A kind of continuous esterification, the rectifier unit of monoxone formicester Active CN208667550U (en)

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CN201821319911.0U CN208667550U (en) 2018-08-16 2018-08-16 A kind of continuous esterification, the rectifier unit of monoxone formicester

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113004143A (en) * 2021-02-24 2021-06-22 宁夏森萱药业有限公司 Method and device for synthesizing ethyl chloroacetate
CN114681944A (en) * 2022-01-20 2022-07-01 济宁福顺化工有限公司 Forced condensation system and method for reducing chloroacetic acid consumption in methyl chloroacetate production

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113004143A (en) * 2021-02-24 2021-06-22 宁夏森萱药业有限公司 Method and device for synthesizing ethyl chloroacetate
CN114681944A (en) * 2022-01-20 2022-07-01 济宁福顺化工有限公司 Forced condensation system and method for reducing chloroacetic acid consumption in methyl chloroacetate production
CN114681944B (en) * 2022-01-20 2023-05-23 济宁福顺化工有限公司 Forced condensing system and method for reducing consumption of chloroacetic acid in production of methyl chloroacetate

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