CN110252212A - A kind of continuous esterification process units of mixed dibasic acid dimethyl ester - Google Patents

A kind of continuous esterification process units of mixed dibasic acid dimethyl ester Download PDF

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Publication number
CN110252212A
CN110252212A CN201910688243.1A CN201910688243A CN110252212A CN 110252212 A CN110252212 A CN 110252212A CN 201910688243 A CN201910688243 A CN 201910688243A CN 110252212 A CN110252212 A CN 110252212A
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CN
China
Prior art keywords
esterification
reaction kettle
continuous
low level
dibasic acid
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Pending
Application number
CN201910688243.1A
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Chinese (zh)
Inventor
赵铎
史红军
巩国顺
陈聚良
王亚新
屈建海
陈亚春
朱子强
曲超
孙浩杰
冯继伟
王社志
薛继平
张军明
李云鹏
马帅
张东
潘勇
刘荣鸽
魏森英
吴世杰
司松凡
张朝领
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Henan Long St Chemical Co Ltd
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Henan Long St Chemical Co Ltd
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Application filed by Henan Long St Chemical Co Ltd filed Critical Henan Long St Chemical Co Ltd
Priority to CN201910688243.1A priority Critical patent/CN110252212A/en
Publication of CN110252212A publication Critical patent/CN110252212A/en
Pending legal-status Critical Current

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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/0046Sequential or parallel reactions, e.g. for the synthesis of polypeptides or polynucleotides; Apparatus and devices for combinatorial chemistry or for making molecular arrays
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/18Stationary reactors having moving elements inside
    • B01J19/1862Stationary reactors having moving elements inside placed in series
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J8/00Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
    • B01J8/008Details of the reactor or of the particulate material; Processes to increase or to retard the rate of reaction
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J8/00Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
    • B01J8/08Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with moving particles
    • B01J8/10Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with moving particles moved by stirrers or by rotary drums or rotary receptacles or endless belts
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C67/00Preparation of carboxylic acid esters
    • C07C67/08Preparation of carboxylic acid esters by reacting carboxylic acids or symmetrical anhydrides with the hydroxy or O-metal group of organic compounds

Abstract

The invention discloses a kind of continuous esterification process units of mixed dibasic acid dimethyl ester, including reaction kettle of the esterification, the gaseous feed pipeline that reaction kettle of the esterification is continuously passed through with high-order continuous feed pipeline, low level continuous discharge pipeline and low level respectively is connected, and overflow baffle is provided in reaction kettle of the esterification;Reaction kettle of the esterification upper lateral part is provided with tower section, is internally provided with blast cap in tower section, blast cap bottom is provided with hydrops slot, the liquid material condensed out is individually recycled by the hydrops slot of blast cap bottom;The reaction kettle of the esterification be it is multiple, multiple reaction kettle of the esterification are sequentially connected in series together by high-order continuous feed pipeline of the low level continuous discharge pipeline of previous reaction kettle of the esterification as the latter reaction kettle of the esterification.The present invention produces mixed dibasic acid dimethyl ester using continuous esterification, and installation cost is low, good product quality, high production efficiency, DBE product purity >=99.0% of acquisition, has good market prospects.

Description

A kind of continuous esterification process units of mixed dibasic acid dimethyl ester
Technical field
The present invention relates to a kind of high-quality high boiling solvent process units, more particularly to a kind of mixed dibasic acid dimethyl ester Continuous esterification process units.
Background technique
Higher boiling mixing dicarboxylic acids dimethyl ester is also known as DBE, by dimethyl succinate, dimethyl glutarate, adipic acid two Three kinds of component compositions of methyl esters are higher boiling, low cost, low volatility and the fragranced with excellent dissolubility, ester, environmental protection Nontoxic, use is safe, can replace that toxicity is big, the isophorone of tanginess, ethylene glycol ether acetate (CAC), ethylene glycol Monobutyl ether (anti-plain boiled water), Propylene Glycol Ether Ester Series Solvent, cyclohexanone, diacetone alcohol, cresols equal solvent.These good characteristics determine DBE can be used widely in fields such as coil steel coating, Baking Paint, coatings for tin plate printing, car paint, woodcare paint, ink industries, because This is analyzed from properties of product, has good market prospects.
Mixed dibasic acid DBA is also known as nylon acid, is the byproduct in adipic acid production process, and main organic principle is for oneself Diacid (ADA), glutaric acid (GA) and succinic acid (SA), therefore also have the title of AGS acid.Mainly for the production of solvent, plasticizer, go back It can be used for manufacturing the raw material of pesticide, auxin, synthetic rubber, foam plastic, production high boiling solvent is the main of it Purposes.With rising rapidly for domestic adipic acid production capacity, the binary acid purposes exploitation of by-product is being constantly updated in adipic acid production. As the solvent industry of binary acid main application, the production technology research of DBE is also constantly improving.
Summary of the invention
The technical problems to be solved by the present invention are: providing a kind of continuous esterification production dress of mixed dibasic acid dimethyl ester It sets, the installation cost is low, good product quality, DBE product purity >=99.0% of acquisition.
The technical solution that the present invention is taken in order to solve the technical problem is as follows:
A kind of continuous esterification process units of mixed dibasic acid dimethyl ester, including reaction kettle of the esterification, the reaction kettle of the esterification difference The gaseous feed pipeline being continuously passed through with high-order continuous feed pipeline, low level continuous discharge pipeline and low level is connected, and is being esterified Overflow baffle is provided in reaction kettle, the height at low level continuous discharge piping inlet end is higher than the bottom of overflow baffle, and a high position is even The discharge end height of continuous feeding line is lower than the top of overflow baffle;Reaction kettle of the esterification upper lateral part is provided with tower section, in tower section It is internally provided with blast cap, blast cap bottom is provided with hydrops slot, the liquid material condensed out passes through the hydrops slot of blast cap bottom Individually recycling;The reaction kettle of the esterification be it is multiple, the low level continuous discharge pipeline of previous reaction kettle of the esterification is as the latter ester The high-order continuous feed pipeline for changing reaction kettle, multiple reaction kettle of the esterification are sequentially connected in series together.
Tower section top is provided with thermometer and pressure gauge, discharging pipeline observation is installed on low level continuous discharge pipeline Visor.
Liquidometer and thermometer, thermometer and steam control valve interlocking, steam control valve are provided on reaction kettle of the esterification It is arranged on steam conveying pipe.
The dredging valve that the reaction kettle of the esterification bottom is connected with bottom discharge pipe and prevents bottom from blocking, it is anti-in esterification It answers and agitating device is installed inside kettle.
The height of the overflow baffle is the 30~95% of the reaction kettle of the esterification height.
The present invention produces mixed dibasic acid dimethyl ester using continuous esterification, and the course of work is as follows:
1, DBA material is continued into series connection reaction kettle of the esterification by high-order continuous feed pipeline, while catalyst is added, and point It is not continually fed into methanol stirring, carries out reaction;
2, overflow baffle is installed before low level continuous discharge pipeline, guarantees that material in reactor sufficiently stops the reaction time, Discharging pipeline observation visor is installed on low level continuous discharge pipeline;
3, at 60~200 DEG C, tower top temperature is controlled at 60~100 DEG C the control of esterification temperature in the kettle;
4, funnel-cap type structure, the liquid condensed out the water and carbinol mixture generated during esterification: are used inside tower section State product is individually recycled by blast cap bottom hydrops slot, and water and carbinol mixture enter in methanol distillation column reuse methanol again;
5, agitating device is installed inside reaction kettle, liquidometer and thermometer are installed, thermometer and steam control valve interlock Control reaction temperature;
6, the dredging valve that bottom goes out pipeline and prevents bottom from blocking is connected in reaction kettle of the esterification bottom.
The present invention produces mixed dibasic acid dimethyl ester using continuous esterification, and installation cost is low, good product quality, raw High-efficient, DBE product purity >=99.0% of acquisition is produced, there are good market prospects.
Detailed description of the invention:
Fig. 1 is the structural diagram of the present invention.
Specific embodiment:
The present invention will be further explained with reference to the accompanying drawing:
Referring to Fig. 1, a kind of continuous esterification process units of mixed dibasic acid dimethyl ester, including reaction kettle of the esterification 1, reaction kettle of the esterification The 1 gaseous feed pipeline 4 being continuously passed through with high-order continuous feed pipeline 2, low level continuous discharge pipeline 3 and low level respectively is connected It connects, overflow baffle 6 is provided in reaction kettle of the esterification 1, the height of 3 input end of low level continuous discharge pipeline is higher than overflow baffle 6 Bottom, the discharge end height of high-order continuous feed pipeline 2 is lower than the top of overflow baffle 6;It is set in 1 upper lateral part of reaction kettle of the esterification It is equipped with tower section 7, is internally provided with blast cap 8 in tower section 7, blast cap bottom is provided with hydrops slot 18, the liquid material condensed out It is individually recycled by the hydrops slot of blast cap bottom;Reaction kettle of the esterification 1 is multiple, the low level continuous discharge of previous reaction kettle of the esterification High-order continuous feed pipeline of the pipeline as the latter reaction kettle of the esterification, multiple reaction kettle of the esterification are sequentially connected in series together.
7 top of tower section is provided with thermometer 9 and pressure gauge 10, discharge nozzle is installed on low level continuous discharge pipeline 3 Line observes visor 5.
Liquidometer 14 and thermometer 15 are provided on reaction kettle of the esterification 1, thermometer 15 and steam control valve 16 are interlocked, steamed Vapour control valve 16 is arranged on steam conveying pipe 17.
In the dredging valve 12 that 1 bottom of reaction kettle of the esterification is connected with bottom discharge pipe 11 and prevents bottom from blocking, in ester Change and agitating device 13 is installed inside reaction kettle 1.
Wherein: the height of overflow baffle 6 is the 30~95% of 1 height of reaction kettle of the esterification.
The present invention produces mixed dibasic acid dimethyl ester using continuous esterification, and installation cost is low, good product quality, raw High-efficient, DBE product purity >=99.0% of acquisition is produced, there are good market prospects.

Claims (5)

1. a kind of continuous esterification process units of mixed dibasic acid dimethyl ester, including reaction kettle of the esterification (1), it is characterised in that: institute State what reaction kettle of the esterification (1) was continuously passed through with high-order continuous feed pipeline (2), low level continuous discharge pipeline (3) and low level respectively Gaseous feed pipeline (4) is connected, and is provided with overflow baffle (6) in reaction kettle of the esterification (1), low level continuous discharge pipeline (3) The height of input end is higher than the bottom of overflow baffle (6), and the discharge end height of high-order continuous feed pipeline (2) is lower than overflow baffle (6) top;In reaction kettle of the esterification (1), upper lateral part is provided with tower section (7), blast cap (8) is internally provided in tower section (7), in wind Cap bottom is provided with hydrops slot (18), and the liquid material condensed out is individually recycled by the hydrops slot of blast cap bottom;The ester Changing reaction kettle (1) is multiple, height of the low level continuous discharge pipeline of previous reaction kettle of the esterification as the latter reaction kettle of the esterification Position continuous feed pipeline, multiple reaction kettle of the esterification are sequentially connected in series together.
2. the continuous esterification process units of mixed dibasic acid dimethyl ester according to claim 1, it is characterised in that: in tower section (7) top is provided with thermometer (9) and pressure gauge (10), and discharging pipeline observation is equipped on low level continuous discharge pipeline (3) Visor (5).
3. the continuous esterification process units of mixed dibasic acid dimethyl ester according to claim 1, it is characterised in that: be esterified Liquidometer (14) and thermometer (15), thermometer (15) and steam control valve (16) interlocking, steam control are provided on reaction kettle (1) Valve (16) processed is arranged on steam conveying pipe (17).
4. the continuous esterification process units of mixed dibasic acid dimethyl ester according to claim 1, it is characterised in that: the ester Change the dredging valve (12) that reaction kettle (1) bottom is connected with bottom discharge pipe (11) and prevents bottom from blocking, in esterification Agitating device (13) are installed inside kettle (1).
5. the continuous esterification process units of mixed dibasic acid dimethyl ester according to claim 1, it is characterised in that: described to overflow The height for flowing baffle (6) is the 30~95% of the reaction kettle of the esterification (1) height.
CN201910688243.1A 2019-07-29 2019-07-29 A kind of continuous esterification process units of mixed dibasic acid dimethyl ester Pending CN110252212A (en)

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CN201910688243.1A CN110252212A (en) 2019-07-29 2019-07-29 A kind of continuous esterification process units of mixed dibasic acid dimethyl ester

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CN201910688243.1A CN110252212A (en) 2019-07-29 2019-07-29 A kind of continuous esterification process units of mixed dibasic acid dimethyl ester

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114307920A (en) * 2021-07-30 2022-04-12 江苏雷蒙新材料有限公司 Continuous production system and production process of polyol acetate

Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH04230242A (en) * 1990-12-27 1992-08-19 Asahi Chem Ind Co Ltd Continuous production of diaryl carbonate
CN201815308U (en) * 2010-09-17 2011-05-04 昌乐屹立化工有限公司 Mixed dibasic acid dimethyl ester continuous esterification reaction unit
CN104128133A (en) * 2014-07-10 2014-11-05 中国化学赛鼎宁波工程有限公司 Swept-back high-efficiency hot-plate diversion rectification multiphase reaction kettle
CN205164701U (en) * 2015-12-01 2016-04-20 湖北汉贝化工有限公司 A reation kettle for producing silane have a separator
CN205710538U (en) * 2016-04-21 2016-11-23 浙江亿诚聚氨酯制造有限公司 A kind of three still continuous polyester synthesis devices
CN109507963A (en) * 2018-11-16 2019-03-22 浙江工业大学 A kind of tetrahydrofuran -3- Formaldehyde Production control system and method based on DCS control
CN210700016U (en) * 2019-07-29 2020-06-09 河南久圣化工有限公司 Continuous esterification production device for mixed dibasic acid dimethyl ester

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH04230242A (en) * 1990-12-27 1992-08-19 Asahi Chem Ind Co Ltd Continuous production of diaryl carbonate
CN201815308U (en) * 2010-09-17 2011-05-04 昌乐屹立化工有限公司 Mixed dibasic acid dimethyl ester continuous esterification reaction unit
CN104128133A (en) * 2014-07-10 2014-11-05 中国化学赛鼎宁波工程有限公司 Swept-back high-efficiency hot-plate diversion rectification multiphase reaction kettle
CN205164701U (en) * 2015-12-01 2016-04-20 湖北汉贝化工有限公司 A reation kettle for producing silane have a separator
CN205710538U (en) * 2016-04-21 2016-11-23 浙江亿诚聚氨酯制造有限公司 A kind of three still continuous polyester synthesis devices
CN109507963A (en) * 2018-11-16 2019-03-22 浙江工业大学 A kind of tetrahydrofuran -3- Formaldehyde Production control system and method based on DCS control
CN210700016U (en) * 2019-07-29 2020-06-09 河南久圣化工有限公司 Continuous esterification production device for mixed dibasic acid dimethyl ester

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114307920A (en) * 2021-07-30 2022-04-12 江苏雷蒙新材料有限公司 Continuous production system and production process of polyol acetate

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