CN108484400A - A kind of methyl formate production equipment - Google Patents
A kind of methyl formate production equipment Download PDFInfo
- Publication number
- CN108484400A CN108484400A CN201810280219.XA CN201810280219A CN108484400A CN 108484400 A CN108484400 A CN 108484400A CN 201810280219 A CN201810280219 A CN 201810280219A CN 108484400 A CN108484400 A CN 108484400A
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- China
- Prior art keywords
- outlet
- entrance
- reaction mass
- rectifying column
- heat exchanger
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Classifications
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/36—Preparation of carboxylic acid esters by reaction with carbon monoxide or formates
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/48—Separation; Purification; Stabilisation; Use of additives
- C07C67/52—Separation; Purification; Stabilisation; Use of additives by change in the physical state, e.g. crystallisation
- C07C67/54—Separation; Purification; Stabilisation; Use of additives by change in the physical state, e.g. crystallisation by distillation
Abstract
The present invention provides a kind of production equipments of methyl formate, its advantage is that equipment is simple, low energy consumption, can realize the continuous production of methyl formate.The production equipment includes mainly reaction mass surge tank (1), heat exchanger (2), electric heater (3), synthesis reactor (4), condenser (5), rectifying column feed pump (6), rectifying column (7), compressor (8), methyl nitrite regenerator (9), wherein reaction mass surge tank (1) outlet is connected with heat exchanger (2) material inlet, its outlet is connected with electric heater (3) entrance, the outlet of electric heater (3) is connected with synthesis reactor (4) entrance, its outlet is connected with the heating medium inlet of heat exchanger (2), its Crude product input is connected with condenser (5) material inlet, condensed material enters rectifying column (7) through rectifying column feed pump (6), condenser (5) uncooled gas phase enters methyl nitrite regenerator (9) by compressor (8).
Description
Technical field
The present invention provides a kind of production equipments of chemical products, and in particular to a kind of production equipment of methyl formate belongs to
In the preparing technical field of methyl formate.
Background technology
Methyl formate is a kind of important C1 chemical intermediates, and purposes is than wide.In chemical industry, it can be used
Make the raw material of organic synthesis product, it is also possible to make the solvent in acetate fiber manufacture;In agricultural, it can be used as insecticide, paddy
Class crop sterilizer, fumigant and agent for tobacco treatment etc.;In medicine, it is phonetic to may be used as sulfonic acid methyl pyrimidine, sulfonic acid methoxy for it
The synthesis material of the drugs such as pyridine.The main production process of methyl formate is Liquid Phase Methanol carbonylation method both at home and abroad at present, but should
Method haves the shortcomings that serious:(1) sodium methoxide is unique catalyst, reacts the progress in anhydrous conditions of needs;(2) reaction needs
Progress, the reaction pressure in a kettle wanted are higher;(3) separation of product formic acid methyl esters is cumbersome;(4) technique can not achieve
The continuous production of methyl formate.Patent 201410141259.8 reports a kind of methyl nitrite formyl and is combined to methyl formate
Catalyst and preparation method thereof, using synthesis gas as raw material, specific reaction equation is the technique:
2CO+H2+2CH3ONO→2HCOOCH3+2NO
The reaction be under normal pressure, 120-140 DEG C, catalyst be Pd/ α-Al2O3Under conditions of carry out.
The shortcomings that in order to overcome Liquid Phase Methanol carbonylation method, it is a kind of easy to operate, energy-saving that this just needs us to develop
Production equipment realize the continuous industrial production of methyl formate.
Invention content
The main purpose of the present invention is to provide a kind of production equipments of methyl formate simple in structure, energy-saving.
The production equipment of methyl formate of the present invention includes mainly reaction mass surge tank, heat exchanger, electric heater, synthesis
Reactor, condenser, rectifying column feed pump, rectifying column, compressor, methyl nitrite regenerator, wherein heat exchanger is to be heated
The entrance of material is connected with the outlet of reaction mass to be heated in reaction mass surge tank, the reaction mass to be heated of heat exchanger
Outlet is connected with the entrance of electric heater reaction mass to be heated, the outlet of electric heater reaction mass to be heated and synthetic reaction
The entrance of device reaction mass is connected, and the reacting rear material outlet of synthesis reactor is connected with the entrance of the heat medium of heat exchanger,
The outlet of the heat medium of heat exchanger is connected with the entrance of condenser material to be condensed, and condenser top export and compressor enter
Mouth is connected, and the outlet of compressor is connected with the reaction mass entrance of methyl nitrite regenerator, the tower of methyl nitrite regenerator
Ejection mouth is connected with the entrance of reaction mass surge tank, the bottom end outlet of the condensed product of condenser and entering for rectifying column feed pump
Mouth is connected, and the outlet of rectifying column feed pump is connected with the material inlet for entering rectifying column.
Wherein the synthesis reactor is fixed-bed column reactor, and the rectifying column is board-like continuous rectifying tower.
The production equipment technological process of methyl formate of the present invention is as follows:
Unstripped gas is passed through in proportion in reaction mass surge tank (1) and is uniformly mixed, entered back into heat exchanger (2) and be preheating to
After certain temperature enter electric heater (3), reactor feed gas after the temperature that electric heater (3) is heated to react required, then into
Enter the formylation reaction that synthesis reactor (4) carries out methyl nitrite, the product and reaction end gas generated after reaction, which enters back into, to be changed
Hot device (2) is preheated as heat medium to reaction mass, and heat medium walks shell, and reaction mass walks tube layer, by heat exchange
Afterwards, product and reaction end gas enter condenser (5) and are condensed, condenser (5) top come out gas by compressor (8) into
Enter methyl nitrite regenerator (9), methyl nitrite enters reaction mass surge tank (1) after regeneration, and methyl nitrite is again
Raw tower bottom of tower waste liquid goes liquid waste treating apparatus, the product of condenser (5) bottom to enter rectifying column (7) through rectifying column feed pump (6)
Rectifying is carried out, what rectifying column (7) top obtained is product formic acid methyl esters, and rectifying column (7) bottom of tower waste liquid imports liquid waste treating apparatus.
The advantages of methyl formate production equipment of the present invention is:(1) heat entrained by the material after synthetic reaction is utilized
The energy consumption of electric heater can be reduced to unstripped gas preheating;Material after simultaneously synthesizing reaction is equivalent to carry out in preheater
Then precooling enters back into condenser condensation, can save the dosage of condensate liquid in this way;(2) formic acid may be implemented in the production equipment
The continuous production of methyl esters.
Description of the drawings
Fig. 1 is the structural schematic diagram of methyl formate production equipment of the present invention.Wherein 1 it is reaction mass surge tank, 2 is heat exchange
Device, 3 be electric heater, 4 be synthesis reactor, 5 be condenser, 6 be rectifying column feed pump, 7 be rectifying column, 8 be compressor, 9
For methyl nitrite regenerator.
Specific implementation mode
Methyl formate production equipment of the present invention is described further below in conjunction with the accompanying drawings.
Referring to attached drawing, the production equipment of methyl formate includes mainly:Reaction mass surge tank (1), the volume of the surge tank
It is determined according to the inlet amount of reaction mass gas, volume is 10-20 times of reaction mass inlet amount;Heat exchanger (2), the heat exchange
Device is shell and tube exchanger, and wherein reaction mass walks tube layer, and heat medium walks shell;Electric heater (3), maximum heating temperature
It is 180 DEG C;Synthesis reactor (4), the synthesis reactor are shell and tube reactor, and tubulation number and length can bases in reactor
The loadings of catalyst determine that tubulation internal diameter is 10mm;Condenser (5), which is shell and tube condenser, wherein freezing
Tube layer is walked in agent, and material walks shell;Rectifying column feed pump (6), the feed pump is using diaphragm metering pump;Rectifying column (7), should
Rectifying column is board-like continuous rectifying tower;Compressor (8), the compressor are circulation reciprocating type compressor;Methyl nitrite regenerator
(9), which is the packed tower that gasket packing is vertical type.
The wherein entrance of the material to be heated of heat exchanger (2) and reaction mass to be heated in reaction mass surge tank (1)
Outlet is connected, and the reacting material outlet to be heated of heat exchanger (2) is connected with electric heater (3) reaction mass entrance to be heated, electricity
Heater (3) reacting material outlet to be heated is connected with the reaction mass entrance of synthesis reactor (4), synthesis reactor (4)
Reacting rear material outlet is connected with the entrance of the heat medium of heat exchanger (2), the Crude product input and condenser of heat exchanger (2)
(4) entrance of material to be condensed is connected, and the outlet of condenser (4) uncooled material is connected with the entrance of compressor (8), compressor
(8) outlet is connected with the reaction mass entrance of methyl nitrite regenerator (9), the nitrous acid of methyl nitrite regenerator (9)
The outlet of methyl esters is connected with the entrance of reaction mass surge tank (1), and the bottom of tower waste liquid of methyl nitrite regenerator (9) is gone at waste liquid
Device is managed, the outlet of condenser (4) condensed material is connected with the entrance of rectifying column feed pump (6), rectifying column feed pump (6)
It exports and is connected with the material inlet for entering rectifying column (7), the overhead distillate of rectifying column (7) exports to obtain target product formic acid first
The bottom of tower waste liquid of ester, rectifying column (7) removes liquid waste treating apparatus;The synthesis reactor (4) is fixed-bed column reactor;Institute
It is board-like continuous rectifying tower to state rectifying column (7).
Claims (2)
1. a kind of methyl formate production equipment includes mainly reaction mass surge tank (1), heat exchanger (2), electric heater (3), closes
At reactor (4), condenser (5), rectifying column feed pump (6), rectifying column (7), compressor (8), methyl nitrite regenerator
(9), it is characterised in that the entrance of the material to be heated of heat exchanger (2) and reaction mass to be heated in reaction mass surge tank (1)
Outlet be connected, the entrance phase of the outlet and electric heater (3) reaction mass to be heated of the reaction mass to be heated of heat exchanger (2)
Even, the outlet of electric heater (3) reaction mass to be heated is connected with the entrance of synthesis reactor (4) reaction mass, synthetic reaction
The reacting rear material outlet of device (4) is connected with the entrance of the heat medium of heat exchanger (2), and the heat medium of heat exchanger (2) goes out
Mouth is connected with the entrance of condenser (4) material to be condensed, the entrance of the outlet and compressor (8) of condenser (4) uncooled material
It is connected, the outlet of compressor (8) is connected with the reaction mass entrance of methyl nitrite regenerator (9), methyl nitrite regenerator
(9) outlet of methyl nitrite is connected with the entrance of reaction mass surge tank (1), the bottom of tower of methyl nitrite regenerator (9)
Waste liquid goes liquid waste treating apparatus, the outlet of condenser (4) condensed material to be connected with the entrance of rectifying column feed pump (6), rectifying
The outlet of tower feed pump (6) is connected with the material inlet for entering rectifying column (7), and the overhead distillate of rectifying column (7) exports to obtain
The bottom of tower waste liquid of target product methyl formate, rectifying column (7) removes liquid waste treating apparatus.
2. methyl formate production equipment according to claim 1, it is characterised in that the synthesis reactor (4) is fixed bed
Shell-and-tube reactor;The rectifying column (7) is board-like continuous rectifying tower.
Priority Applications (1)
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CN201810280219.XA CN108484400A (en) | 2018-04-02 | 2018-04-02 | A kind of methyl formate production equipment |
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CN201810280219.XA CN108484400A (en) | 2018-04-02 | 2018-04-02 | A kind of methyl formate production equipment |
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CN108484400A true CN108484400A (en) | 2018-09-04 |
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Citations (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
EP0655433A1 (en) * | 1993-11-30 | 1995-05-31 | Ube Industries, Ltd. | Process for continuously producing dimethyl carbonate |
EP0742198A1 (en) * | 1995-05-12 | 1996-11-13 | Ube Industries Limited | Process for continuously producing dimethyl carbonate |
CN1227839A (en) * | 1999-02-01 | 1999-09-08 | 天津大学 | Process for low-pressure synthesis of dimethyl carbonate by carbon monoxide |
CN1075486C (en) * | 1993-07-15 | 2001-11-28 | 拜尔公司 | Process for the preparation of dimethyl cxarbonate |
CN1724506A (en) * | 2005-07-12 | 2006-01-25 | 中国石油化工集团公司 | Method of producing dimethyl carbonate |
CN102850216A (en) * | 2012-09-27 | 2013-01-02 | 安徽淮化股份有限公司 | Dimethyl oxalate production device |
CN107935856A (en) * | 2017-12-29 | 2018-04-20 | 成都盛利达科技有限公司 | Energy-saving methyl formate process units and its technique |
-
2018
- 2018-04-02 CN CN201810280219.XA patent/CN108484400A/en active Pending
Patent Citations (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN1075486C (en) * | 1993-07-15 | 2001-11-28 | 拜尔公司 | Process for the preparation of dimethyl cxarbonate |
EP0655433A1 (en) * | 1993-11-30 | 1995-05-31 | Ube Industries, Ltd. | Process for continuously producing dimethyl carbonate |
EP0742198A1 (en) * | 1995-05-12 | 1996-11-13 | Ube Industries Limited | Process for continuously producing dimethyl carbonate |
CN1227839A (en) * | 1999-02-01 | 1999-09-08 | 天津大学 | Process for low-pressure synthesis of dimethyl carbonate by carbon monoxide |
CN1724506A (en) * | 2005-07-12 | 2006-01-25 | 中国石油化工集团公司 | Method of producing dimethyl carbonate |
CN102850216A (en) * | 2012-09-27 | 2013-01-02 | 安徽淮化股份有限公司 | Dimethyl oxalate production device |
CN107935856A (en) * | 2017-12-29 | 2018-04-20 | 成都盛利达科技有限公司 | Energy-saving methyl formate process units and its technique |
Non-Patent Citations (1)
Title |
---|
戴珂琦等: "H2对CO偶联制备草酸二甲酯反应影响的研究", 《天然气化工(C1化学与化工)》 * |
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Application publication date: 20180904 |