CN115106025B - Environment-friendly and energy-saving dimethylformamide production device and production method - Google Patents

Environment-friendly and energy-saving dimethylformamide production device and production method Download PDF

Info

Publication number
CN115106025B
CN115106025B CN202210595767.8A CN202210595767A CN115106025B CN 115106025 B CN115106025 B CN 115106025B CN 202210595767 A CN202210595767 A CN 202210595767A CN 115106025 B CN115106025 B CN 115106025B
Authority
CN
China
Prior art keywords
dimethylamine
separator
synthesis reactor
cooler
inlet
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Active
Application number
CN202210595767.8A
Other languages
Chinese (zh)
Other versions
CN115106025A (en
Inventor
程建军
徐爱军
张超奇
张连飞
尉宏光
陈义全
许耀辉
刘纪中
高毅
赵利利
祁宏亮
李楠
杨晓芳
王琰
刘小羽
牛振
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Anyang Jiutian Fine Chemical Co ltd
Original Assignee
Anyang Jiutian Fine Chemical Co ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Anyang Jiutian Fine Chemical Co ltd filed Critical Anyang Jiutian Fine Chemical Co ltd
Priority to CN202210595767.8A priority Critical patent/CN115106025B/en
Publication of CN115106025A publication Critical patent/CN115106025A/en
Application granted granted Critical
Publication of CN115106025B publication Critical patent/CN115106025B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • 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
    • B01J8/087Heating or cooling the reactor
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D5/00Condensation of vapours; Recovering volatile solvents by condensation
    • B01D5/0057Condensation of vapours; Recovering volatile solvents by condensation in combination with other processes
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C231/00Preparation of carboxylic acid amides
    • C07C231/10Preparation of carboxylic acid amides from compounds not provided for in groups C07C231/02 - C07C231/08
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C231/00Preparation of carboxylic acid amides
    • C07C231/22Separation; Purification; Stabilisation; Use of additives
    • C07C231/24Separation; Purification
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2208/00Processes carried out in the presence of solid particles; Reactors therefor
    • B01J2208/00008Controlling the process
    • B01J2208/00017Controlling the temperature
    • B01J2208/00106Controlling the temperature by indirect heat exchange
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00Technologies relating to chemical industry
    • Y02P20/10Process efficiency

Landscapes

  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

The invention belongs to the technical field of dimethylformamide production, and discloses an environment-friendly and energy-saving dimethylformamide production device which comprises a tail gas condenser, a synthesis reactor, a first separator, a reaction cooler, a second separator, a dimethylamine cooler and a dimethylamine circulating pump. According to the invention, two separators and two condensers are additionally arranged to replace a circulating liquid cooler and a soft water cooler in the original process flow, and dimethylamine is changed into indirect feeding to replace the direct feeding of dimethylamine into a synthesis reactor in the original process flow, so that the dimethylamine containing trace water is prevented from directly entering the synthesis reactor and reacting with sodium methoxide catalyst to generate catalyst slag substances, the substances are prevented from being separated out on the pipe walls of the reaction cooler and the dimethylamine cooler, the problem that the heat exchange pipe of the cooler is blocked by the catalyst slag substances in the production process is thoroughly solved, and the production process is more environment-friendly, energy-saving and safer.

Description

Environment-friendly and energy-saving dimethylformamide production device and production method
Technical Field
The invention belongs to the technical field of dimethylformamide production, and relates to an environment-friendly and energy-saving dimethylformamide production device and method.
Background
Dimethylformamide (DMF) is an important organic chemical raw material and an excellent aprotic polar organic solvent. It can be mixed with water, diethyl ether, ethanol, kerosene, chlorinated hydrocarbon, aromatic hydrocarbon and most organic solvents, and can dissolve polymers such as ethyl cellulose, nitrocellulose, butyl acetate cellulose, polyacrylonitrile, vinyl chloride and polyvinyl chloride at normal temperature, and is called as a totipotent solvent; DMF is used as raw material, and can be used for synthesizing amine, amide, ether, aldehyde, nitrile, peptide, halogenated, heterocycle and phosphorus-containing compound, and can also be used for producing medicines such as cortisone, chlorphenamine, doxycycline, vitamin B6, and flex-expelling agent; can be used as a catalyst for chemical reaction; DMF can be used as a solvent for wet polyurethane synthetic leather and a solvent for preparing acrylic fibers and synthetic fibers by dry spinning of polyacrylonitrile; DMF may be used as an extractant for separation of substances, such as for extraction of butadiene from ethylene cracking gas C4, etc.
The main production process of DMF (shown in figure 1) is that dimethylamine and carbon monoxide react under the catalysis of sodium methoxide catalyst, and because dimethylamine as raw material used in the production process contains trace water, carbon monoxide contains trace carbon dioxide, oxygen, moisture and the like, the substances can react with sodium methoxide to produce sodium hydroxide, sodium carbonate, sodium formate and the like, the solubility of the substances in DMF solution is very small, and the substances are easy to separate out on the pipe wall of a heat exchange pipe of a DMF water cooler. These substances are continuously separated out on the heat exchange tube, so that the heat exchange efficiency of the heat exchanger is affected, the flow area of the heat exchange tube is blocked, the heat exchange capacity of the heat exchanger is continuously reduced, and finally, the heat released during DMF synthesis cannot be timely taken away, so that the synthesis reactor is overtemperature, the water cooler is forced to be switched, the reaction materials in the water cooler are discharged, and the water cooler is cleaned by hot water, so that the heat exchange capacity of the water cooler is recovered. The water cooler can generate peculiar smell during cleaning, which affects the health of workers. The water cooler is cleaned by using high-temperature steam condensate, and accidents such as scalding and the like can occur due to improper operation. Each team cleans the water cooler, which increases the labor intensity of workers.
The materials in the water cooler are recovered before cleaning, but because of the more pipeline valves, the materials in the system are difficult to clean, a large amount of organic wastewater is generated when the water cooler is cleaned by hot water, and the wastewater contains a large amount of amide substances, so that the wastewater has a bactericidal effect and cannot be directly subjected to biochemical treatment. The treatment methods commonly used at present are as follows: the incinerator is used for incineration treatment, but the waste water contains a large amount of sodium salt, so that the sodium salt severely corrodes the incinerator wall; if sodium hydroxide is adopted for alkaline hydrolysis, DMF and sodium hydroxide react to produce dimethylamine and sodium formate, so that a large amount of steam and sodium hydroxide are consumed, and large sodium salt wastewater is produced, and the operation cost is high.
Thus, there is a need for improved processes for the production of dimethylformamide.
Disclosure of Invention
The invention aims to provide an environment-friendly and energy-saving dimethylformamide production device and a production method, which thoroughly solve the problem that a cooler heat exchange tube is blocked by catalyst slag substances in the production process, solve the problem that a cooler needs frequent switching and cleaning to generate a large amount of high-content amide organic wastewater, improve the heat exchange effect of the cooler, reduce the occurrence of scalding accidents, lighten the labor intensity of operators, and are more environment-friendly, energy-saving and safer.
In order to achieve the above purpose, the present invention adopts the following technical scheme:
the invention provides an environment-friendly and energy-saving dimethylformamide production device, which comprises a tail gas condenser, a synthesis reactor, a first separator, a reaction cooler, a second separator, a dimethylamine cooler and a dimethylamine circulating pump, wherein the tail gas condenser is connected with the reaction cooler; the method comprises the steps that a CO inlet and a catalyst inlet of a synthesis reactor are respectively connected with a CO conveying pipeline and a catalyst conveying pipeline, a gas outlet at the top of the synthesis reactor is sequentially connected with a gas inlet of a condenser and a gas inlet of a tail gas condenser through pipelines, a condensate outlet of the condenser and a condensate outlet of the tail gas condenser are connected with a condensate inlet at the lower part of the synthesis reactor through pipelines, a DMF outlet at the bottom of the synthesis reactor is connected with a liquid inlet at the upper part of a first separator through pipelines, a gas outlet at the top of the first separator is connected with a gas inlet of a reaction cooler through pipelines, a condensate outlet of the reaction cooler is connected with a condensate inlet of a second separator through pipelines, a DMF outlet at the bottom of the first separator is respectively connected with a circulating liquid inlet at the lower part of the second separator and a subsequent rectifying system through pipelines, a dimethylamine outlet at the top of the second separator is connected with a dimethylamine inlet of the synthesis reactor through pipelines, a dimethylamine inlet at the middle part of the second separator is connected with a dimethylamine conveying pipeline, and a condensate outlet of the dimethylamine cooler is connected with a condensate inlet of the second separator through pipelines.
In one technical scheme, the noncondensable gas outlet of the tail gas condenser is connected with a torch system through a pipeline.
In one technical scheme, the non-condensable gas outlet of the reaction cooler and the non-condensable gas outlet of the dimethylamine cooler are both connected with a flare system through pipelines.
In one technical scheme, a serpentine coil is arranged in the synthesis reactor, and one end of the serpentine coil is connected with a steam pipeline, and the other end of the serpentine coil is connected with a condensate pipeline.
In one technical scheme, be provided with the CO distributor in the synthetic reactor, the CO distributor comprises the inside and outside multilayer gas distribution pipe of annular distribution, and outer gas distribution pipe communicates each other with the inlayer gas distribution pipe through two distributing branch pipes of alternately distributing, sets up a plurality of shower nozzles along the circumference on the inlayer gas distribution pipe.
In a preferred technical scheme, the pipe diameter of the outer-layer gas distribution pipe is larger than that of the inner-layer gas distribution pipe.
The invention also provides an environment-friendly and energy-saving dimethylformamide production method, which comprises the following steps of:
2.3MPa of catalyst enters the upper part of the synthesis reactor through a catalyst inlet, and 2.3MPa of CO enters the lower part of the synthesis reactor through a CO inlet;
dimethylamine enters the second separator through a dimethylamine inlet, the dimethylamine is utilized to absorb heat by vaporization to reduce the temperature of a synthetic material, the vaporized dimethylamine steam is cooled by a dimethylamine cooler and then condensed into liquid dimethylamine, the liquid dimethylamine returns to the second separator by gravity for recycling, the dimethylamine is continuously vaporized and condensed to indirectly finish cooling the circulating liquid entering the second separator, the circulating liquid containing dimethylamine, which is discharged from the bottom of the second separator, enters the upper part of the synthesis reactor through the dimethylamine inlet after being pressurized by a pump to take away the heat released by the synthesis reaction, and the operation temperature of the synthesis reactor is 110-120 ℃ and the operation pressure is 2.0MPa;
unreacted gas phase materials in the synthesis reactor enter a condenser from the top, condensate returns to the synthesis reactor through a condensate inlet after being cooled, noncondensable gas enters a tail gas condenser, condensate returns to the synthesis reactor through a condensate inlet after being condensed, and top noncondensable gas is sent to a flare system;
and (3) enabling DMF at the bottom of the synthesis reactor to enter a first separator, enabling gas at the top of the first separator to enter a reaction cooler for cooling after flash evaporation, enabling condensate to enter a second separator, enabling non-condensable gas to be sent to a torch for incineration, enabling a part of DMF at the bottom of the first separator to be sent to a subsequent rectifying system, and enabling a part of DMF at the bottom of the first separator to be sent into the second separator as circulating liquid to be mixed with dimethylamine.
In one technical scheme, the operating pressure of the first separator is 0.6-0.7 MPa, and the operating pressure of the second separator is 0.55-0.65 MPa.
In one technical scheme, a serpentine coil is arranged in the synthesis reactor, one end of the serpentine coil is connected with a steam pipeline, the other end of the serpentine coil is connected with a condensate pipeline, steam is used for heating circulating liquid in the synthesis reactor by starting the serpentine coil in the start-up stage of the synthesis reactor, and when the temperature in the synthesis reactor reaches more than 85 ℃, CO is introduced into the synthesis reactor, and dimethylamine is added into the second separator.
In one technical scheme, a CO distributor is arranged in the synthesis reactor and is used for uniformly distributing CO introduced into the synthesis reactor.
Compared with the prior art, the invention has the beneficial effects that:
the invention adds two separators and two condensers to replace the circulating liquid cooler and soft water cooler in the original process flow, simultaneously, the circulating liquid entering the second separator is cooled indirectly by continuously gasifying and condensing dimethylamine in the second separator and the dimethylamine cooler, and then the circulating liquid containing dimethylamine from the bottom of the second separator enters the upper part of the synthesis reactor through a dimethylamine inlet after being pressurized by a pump to take away the heat released by the synthesis reaction, thereby replacing the prior process flow to directly enter dimethylamine into the synthesis reactor, thereby avoiding the dimethylamine containing trace water from directly entering the synthesis reactor to react with sodium methoxide catalyst to generate catalyst slag substances with lower solubility in DMF solution, such as sodium hydroxide, sodium carbonate, sodium formate and the like, and avoiding the precipitation of the substances on the pipe wall of the reaction cooler, and the invention comprises the following steps: 1) Thoroughly solves the problem that the heat exchange tube of the cooler is blocked by catalyst slag substances in the production process, and ensures the stability and continuity of DMF production; 2) Solves the problem that the cooler is blocked and needs frequent switching and cleaning to generate a large amount of high-content amide organic wastewater, so the production method is more environment-friendly; 3) Because the cooler has no blockage problem, the heat exchange effect of the cooler is improved, the circulation volume of the circulating liquid entering the synthesis reactor is greatly reduced, the power of the circulating pump is reduced by more than 50 percent, and meanwhile, a soft water circulating pump is omitted, so that the production method is more energy-saving; 4) The method reduces the steps of using hot water to clean the catalyst residues on the cooler, reduces the occurrence of scalding accidents, and also reduces the labor intensity of operators, so that the production method is safer.
Drawings
FIG. 1 is a flow chart of a prior art dimethylformamide production process.
FIG. 2 is a flow chart of the dimethylformamide production process according to the present invention.
FIG. 3 is a schematic diagram of the structure of a serpentine coil in a synthesis reactor according to the present invention.
FIG. 4 is a schematic diagram of the structure of a CO distributor in the synthesis reactor of the present invention.
The reference numbers in the drawings: the device comprises a tail gas condenser 1, a condenser 2, a synthesis reactor 3, a synthesis circulating pump 4, a circulating liquid cooler 5, a soft water circulating pump 6, a soft water cooler 7, a first separator 8, a reaction cooler 9, a second separator 10, a dimethylamine cooler 11, a dimethylamine pump 12, a serpentine coil 13 and a CO distributor 14.
Detailed Description
The following examples are illustrative of the present invention and are not intended to limit the scope of the invention. The technical means used in the examples are conventional means well known to those skilled in the art unless otherwise indicated. The test methods in the following examples are conventional methods unless otherwise specified.
Example 1
As shown in fig. 2, the invention relates to an environment-friendly and energy-saving dimethylformamide production device, which comprises a tail gas condenser 1, a condenser 2, a synthesis reactor 3, a first separator 8, a reaction cooler 9, a second separator 10, a dimethylamine cooler 11 and a dimethylamine circulating pump 12.
The connection relation of each device in the production device is determined according to the material trend, and the connection relation is specifically as follows: the CO inlet and the catalyst inlet of the synthesis reactor 3 are respectively connected with a CO material conveying pipeline and a catalyst material conveying pipeline, the gas outlet at the top of the synthesis reactor 3 is sequentially connected with the gas inlet of the condenser 2 and the gas inlet of the tail gas condenser 1 through pipelines, the condensate outlet of the condenser 2 and the condensate outlet of the tail gas condenser 1 are connected with the gas inlet at the lower part of the synthesis reactor 3 through pipelines, the DMF outlet at the bottom of the synthesis reactor 3 is connected with the liquid inlet at the upper part of the first separator 8 through pipelines, the gas outlet at the top of the first separator 8 is connected with the gas inlet of the reaction cooler 9 through pipelines, the condensate outlet of the reaction cooler 9 is connected with the condensate inlet of the second separator (10) through pipelines, the DMF outlet at the bottom of the first separator 8 is respectively connected with the circulating liquid inlet at the lower part of the second separator 10 and the subsequent rectification system through pipelines, the gas outlet at the top of the second separator 10 is connected with the gas inlet of the dimethylamine cooler 11 through pipelines, the dimethylamine outlet at the bottom of the second separator 10 is connected with the dimethylamine inlet of the synthesis reactor 3 through pipelines, the dimethylamine inlet at the middle part of the second separator 10 is connected with the dimethylamine inlet of the dimethylamine cooler through pipelines, and the condensate outlet of the dimethylamine cooler 11 is connected with the condensate inlet of the second separator 10.
As shown in fig. 2, the condenser 2, the reaction cooler 9 and the dimethylamine cooler 11 in the invention are all cooled by circulating water, the tail gas condenser 1 is cooled by a methanol water solution with the temperature of minus 10 ℃, and the non-condensable gas outlet of the tail gas condenser 1, the non-condensable gas outlet of the reaction cooler 9 and the non-condensable gas outlet of the dimethylamine cooler 11 are all connected with a torch system through pipelines.
As shown in figure 3, in order to meet the heating requirement of the synthesis reactor 3 in the starting stage, a group of serpentine coils 13 are arranged in the synthesis reactor 3, one end of each serpentine coil 13 is connected with a steam pipeline, the other end is connected with a condensate pipeline, circulating liquid is directly heated by steam to heat, when the temperature in the synthesis reactor 3 reaches more than 85 ℃, CO is introduced into the synthesis reactor 3, dimethylamine is added into the second separator 10, the components of the reaction liquid are analyzed, the catalyst addition amount is determined according to the water content, the reactor pressure is controlled to be less than or equal to 2.0MPa (G), the temperature is controlled to be between 110 and 120 ℃, and the liquid level is controlled to be about 80%.
As shown in fig. 4, a CO distributor 14 is provided in the synthesis reactor 3 to uniformly distribute CO introduced into the synthesis reactor 3. The CO distributor 14 is composed of an inner layer gas distribution pipe and an outer layer gas distribution pipe which are distributed in a ring shape, and the outer layer gas distribution pipe is communicated with the inner layer gas distribution pipe through two distribution branch pipes which are distributed in a cross mode, a plurality of spray heads are evenly arranged on the inner layer gas distribution pipe along the circumference, and the pipe diameter of the outer layer gas distribution pipe is larger than that of the inner layer gas distribution pipe.
It should be noted that the serpentine coil 13 and the CO distributor 14 disposed in the synthesis reactor 3 according to the present invention have upper and lower positions, and in order to prevent the serpentine coil 13 from affecting the gas distribution effect of CO in the synthesis reactor 3, the CO distributor 14 is disposed above the serpentine coil 13.
The production method of the dimethylformamide based on the production device comprises the following steps:
2.3MPa sodium methoxide catalyst enters the upper part of the synthesis reactor 3 through a catalyst inlet, and 2.3MPa CO from the gasification device enters the lower part of the synthesis reactor 3 through a CO inlet;
dimethylamine from a methylamine device enters the second separator 10 through a dimethylamine inlet, the dimethylamine is utilized to absorb heat by vaporization to reduce the temperature of a synthetic material, vaporized dimethylamine steam is cooled by a dimethylamine cooler 11 and then condensed into liquid dimethylamine, the liquid dimethylamine returns to the second separator 10 by gravity for recycling, the dimethylamine is continuously vaporized and condensed to indirectly finish cooling the circulating liquid entering the second separator 10, the circulating liquid containing dimethylamine from the bottom of the second separator 10 is pressurized by a dimethylamine pump 12 and then enters the upper part of the synthesis reactor 3 through the dimethylamine inlet to take away the heat released by the synthesis reaction, the operating temperature of the synthesis reactor 3 is 110-120 ℃, and the operating pressure is 2.0MPa;
unreacted gas phase materials in the synthesis reactor 3 enter the condenser 2 from the top, condensate is cooled and then returned to the synthesis reactor 3 through a condensate inlet, noncondensable gas enters the tail gas condenser 1, condensate is condensed and then returned to the synthesis reactor 3 through a condensate inlet, and the top noncondensable gas is sent to a torch system;
DMF at the bottom of the synthesis reactor 3 enters a first separator 8, gas at the top of the first separator 8 enters a reaction cooler 9 for cooling after flash evaporation, condensate enters a second separator 10, noncondensable gas is sent to a torch for incineration, and a part of DMF at the bottom of the first separator 8 is sent to a subsequent rectifying system, and the other part of DMF is sent into the second separator 10 as circulating liquid to be mixed with dimethylamine.
In one embodiment, the operation pressure of the first separator 8 is 0.6-0.7 mpa, and the operation pressure of the second separator is 0.55-0.65 mpa, so that a better gas-liquid separation effect can be achieved.
In the dimethylformamide production process, two separators (a first separator 8 and a second separator 10) and two condensers (a reaction cooler 9 and a dimethylamine cooler 11) are additionally arranged to replace a circulating liquid cooler 5 and a soft water cooler 7 in the original process flow, and simultaneously, the circulating liquid entering the second separator 10 is cooled indirectly by continuously gasifying and condensing dimethylamine in the second separator 10 and the dimethylamine cooler 11, and then the circulating liquid containing dimethylamine, which is discharged from the bottom of the second separator 10, enters the upper part of the synthesis reactor 3 through a dimethylamine inlet after being pressurized by a pump so as to take away the heat released by the synthesis reaction, and replaces the prior process flow to directly enter the dimethylamine into the synthesis reactor, thereby avoiding the direct entering of the dimethylamine containing trace water into the synthesis reactor 3, reacting with sodium methoxide catalyst to generate catalyst slag substances with lower solubility in DMF solution, such as sodium carbonate, sodium formate and the like, and avoiding the precipitation of the substances on the pipe wall of the reaction cooler 9, so that: 1) Thoroughly solves the problem that the heat exchange tube of the cooler is blocked by catalyst slag substances in the production process, and ensures the stability and continuity of DMF production; 2) Solves the problem that the cooler is blocked and needs frequent switching and cleaning to generate a large amount of high-content amide organic wastewater, so the production method is more environment-friendly; 3) Because the cooler has no blockage problem, the heat exchange effect of the cooler is improved, the circulation volume of the circulating liquid entering the synthesis reactor is greatly reduced, the power of the circulating pump is reduced by more than 50 percent, and meanwhile, the soft water circulating pump 6 (the power of the synthesis circulating pump is equivalent to that of the dimethylamine pump 12) is omitted, so that the production method is more energy-saving; 4) The method reduces the steps of using hot water to clean the catalyst residues on the cooler, reduces the occurrence of scalding accidents, and also reduces the labor intensity of operators, so that the production method is safer.
The above-mentioned embodiments are merely preferred embodiments of the present invention, which are not intended to limit the scope of the present invention, and other embodiments can be easily made by those skilled in the art through substitution or modification according to the technical disclosure in the present specification, so that all changes and modifications made in the principle of the present invention shall be included in the scope of the present invention.

Claims (10)

1. The production device of the dimethylformamide comprises a tail gas condenser (1), a condenser (2) and a synthesis reactor (3), and is characterized by further comprising a first separator (8), a reaction cooler (9), a second separator (10), a dimethylamine cooler (11) and a dimethylamine circulating pump (12); the CO inlet and the catalyst inlet of the synthesis reactor (3) are respectively connected with a CO material conveying pipeline and a catalyst material conveying pipeline, the gas outlet at the top of the synthesis reactor (3) is sequentially connected with the gas inlet of the condenser (2) and the gas inlet of the tail gas condenser (1) through pipelines, the condensate outlet of the condenser (2) and the condensate outlet of the tail gas condenser (1) are respectively connected with the condensate inlet at the lower part of the synthesis reactor (3) through pipelines, the DMF outlet at the bottom of the synthesis reactor (3) is connected with the liquid inlet at the upper part of the first separator (8) through pipelines, the gas outlet at the top of the first separator (8) is connected with the gas inlet of the reaction cooler (9) through pipelines, the condensate outlet of the reaction cooler (9) is connected with the condensate inlet of the second separator (10) through pipelines, the DMF outlet at the bottom of the first separator (8) is respectively connected with the circulating liquid inlet at the lower part of the second separator (10) and the subsequent rectification system through pipelines, the gas outlet at the top of the second separator (10) is connected with the gas inlet of the dimethylamine cooler (11) through pipelines, the dimethylamine outlet at the bottom of the second separator (10) is connected with the dimethylamine inlet at the middle part of the second separator (3) through pipelines, the condensate outlet of the dimethylamine cooler (11) is connected with the condensate inlet of the second separator (10) through a pipeline.
2. The production plant according to claim 1, characterized in that the noncondensable gas outlet of the off-gas condenser (1) is connected to a flare system by means of a pipe.
3. The production plant according to claim 1, characterized in that the non-condensable gas outlet of the reaction cooler (9) and the non-condensable gas outlet of the dimethylamine cooler (11) are both connected to a flare system by piping.
4. The production device according to claim 1, characterized in that a serpentine coil (13) is arranged in the synthesis reactor (3), one end of the serpentine coil (13) being connected to a steam pipe and the other end being connected to a condensate pipe.
5. The production device according to claim 1, wherein a CO distributor (14) is arranged in the synthesis reactor (3), the CO distributor (14) is composed of an inner layer gas distribution pipe and an outer layer gas distribution pipe which are distributed in a ring shape, the outer layer gas distribution pipe is mutually communicated with the inner layer gas distribution pipe through two distribution branch pipes which are distributed in a crossed manner, and a plurality of spray heads are arranged on the inner layer gas distribution pipe along the circumference.
6. The apparatus for producing of claim 5, wherein the pipe diameter of the outer cloth pipe is greater than the pipe diameter of the inner cloth pipe.
7. The method for producing dimethylformamide based on the production apparatus according to any one of claims 1 to 6, comprising the steps of:
2.3MPa of catalyst enters the upper part of the synthesis reactor (3) through a catalyst inlet, and 2.3MPa of CO enters the lower part of the synthesis reactor (3) through a CO inlet;
dimethylamine enters the second separator (10) through a dimethylamine inlet, the temperature of a synthetic material is reduced by utilizing dimethylamine vaporization and absorption heat, vaporized dimethylamine steam is cooled by a dimethylamine cooler (11) and then condensed into liquid dimethylamine, the liquid dimethylamine returns to the second separator (10) by gravity for recycling, the dimethylamine is continuously vaporized and condensed to indirectly finish cooling the circulating liquid entering the second separator (10), the circulating liquid containing dimethylamine, which is discharged from the bottom of the second separator (10), enters the upper part of the synthesis reactor (3) through the dimethylamine inlet after being pressurized by a pump so as to take away the heat released by the synthesis reaction, and the operating temperature of the synthesis reactor (3) is 110-120 ℃ and the operating pressure is 2.0MPa;
unreacted gas phase materials in the synthesis reactor (3) enter the condenser (2) from the top, condensate returns to the synthesis reactor (3) through a condensate inlet after being cooled, noncondensable gas enters the tail gas condenser (1), condensate returns to the synthesis reactor (3) through a condensate inlet after being condensed, and the top noncondensable gas is sent to a torch system;
DMF at the bottom of the synthesis reactor (3) enters a first separator (8), gas at the top of the first separator (8) enters a reaction cooler (9) for cooling after flash evaporation, condensate enters a second separator (10), non-condensable gas is sent to a torch for incineration, a part of DMF at the bottom of the first separator (8) is sent to a subsequent rectifying system, and the other part of DMF is sent into the second separator (10) as circulating liquid for mixing with dimethylamine.
8. The dimethylformamide production process according to claim 7, wherein the operating pressure of the first separator (8) is 0.6 to 0.7mpa and the operating pressure of the second separator is 0.55 to 0.65mpa.
9. The dimethylformamide production method as claimed in claim 7, wherein a serpentine coil (13) is arranged in the synthesis reactor (3), one end of the serpentine coil (13) is connected with a steam pipeline, the other end of the serpentine coil is connected with a condensate pipeline, the serpentine coil (13) is started to heat circulating liquid in the synthesis reactor (3) by utilizing steam in a starting stage of the synthesis reactor (3), and when the temperature in the synthesis reactor (3) reaches above 85 ℃, CO is introduced into the synthesis reactor (3), and dimethylamine is added into the second separator (10).
10. The dimethylformamide production process according to claim 7, wherein a CO distributor (14) is provided in the synthesis reactor (3) for uniformly distributing CO introduced into the synthesis reactor (3).
CN202210595767.8A 2022-05-30 2022-05-30 Environment-friendly and energy-saving dimethylformamide production device and production method Active CN115106025B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202210595767.8A CN115106025B (en) 2022-05-30 2022-05-30 Environment-friendly and energy-saving dimethylformamide production device and production method

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202210595767.8A CN115106025B (en) 2022-05-30 2022-05-30 Environment-friendly and energy-saving dimethylformamide production device and production method

Publications (2)

Publication Number Publication Date
CN115106025A CN115106025A (en) 2022-09-27
CN115106025B true CN115106025B (en) 2023-08-18

Family

ID=83326400

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202210595767.8A Active CN115106025B (en) 2022-05-30 2022-05-30 Environment-friendly and energy-saving dimethylformamide production device and production method

Country Status (1)

Country Link
CN (1) CN115106025B (en)

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN116143659A (en) * 2022-12-20 2023-05-23 陕西延长石油(集团)有限责任公司 System and method for preparing dimethylamine N, N-dimethylcarbamate from carbon dioxide and dimethylamine

Citations (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR79635E (en) * 1960-03-29 1962-12-28 Exxon Research Engineering Co Process for the production of methyl esters of polycarboxylic aromatic acids
US6723877B1 (en) * 2003-06-16 2004-04-20 Air Products And Chemicals, Inc. Dimethylformamide synthesis via reactive distillation of methyl formate and dimethylamine
CN1680273A (en) * 1994-10-27 2005-10-12 住友化学株式会社 Process for producing n-(1-(2,4-dichlorophenyl)ethyl)-2- cyano-3,3-dimethylbutanamide
CN1908569A (en) * 2006-08-14 2007-02-07 浙江大学 Method for heat exchanger anti-blocking in N,N-dimethyl formamide production process and anti-blocking heat exchanger
WO2014146961A1 (en) * 2013-03-18 2014-09-25 Evonik Industries Ag Process for preparation of methacrylic acid and methacrylic acid esters
CN204093422U (en) * 2014-07-14 2015-01-14 鲁西化工集团股份有限公司氯碱化工分公司 A kind of dimethyl formamide reactor and corollary equipment
CN206396087U (en) * 2016-12-08 2017-08-11 陕西延长石油兴化化工有限公司 A kind of DMF reactors indirect type heat-exchanger rig
AR105789A2 (en) * 2008-04-30 2017-11-08 Xyleco Inc METHOD FOR PREPARING A SACAROSE SOLUTION
WO2017190299A1 (en) * 2016-05-05 2017-11-09 章旭元 Seven-tower five-effect rectification system for dmac or dmf waste liquid and method for recovering same
WO2020246902A1 (en) * 2019-06-07 2020-12-10 Uniwersytet Warszawski An initiator of atrp radical polymerisation, a method of its synthesis, and a method of synthesis of low-dispersion polymer and copolymer using this initiator
CN213446917U (en) * 2020-08-05 2021-06-15 洛阳友汇环保设备股份有限公司 Dimethyl formamide (DMF) waste liquid recycling device

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
TWI667224B (en) * 2014-06-09 2019-08-01 美商陶氏農業科學公司 Pesticidal compositions and processes related thereto

Patent Citations (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR79635E (en) * 1960-03-29 1962-12-28 Exxon Research Engineering Co Process for the production of methyl esters of polycarboxylic aromatic acids
CN1680273A (en) * 1994-10-27 2005-10-12 住友化学株式会社 Process for producing n-(1-(2,4-dichlorophenyl)ethyl)-2- cyano-3,3-dimethylbutanamide
US6723877B1 (en) * 2003-06-16 2004-04-20 Air Products And Chemicals, Inc. Dimethylformamide synthesis via reactive distillation of methyl formate and dimethylamine
CN1908569A (en) * 2006-08-14 2007-02-07 浙江大学 Method for heat exchanger anti-blocking in N,N-dimethyl formamide production process and anti-blocking heat exchanger
AR105789A2 (en) * 2008-04-30 2017-11-08 Xyleco Inc METHOD FOR PREPARING A SACAROSE SOLUTION
WO2014146961A1 (en) * 2013-03-18 2014-09-25 Evonik Industries Ag Process for preparation of methacrylic acid and methacrylic acid esters
CN204093422U (en) * 2014-07-14 2015-01-14 鲁西化工集团股份有限公司氯碱化工分公司 A kind of dimethyl formamide reactor and corollary equipment
WO2017190299A1 (en) * 2016-05-05 2017-11-09 章旭元 Seven-tower five-effect rectification system for dmac or dmf waste liquid and method for recovering same
CN206396087U (en) * 2016-12-08 2017-08-11 陕西延长石油兴化化工有限公司 A kind of DMF reactors indirect type heat-exchanger rig
WO2020246902A1 (en) * 2019-06-07 2020-12-10 Uniwersytet Warszawski An initiator of atrp radical polymerisation, a method of its synthesis, and a method of synthesis of low-dispersion polymer and copolymer using this initiator
CN213446917U (en) * 2020-08-05 2021-06-15 洛阳友汇环保设备股份有限公司 Dimethyl formamide (DMF) waste liquid recycling device

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
DMF装置优化改造总结;昝海鸥;郭尊礼;;中氮肥(02);全文 *

Also Published As

Publication number Publication date
CN115106025A (en) 2022-09-27

Similar Documents

Publication Publication Date Title
CN101570375B (en) Method for recovery and cascade utilization of waste heat of supercritical water treatment system of waste organic substances
CN101157442B (en) Waste heat reclaiming process for CO transformation
CN115106025B (en) Environment-friendly and energy-saving dimethylformamide production device and production method
CN107399870B (en) Texaco gasifier black water heat recovery processing system
CN103055526B (en) Method for evaporating cyclohexanone-oxime
CN102502901B (en) Condensed fluid stripping method matched with CO transforming device
CN106753569A (en) Low pressure dry powder coal gasifying process
CN110937744B (en) Dimethylamine treatment process in synthetic leather DMF (dimethyl formamide) wastewater heat pump rectification process
CN201190132Y (en) Coalgas phenol-containing water treatment device
CN102337161A (en) Low water-to-gas ratio serial saturation tower and hot water tower CO conversion process
CN211688931U (en) Device for recovering heat of coal water slurry gasification flash system
CN218115019U (en) Skid-mounted equipment for producing mixed hydrogen
CN103864602A (en) Energy-saving acyclic acid preparation system having two sets of oxidation devices and one set of refining unit and energy-saving acyclic acid preparation method
CN113842852B (en) Process and system for annual production of 20 ten thousand tons of methylamine
CN214840952U (en) Energy-saving steam air preheater system
CN107473294A (en) A kind of handling process and processing system of acrylonitrile recovery tower tower bottoms
CN108504392A (en) A kind of coal gasification apparatus and technique
CN114028831A (en) Sleeve type desulfurization slurry flash evaporation heat extraction system and working method thereof
CN210186750U (en) VOC recovery system and biodiesel production system
CN116023250A (en) PTA process waste heat recovery system, PTA process system and PTA process
CN203486931U (en) Sewage treatment unit for production of coal chemical industry
CN206188752U (en) Powder coal gasification system is done to low pressure
CN102635779A (en) New liquid chlorine vaporizing technology and system
CN207313499U (en) A kind of device using biomass material rapid polymerization humic acid
CN218710086U (en) Low-pressure methanol synthesis device

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant