CN115106025A - Environment-friendly and energy-saving production device and production method of dimethylformamide - Google Patents
Environment-friendly and energy-saving production device and production method of dimethylformamide Download PDFInfo
- Publication number
- CN115106025A CN115106025A CN202210595767.8A CN202210595767A CN115106025A CN 115106025 A CN115106025 A CN 115106025A CN 202210595767 A CN202210595767 A CN 202210595767A CN 115106025 A CN115106025 A CN 115106025A
- 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.)
- Granted
Links
Images
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
- B01J8/08—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with moving particles
- B01J8/087—Heating or cooling the reactor
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D5/00—Condensation of vapours; Recovering volatile solvents by condensation
- B01D5/0057—Condensation of vapours; Recovering volatile solvents by condensation in combination with other processes
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C231/00—Preparation of carboxylic acid amides
- C07C231/10—Preparation of carboxylic acid amides from compounds not provided for in groups C07C231/02 - C07C231/08
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C231/00—Preparation of carboxylic acid amides
- C07C231/22—Separation; Purification; Stabilisation; Use of additives
- C07C231/24—Separation; Purification
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2208/00—Processes carried out in the presence of solid particles; Reactors therefor
- B01J2208/00008—Controlling the process
- B01J2208/00017—Controlling the temperature
- B01J2208/00106—Controlling the temperature by indirect heat exchange
-
- Y—GENERAL 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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
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. The invention adds two separators and two condensers to replace a circulating liquid cooler and a soft water cooler in the original process flow, simultaneously changes dimethylamine into indirect feeding, and replaces the original process flow that dimethylamine directly enters a synthesis reactor, thereby preventing the dimethylamine containing trace water from directly entering the synthesis reactor and reacting with a sodium methoxide catalyst to generate a catalyst slag substance, preventing the substances from being separated out on the tube walls of the reaction cooler and the dimethylamine cooler, thoroughly solving the problem that a heat exchange tube of the cooler is blocked by the catalyst slag substance in the production process, and ensuring that the production process is more environment-friendly, energy-saving and safe.
Description
Technical Field
The invention belongs to the technical field of dimethylformamide production, and relates to an environment-friendly and energy-saving production device and a production method of dimethylformamide.
Background
Dimethylformamide (DMF) is an important organic chemical raw material and an excellent aprotic polar organic solvent. It can be mixed with water, 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, polyvinyl chloride and the like at normal temperature, so that the solvent is called as an all-purpose solvent; DMF as raw material can be used for synthesizing amine, amide, ether, aldehyde, nitrile, peptide, halogenated, heterocyclic and phosphorus-containing compounds, and can also be used for producing cortisone, chlorpheniramine, doxycycline, vitamin B6, and fluazinam; 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 dry spinning acrylic fibers and synthetic fibers from polyacrylonitrile; DMF can be used as an extracting agent for separating substances, such as extracting butadiene from ethylene cracking gas C4.
The main production process of DMF (as shown in figure 1) is generated by the reaction of dimethylamine and carbon monoxide under the catalysis of sodium methoxide catalyst, because the dimethylamine used as the raw material in the production process contains a small amount of water and the carbon monoxide contains a small amount of carbon dioxide, oxygen, moisture and the like, all the substances can react with sodium methoxide to produce sodium hydroxide, sodium carbonate, sodium formate and the like, and all the substances have small solubility in DMF solution and are easy to separate out on the tube wall of a heat exchange tube of a DMF water cooler. The substances are continuously separated out on the heat exchange tube, so that the heat exchange efficiency of the heat exchanger is influenced, the flow area of the heat exchange tube is blocked, the heat exchange capacity of the heat exchanger is continuously reduced, and finally, the synthesis reactor is forced to be changed over due to the fact that heat emitted during DMF synthesis cannot be taken away in time, 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. Peculiar smell can be produced when the water cooler is cleaned, and the health of workers is influenced. The water cooler is cleaned by high-temperature steam condensate, and accidents such as scalding and the like can occur due to improper operation. And each team and group cleans the water cooler, so that the labor intensity of workers is increased.
The materials in the water cooler are recycled firstly before being cleaned, but the materials in the system are difficult to clean due to more pipeline valves, 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 which have a sterilization effect and cannot be directly subjected to biochemical treatment. The treatment methods commonly used at present are: the incinerator is used for incineration treatment, but the waste water contains a large amount of sodium salt which seriously corrodes the wall of the incinerator; if sodium hydroxide is adopted for alkaline hydrolysis treatment, DMF and sodium hydroxide react to produce dimethylamine and sodium formate, a large amount of steam and sodium hydroxide are consumed, large sodium salt wastewater is generated, and the operation cost is very high.
Therefore, there is a need for an improved process for the production of dimethylformamide.
Disclosure of Invention
The invention aims to provide an environment-friendly and energy-saving production device and a production method of dimethylformamide, which thoroughly solve the problem that a heat exchange tube of a cooler is blocked by catalyst slag substances in the production process, solve the problem that a large amount of amide organic wastewater with high content is generated due to frequent replacement and cleaning of the cooler caused by blockage, improve the heat exchange effect of the cooler, reduce the occurrence of scalding accidents, reduce the labor intensity of operators, and are more environment-friendly, energy-saving and safe.
In order to realize the purpose, the invention adopts the following technical scheme:
the invention provides an environment-friendly and energy-saving production device of dimethylformamide, 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 synthesis reactor; the CO inlet and the catalyst inlet of the synthesis reactor are respectively connected with a CO conveying pipeline and a catalyst conveying pipeline, the gas outlet at the top of the synthesis reactor is sequentially connected with the gas inlet of a condenser and the gas inlet of a tail gas condenser through pipelines, the condensate outlet of the condenser and the condensate outlet of the tail gas condenser are connected with the condensate inlet at the lower part of the synthesis reactor through pipelines, the DMF outlet at the bottom of the synthesis reactor is connected with the liquid inlet at the upper part of a first separator through a pipeline, the gas outlet at the top of the first separator is connected with the gas inlet of a reaction cooler through a pipeline, the condensate outlet of the reaction cooler is connected with the condensate inlet of a second separator through a pipeline, the DMF outlet at the bottom of the first separator is respectively connected with the circulating liquid inlet at the lower part of the second separator and a subsequent rectification system through a pipeline, and the gas outlet at the top of the second separator is connected with the gas inlet of a dimethylamine cooler through a pipeline, a dimethylamine outlet at the bottom of the second separator is connected with a dimethylamine inlet of the synthesis reactor through a pipeline, a dimethylamine inlet at the middle part of the second separator is connected with a dimethylamine delivery pipeline, and a condensate outlet of a dimethylamine cooler is connected with a condensate inlet of the second separator through a pipeline.
In one technical scheme, the non-condensable gas outlet of the tail gas condenser is connected with a flare 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 torch system through pipelines.
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, and the other end of the serpentine coil is connected with a condensate pipeline.
In one technical scheme, a CO distributor is arranged in the synthesis reactor, the CO distributor consists of an inner layer of air distribution pipes and an outer layer of air distribution pipes which are distributed annularly, the outer layer of air distribution pipes are communicated with the inner layer of air distribution pipes through two distributed branch pipes which are distributed in a crossed mode, and a plurality of spray heads are arranged on the inner layer of air distribution pipes along the circumference.
In a preferred technical scheme, the pipe diameter of the outer layer air distribution pipe is larger than that of the inner layer air distribution pipe.
The invention also provides an environment-friendly and energy-saving production method of dimethylformamide, which comprises the following steps:
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 a second separator through a dimethylamine inlet, the temperature of a synthesized material is reduced by utilizing the vaporization and heat absorption of dimethylamine, vaporized dimethylamine steam is cooled and condensed into liquid dimethylamine through a dimethylamine cooler and returns to the second separator by virtue of gravity for recycling, the dimethylamine indirectly cools circulating liquid entering the second separator through continuous vaporization and condensation, the circulating liquid containing the dimethylamine and coming out of the bottom of the second separator is pressurized by a pump and then enters the upper part of a synthesis reactor through the dimethylamine inlet to take away the heat emitted by the synthesis reaction, the operating temperature of the synthesis reactor is 110-120 ℃, and the operating pressure is 2.0 MPa;
unreacted gas-phase materials in the synthesis reactor enter a condenser from the top, after the gas-phase materials are cooled, condensate liquid returns to the synthesis reactor through a condensate liquid inlet, non-condensable gas enters a tail gas condenser, after the non-condensable gas is condensed, the condensate liquid returns to the synthesis reactor through the condensate liquid inlet, and the non-condensable gas at the top is sent to a torch system;
DMF at the bottom of the synthesis reactor enters a first separator, gas at the top of the first separator enters a reaction cooler for cooling after flash evaporation, condensate enters a second separator, non-condensable gas is sent to a torch for burning, a part of DMF at the bottom of the first separator is sent to a subsequent rectification system, and a part of DMF at the bottom of the first separator is sent to the second separator as a 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, the serpentine coil is started at the starting stage of the synthesis reactor to heat circulating liquid in the synthesis reactor by using steam, and when the temperature in the synthesis reactor reaches over 85 ℃, CO is introduced into the synthesis reactor, and dimethylamine is added into the second separator.
In one embodiment, a CO distributor is disposed in the synthesis reactor to uniformly distribute CO introduced into the synthesis reactor.
Compared with the prior art, the invention has the beneficial effects that:
the invention relates to a process for preparing dimethyl formamide, which comprises adding two separators and two condensers instead of a circulating liquid cooler and a soft water cooler in the prior process, gasifying and condensing dimethylamine in the second separator and the dimethylamine cooler to indirectly cool the circulating liquid in the second separator, pressurizing the circulating liquid containing dimethylamine from the bottom of the second separator by a pump, introducing the pressurized circulating liquid into the upper part of a synthesis reactor through an dimethylamine inlet to remove the heat released by the synthesis reaction, and replacing the prior process that the dimethylamine is directly introduced into the synthesis reactor, thereby preventing the dimethylamine containing trace water from directly entering the synthesis reactor to react with a sodium methoxide catalyst to generate catalyst residue substances with low solubility in DMF solution, such as sodium hydroxide, sodium carbonate, sodium formate and the like, and preventing the substances from being separated out on the tube wall of the reaction cooler, this is done: 1) the problem that the heat exchange tube of the cooler is blocked by the catalyst slag in the production process is thoroughly solved, and the stability and continuity of DMF production are ensured; 2) the problem that a large amount of high-content amide organic wastewater is generated due to frequent switching and cleaning of the cooler caused by blockage is solved, so that 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 amount 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 the production method is more energy-saving; 4) the step of cleaning the catalyst slag on the cooler by using hot water is reduced, the occurrence of scalding accidents is reduced, and the labor intensity of operators is also reduced, so that the production method is safer.
Drawings
FIG. 1 is a flow diagram of a process for producing dimethylformamide of the prior art.
FIG. 2 is a flow chart of the process for producing dimethylformamide according to the present invention.
FIG. 3 is a schematic diagram of a serpentine coil in a synthesis reactor according to the present invention.
FIG. 4 is a schematic diagram of a CO distributor in a synthesis reactor according to the present invention.
The reference numbers in the drawings: 1 is the tail gas condenser, 2 is the condenser, 3 is the synthesis reactor, 4 is the synthesis circulating pump, 5 is the circulation liquid cooler, 6 is the soft water circulating pump, 7 is the soft water cooler, 8 is first separator, 9 is the reaction cooler, 10 is the second separator, 11 is the dimethylamine cooler, 12 is the dimethylamine pump, 13 is serpentine coil, 14 is the CO distributor.
Detailed Description
The following examples are intended to illustrate the invention, but are not intended to limit the scope of the invention. Unless otherwise specified, the technical means used in the examples are conventional means well known to those skilled in the art. The test methods in the following examples are conventional methods unless otherwise specified.
Example one
As shown in fig. 2, the environment-friendly and energy-saving dimethylformamide production device of the invention comprises a tail gas condenser 1, a condenser 2 and a synthesis reactor 3, and further comprises a first separator 8, a reaction cooler 9, a second separator 10, a dimethylamine cooler 11 and a dimethylamine circulating pump 12.
Determining the connection relation of each device in the production device according to the material trend, which comprises the following specific steps: a CO inlet and a catalyst inlet of a synthesis reactor 3 are respectively connected with a CO conveying pipeline and a catalyst conveying pipeline, a gas outlet at the top of the synthesis reactor 3 is sequentially connected with a gas inlet of a condenser 2 and a gas inlet of a tail gas condenser 1 through pipelines, a condensate outlet of the condenser 2 and a condensate outlet of the tail gas condenser 1 are connected with a condensate inlet at the lower part of the synthesis reactor 3 through pipelines, a DMF outlet at the bottom of the synthesis reactor 3 is connected with a liquid inlet at the upper part of a first separator 8 through a pipeline, a gas outlet at the top of the first separator 8 is connected with a gas inlet of a reaction cooler 9 through a pipeline, a condensate outlet of the reaction cooler 9 is connected with a condensate inlet of a second separator (10) through a pipeline, and a DMF outlet at the bottom of the first separator 8 is respectively connected with a circulating liquid inlet at the lower part of the second separator 10 and a subsequent rectification system through pipelines, a gas outlet at the top of the second separator 10 is connected with a gas inlet of a dimethylamine cooler 11 through a pipeline, a dimethylamine outlet at the bottom of the second separator 10 is connected with a dimethylamine inlet of the synthesis reactor 3 through a pipeline, a dimethylamine inlet at the middle part of the second separator 10 is connected with a dimethylamine delivery pipeline, and a condensate outlet of the dimethylamine cooler 11 is connected with a condensate inlet of the second separator 10 through a pipeline.
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 methanol aqueous solution at-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 fig. 3, in order to meet the temperature rise requirement of the synthesis reactor 3 in the start-up stage, a group of serpentine coils 13 is arranged in the synthesis reactor 3, one end of each serpentine coil 13 is connected with a steam pipeline, the other end of each serpentine coil 13 is connected with a condensate pipeline, the circulating liquid is heated by directly heating steam, when the temperature in the synthesis reactor 3 reaches above 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 adding amount of the catalyst is determined according to the amount of water, the pressure of the reactor is controlled to be less than or equal to 2.0mpa (g), the temperature is controlled to be 110-120 ℃, 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 air distribution pipe and an outer layer air distribution pipe which are distributed in an annular mode, the outer layer air distribution pipe is communicated with the inner layer air distribution pipe through two distributed branch pipes which are distributed in a crossed mode, a plurality of spray heads are evenly arranged on the inner layer air distribution pipe along the circumference, and the pipe diameter of the outer layer air distribution pipe is larger than that of the inner layer air distribution pipe.
It should be noted that the serpentine 13 and the CO distributor 14 disposed in the synthesis reactor 3 according to the present invention have upper and lower position limitations, and the CO distributor 14 is disposed above the serpentine 13 in order to prevent the serpentine 13 from affecting the gas distribution effect of CO in the synthesis reactor 3.
The production method of the dimethylformamide based on the production device comprises the following steps:
2.3MPa of sodium methoxide catalyst enters the upper part of the synthesis reactor 3 through a catalyst inlet, and 2.3MPa of CO from a gasification device enters the lower part of the synthesis reactor 3 through a CO inlet;
dimethylamine from a methylamine device enters a second separator 10 through a dimethylamine inlet, the temperature of a synthetic material is reduced by utilizing the vaporization and heat absorption of the dimethylamine, vaporized dimethylamine steam is cooled and condensed into liquid dimethylamine through a dimethylamine cooler 11 and returns to the second separator 10 by virtue of gravity for recycling, the dimethylamine indirectly cools a circulating liquid entering the second separator 10 through continuous vaporization and condensation, the circulating liquid containing the dimethylamine and coming out of the bottom of the second separator 10 is pressurized through a dimethylamine pump 12 and then enters the upper part of a synthetic reactor 3 through the dimethylamine inlet to take away the heat discharged by the synthetic reaction, the operating temperature of the synthetic reactor 3 is 110-120 ℃, and the operating pressure is 2.0 MPa;
unreacted gas-phase materials in the synthesis reactor 3 enter the condenser 2 from the top, after being cooled, condensate liquid returns to the synthesis reactor 3 through a condensate liquid inlet, non-condensable gas enters the tail gas condenser 1, after being condensed, the condensate liquid returns to the synthesis reactor 3 through the condensate liquid inlet, and the non-condensable gas at the top 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 burning, a part of DMF at the bottom of the first separator 8 is sent to a subsequent rectification system, and a part of DMF as circulating liquid is sent to the second separator 10 to be mixed with dimethylamine.
In one embodiment, the first separator 8 has an operating pressure of 0.6 to 0.7MPa and the second separator has an operating pressure of 0.55 to 0.65MPa, so that a good gas-liquid separation effect can be achieved.
The invention adds two separators (a first separator 8 and a second separator 10) and two condensers (a reaction cooler 9 and a dimethylamine cooler 11) in the production process of the dimethylformamide to replace a circulating liquid cooler 5 and a soft water cooler 7 in the original process flow, simultaneously, the dimethylamine is continuously gasified and condensed in the second separator 10 and the dimethylamine cooler 11 to indirectly cool the circulating liquid entering the second separator 10, then the circulating liquid containing the dimethylamine and coming out from the bottom of the second separator 10 is pressurized by a pump and enters the upper part of a synthesis reactor 3 through a dimethylamine inlet to take away the heat released by the synthesis reaction, and the invention replaces the original process flow that the dimethylamine directly enters the synthesis reactor, thereby avoiding that the dimethylamine containing a little water directly enters the synthesis reactor 3 to react with a sodium methoxide catalyst to generate sodium hydroxide, The catalyst slag substances such as sodium carbonate and sodium formate, etc., which have low solubility in the DMF solution, thus preventing the substances from being precipitated on the tube wall of the reaction cooler 9, thus: 1) the problem that the heat exchange tube of the cooler is blocked by catalyst slag substances in the production process is thoroughly solved, and the stability and the continuity of DMF production are ensured; 2) the problem that a large amount of high-content amide organic wastewater is generated due to frequent switching and cleaning of the cooler caused by blockage is solved, so that 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 quantity of the circulation liquid entering the synthesis reactor is greatly reduced, the power of the circulation pump is reduced by more than 50 percent, and a soft water circulation pump 6 (the power of the synthesis circulation pump is equivalent to that of a dimethylamine pump 12) is saved, so that the production method is more energy-saving; 4) the step of cleaning the catalyst slag on the cooler by using hot water is reduced, the occurrence of scalding accidents is reduced, and the labor intensity of operators is also reduced, so that the production method is safer.
The above-mentioned embodiments are merely preferred embodiments of the present invention, which are merely illustrative and not restrictive, and it should be understood that other embodiments may be easily made by those skilled in the art by replacing or changing the technical contents disclosed in the specification, and therefore, all changes and modifications that are made on the principle of the present invention should be included in the scope of the claims of the present invention.
Claims (10)
1. The production device of the dimethyl formamide of a kind of environmental protection and energy saving, including end gas condenser (1), condenser (2) and synthesis reactor (3), characterized by, also include the first separator (8), react cooler (9), the second separator (10), dimethylamine cooler (11) and dimethylamine circulating pump (12); the device is characterized in that a CO inlet and a catalyst inlet of a synthesis reactor (3) are respectively connected with a CO conveying pipeline and a catalyst conveying pipeline, a gas outlet at the top of the synthesis reactor (3) is sequentially connected with a gas inlet of a condenser (2) and a gas inlet of a tail gas condenser (1) through pipelines, a condensate outlet of the condenser (2) and a condensate outlet of the tail gas condenser (1) are connected with a condensate inlet at the lower part of the synthesis reactor (3) through pipelines, a DMF outlet at the bottom of the synthesis reactor (3) is connected with a liquid inlet at the upper part of a first separator (8) through a pipeline, a gas outlet at the top of the first separator (8) is connected with a gas inlet of a reaction cooler (9) through a pipeline, a condensate outlet of the reaction cooler (9) is connected with a condensate inlet of a second separator (10) through a pipeline, and a DMF outlet at the bottom of the first separator (8) is respectively connected with a circulating liquid inlet at the lower part of the second separator (10) and a subsequent rectification system through pipelines The gas outlet at the top of the second separator (10) is connected with the gas inlet of a dimethylamine cooler (11) through a pipeline, the dimethylamine outlet at the bottom of the second separator (10) is connected with the dimethylamine inlet of the synthesis reactor (3) through a pipeline, the dimethylamine inlet at the middle part of the second separator (10) is connected with a dimethylamine delivery pipeline, and 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 non-condensable gas outlet of the tail gas condenser (1) is connected to a flare system by means of a pipeline.
3. The production apparatus according to claim 1, wherein the noncondensable gas outlet of the reaction cooler (9) and the noncondensable gas outlet of the dimethylamine cooler (11) are connected to a flare system through pipes.
4. The production plant according to claim 1, characterized in that a serpentine (13) is arranged inside the synthesis reactor (3), said serpentine (13) being connected at one end to a steam line and at the other end to a condensate line.
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 annularly, the outer layer gas distribution pipe is communicated with the inner layer gas distribution pipe through two distributed 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 production device according to claim 5, wherein the pipe diameter of the outer layer air distribution pipe is larger than that of the inner layer air distribution pipe.
7. A dimethylformamide production method based on the production apparatus as set forth in any one of claims 1 to 6, characterized by 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 a second separator (10) through a dimethylamine inlet, the temperature of a synthesized material is reduced by utilizing the vaporization and heat absorption of dimethylamine, vaporized dimethylamine steam is cooled and condensed into liquid dimethylamine through a dimethylamine cooler (11) and returns to the second separator (10) by means of gravity for recycling, the dimethylamine indirectly cools a circulating liquid entering the second separator (10) through continuous vaporization and condensation, the circulating liquid containing dimethylamine and coming out of the bottom of the second separator (10) is pressurized through a pump and then enters the upper part of a synthesis reactor (3) through the dimethylamine inlet to take away the heat emitted by the synthesis reaction, the operating temperature of the synthesis reactor (3) is 110-120 ℃, and the operating pressure is 2.0 MPa;
unreacted gas-phase materials in the synthesis reactor (3) enter a condenser (2) from the top, after being cooled, condensate liquid returns to the synthesis reactor (3) through a condensate liquid inlet, non-condensable gas enters a tail gas condenser (1), after being condensed, the condensate liquid returns to the synthesis reactor (3) through the condensate liquid inlet, and the non-condensable gas at the top 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, one part of DMF at the bottom of the first separator (8) is sent to a subsequent rectification system, and the other part of DMF as circulating liquid is sent to the second separator (10) to be mixed with dimethylamine.
8. The dimethylformamide production process according to claim 7, characterized in that 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 0.65 MPa.
9. The dimethylformamide production method as claimed in claim 7, characterized in that 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 use steam to heat the circulating liquid in the synthesis reactor (3) in the start-up stage of the synthesis reactor (3), 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. A dimethylformamide production process according to claim 7, characterized in that a CO distributor (14) is provided inside said synthesis reactor (3) for the uniform distribution of the CO fed into the synthesis reactor (3).
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 true CN115106025A (en) | 2022-09-27 |
CN115106025B 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) |
Citations (12)
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 |
US20150353477A1 (en) * | 2014-06-09 | 2015-12-10 | Dow Agrosciences Llc | Pesticidal compositions and processes related thereto |
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 |
-
2022
- 2022-05-30 CN CN202210595767.8A patent/CN115106025B/en active Active
Patent Citations (12)
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 |
US20150353477A1 (en) * | 2014-06-09 | 2015-12-10 | Dow Agrosciences Llc | Pesticidal compositions and processes related thereto |
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 (3)
Title |
---|
南碎飞,陈宏艳,窦梅: "N,N-二甲基甲酰胺的清洁生产工艺", 环境污染与防治, no. 05 * |
宋德文;: "短期提高DMF产量的方法探讨", 中氮肥, no. 03 * |
昝海鸥;郭尊礼;: "DMF装置优化改造总结", 中氮肥, no. 02 * |
Also Published As
Publication number | Publication date |
---|---|
CN115106025B (en) | 2023-08-18 |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
CN101157442B (en) | Waste heat reclaiming process for CO transformation | |
EP2367912A2 (en) | Method for heat exchange, system and use | |
CN109847394B (en) | System and method for recycling process waste heat of ethylene glycol rectification device | |
CN101497551A (en) | Methane chlorides production process utilizing chlorination reaction heat | |
CN107158891B (en) | A kind of coal gasified black water flashed vapour utilizes technique | |
CN102408298A (en) | Method of distilling crude benzene by decompression method and device thereof | |
CN103055526B (en) | Method for evaporating cyclohexanone-oxime | |
CN101503336A (en) | Improved methane chloride production process | |
CN106753569A (en) | Low pressure dry powder coal gasifying process | |
CN115745794A (en) | Process and device for producing vinyl acetate by ethylene method | |
CN102844086B (en) | A kind of falling film type stripper decomposed for carbamate | |
CN115106025B (en) | Environment-friendly and energy-saving dimethylformamide production device and production method | |
KR101633832B1 (en) | Apparatus for manufacturing bio fuel using animal and vegetable fats of high acid value | |
CN102337161A (en) | Low water-to-gas ratio serial saturation tower and hot water tower CO conversion process | |
CN218115019U (en) | Skid-mounted equipment for producing mixed hydrogen | |
CN113842852B (en) | Process and system for annual production of 20 ten thousand tons of methylamine | |
CN214840952U (en) | Energy-saving steam air preheater system | |
CN111039752A (en) | Method for continuously producing methanol by hydrogenating methyl formate byproduct in process of preparing ethylene glycol from coal | |
CN103342733B (en) | A kind of extracting method of juice albumen | |
CN115557468A (en) | Method for extracting bromine from brine | |
CN108504392A (en) | A kind of coal gasification apparatus and technique | |
CN107473294A (en) | A kind of handling process and processing system of acrylonitrile recovery tower tower bottoms | |
CN210186750U (en) | VOC recovery system and biodiesel production system | |
CN203486931U (en) | Sewage treatment unit for production of coal chemical industry | |
CN107033967A (en) | Coal gasification apparatus with heat recovery function |
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 |