CN113083204B - NMP synthesis process - Google Patents
NMP synthesis process Download PDFInfo
- Publication number
- CN113083204B CN113083204B CN202110515521.0A CN202110515521A CN113083204B CN 113083204 B CN113083204 B CN 113083204B CN 202110515521 A CN202110515521 A CN 202110515521A CN 113083204 B CN113083204 B CN 113083204B
- Authority
- CN
- China
- Prior art keywords
- monomethylamine
- raw material
- gbl
- tank
- purity
- 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
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
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/24—Stationary reactors without moving elements inside
- B01J19/2415—Tubular reactors
- B01J19/243—Tubular reactors spirally, concentrically or zigzag wound
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F25/00—Flow mixers; Mixers for falling materials, e.g. solid particles
- B01F25/40—Static mixers
- B01F25/42—Static mixers in which the mixing is affected by moving the components jointly in changing directions, e.g. in tubes provided with baffles or obstructions
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D207/00—Heterocyclic compounds containing five-membered rings not condensed with other rings, with one nitrogen atom as the only ring hetero atom
- C07D207/02—Heterocyclic compounds containing five-membered rings not condensed with other rings, with one nitrogen atom as the only ring hetero atom with only hydrogen or carbon atoms directly attached to the ring nitrogen atom
- C07D207/18—Heterocyclic compounds containing five-membered rings not condensed with other rings, with one nitrogen atom as the only ring hetero atom with only hydrogen or carbon atoms directly attached to the ring nitrogen atom having one double bond between ring members or between a ring member and a non-ring member
- C07D207/22—Heterocyclic compounds containing five-membered rings not condensed with other rings, with one nitrogen atom as the only ring hetero atom with only hydrogen or carbon atoms directly attached to the ring nitrogen atom having one double bond between ring members or between a ring member and a non-ring member with hetero atoms or with carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, e.g. ester or nitrile radicals, directly attached to ring carbon atoms
- C07D207/24—Oxygen or sulfur atoms
- C07D207/26—2-Pyrrolidones
- C07D207/263—2-Pyrrolidones with only hydrogen atoms or radicals containing only hydrogen and carbon atoms directly attached to other ring carbon atoms
- C07D207/267—2-Pyrrolidones with only hydrogen atoms or radicals containing only hydrogen and carbon atoms directly attached to other ring carbon atoms with only hydrogen atoms or radicals containing only hydrogen and carbon atoms directly attached to the ring nitrogen atom
-
- 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
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Dispersion Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention belongs to the technical field of chemical production, and particularly relates to an NMP synthesis process, which comprises the following steps: introducing GBL raw material into GBL overhead tank, and introducing high-purity monomethylamine raw material into monomethylamine overhead tank; feeding a GBL raw material with stable pressure from a GBL overhead tank into a static mixer, and feeding a high-purity monomethylamine raw material with stable pressure from a monomethylamine overhead tank into the static mixer; feeding the mixed GBL raw material and the high-purity monomethylamine raw material into a reactor; adding heat conduction oil into the reactor shell to heat the raw materials, so that the raw materials react; after the raw materials react for 2 to 6 hours, discharging the product from the reactor to a residual reaction device for cyclic reaction, and discharging the raw materials for the next working procedure after the reaction reaches the set standard. The raw material of the reactor adopts high-purity monomethylamine, so that the water in the raw material is reduced, the raw material is fully reacted, and the residual raw material in the sewage is reduced, thereby reducing the sewage discharge amount and the treatment cost.
Description
Technical Field
The invention belongs to the technical field of chemical production, and particularly relates to an NMP synthesis process.
Background
NMP is N-methyl pyrrolidone (NMP), which is a high boiling point and environment friendly solvent, and has the advantages of low viscosity, high chemical stability, high heat stability, high polarity, low volatility, infinite miscibility with water and many organic solvents, etc. The market application field of N-methyl pyrrolidone is mainly concentrated in industries such as lithium batteries, circuit boards, insulating materials, petrifaction, medicines, pesticides, cleaning, macromolecules and the like. NMP is produced mainly by ammonification of GBL with monomethylamine.
The prior art CN202010960297.1 discloses a process for synthesizing NMP by using a solid strong acid catalyst, comprising the steps of: preheating 1, 4-butanediol by a preheater and then feeding the preheated 1, 4-butanediol into a vaporizer for vaporization; the vaporized gas phase material enters a heater to be heated, enters a GBL reactor to react, and the temperature of 180-250 ℃ and the normal pressure condition are controlled under the action of a copper catalyst; the mixed gas of the generated butyrolactone and the hydrogen firstly passes through a heat exchanger, then enters a first-stage condenser and a second-stage condenser, one part of the hydrogen is emptied, and the other part of the hydrogen is sent to the hydrogen circulation by a fan; and condensing to obtain a gamma-butyrolactone crude product, directly feeding the gamma-butyrolactone crude product into an NMP reactor, and adding a methylamine solution and a solid strong acid catalyst for reaction to obtain the NMP crude product. The scheme can synthesize the NMP with high purity, fully utilizes heat energy to achieve the effects of energy conservation and consumption reduction, improves the utilization rate of resources, and has higher social use value and application prospect.
The proposal adopts methylamine liquid to increase the transportation cost of raw material purchase, and simultaneously, the sewage treatment capacity is 3.5 times of the reaction theoretical capacity, thereby increasing the sewage treatment capacity and increasing the environmental pollution.
Disclosure of Invention
The scheme provides an NMP synthesis process for reducing sewage treatment capacity.
In order to achieve the above purpose, the present solution provides an NMP synthesis process, which includes the following steps:
step one: introducing GBL raw material into GBL overhead tank, and introducing high-purity monomethylamine raw material into monomethylamine overhead tank;
step two: feeding a GBL raw material with stable pressure from a GBL overhead tank into a static mixer, and feeding a high-purity monomethylamine raw material with stable pressure from a monomethylamine overhead tank into the static mixer;
step three: feeding the mixed GBL raw material and the high-purity monomethylamine raw material into a reactor;
step four: adding heat conduction oil into the reactor shell to heat the raw materials, so that the raw materials react;
step five: after the raw materials react for 2 to 6 hours, discharging the product from the reactor to a residual reaction device for cyclic reaction, and discharging the raw materials for the next working procedure after the reaction reaches the set standard.
The beneficial effects are that: the water in the raw materials is reduced by using the high-purity monomethylamine, so that the sewage treatment capacity after the reaction and the raw material transportation cost are reduced; the residual raw materials in the sewage are reduced by fully reacting the raw materials through the residual reaction device, so that the sewage treatment capacity after the reaction is reduced.
Further, the molar ratio of the high purity monomethylamine feed to the GBL feed in the step two static mixer was 1.06. The process proportion is optimized to 1.06 from 1.11, and the material loss is reduced.
Furthermore, in the second step, a monomethylamine metering pump and a GBL metering pump are adopted to mix the high-purity monomethylamine raw material and the GBL raw material. Can precisely control the mixture ratio of the high-purity monomethylamine raw material and the GBL raw material.
Further, the temperature of the heat conducting oil in the third step is 255-280 ℃.
Further, the reactor in the third step comprises a coil pipe and a shell; the coil pipe is fixedly arranged in the shell; a gap exists between the coil pipe and the shell; and the two ends of the shell are respectively provided with an oil inlet and an oil outlet.
Furthermore, the two ends of the shell are respectively provided with four oil inlets and four oil outlets, so that the heat conduction oil can be rapidly filled up and flows uniformly distributed in the tank body.
Further, the residual reaction device comprises a high-pressure buffer tank, a PLC controller and a monomethylamine detector; the high-pressure buffer tank is communicated with the reactor coil; the high-pressure buffer tank is provided with an exhaust hole, and an electric valve is arranged at the exhaust hole; the exhaust hole is communicated with a disqualified tank which is communicated with the static mixer; the monomethylamine detector is arranged at the feed inlet of the high-pressure buffer tank, and is positioned in the high-pressure buffer tank; the PLC controller is fixedly arranged on the high-pressure buffer tank; and the PLC is electrically connected with the monomethylamine detector and the electric valve switch.
When the product in the coil pipe is discharged into the high-pressure buffer tank, and when the reaction is unqualified, a certain amount of monomethylamine remains in the high-pressure buffer tank, and when the monomethylamine detector detects that the monomethylamine concentration exceeds a set value, the PLC controller controls to open an electric valve, so that the reacted high-temperature gas is discharged into the unqualified tank and enters the static mixer again for reaction. When the concentration of monomethylamine is lower than the set value, the PLC controls the electric valve to be closed. The prior art judges that the product is qualified according to experience or inspection when the product is finished, and the cost of the product is relatively high. And whether the finished product is qualified or not is detected by a monomethylamine detector, and the reaction is performed again after the finished product is unqualified, so that the cost is saved, and the product yield is improved.
Further, a nitrogen inlet is arranged on the high-pressure buffer tank, and the nitrogen inlet is communicated with a high-pressure nitrogen tank; the nitrogen gas inlet is communicated with a first branch pipe, and the outlet of the first branch pipe corresponds to the detection port of the monomethylamine detector; the first branch pipe is internally provided with a first electric valve, and the first electric valve switch is electrically connected with the PLC.
When the monomethylamine detector detects that the monomethylamine concentration exceeds a set value, a PLC controller is enabled to open a first electric valve, a first branch pipe is enabled to be opened, high-pressure nitrogen enters a high-pressure buffer tank from the first branch pipe, and high-pressure gas enables reaction products to completely enter an unqualified tank, so that product residues are prevented; the high-pressure gas can accelerate the reaction speed of the reaction product (for chemical reactions involving gas, other conditions are unchanged (volume is divided), the pressure is increased, namely the volume is reduced, the concentration of the reactant is increased, the number of activated molecules in unit volume is increased, the effective collision times in unit time is increased, and the reaction speed is accelerated), so that the raw materials are fully reacted; and meanwhile, the nitrogen washes the monomethylamine detector, so that monomethylamine is prevented from remaining on the monomethylamine detector, and the sensitivity of the monomethylamine detector is ensured.
Further, the nitrogen gas inlet is communicated with a second branch pipe, and the outlet of the second branch pipe corresponds to the detection port of the monomethylamine detector; a second electric valve is arranged in the second branch pipe, and a second electric valve switch is electrically connected with the PLC; the first branch pipe and the second branch pipe are respectively positioned at two ends of the monomethylamine detector. When the monomethylamine detector detects that the monomethylamine concentration exceeds a set value, the PLC controller is enabled to intermittently switch and open the first electric valve or the second electric valve in set time, so that nitrogen washes the monomethylamine detector, the monomethylamine detector is cleaned more comprehensively, and the sensitivity of the monomethylamine detector is guaranteed.
The beneficial effect of this scheme: continuous production is realized, the productivity reaches tens of thousands of tons/year, and the method is suitable for large-scale industrial production; the water content in the reactor product is 15 percent, which is 27 percent of the prior art, so that the production energy consumption is effectively reduced, the sewage discharge amount is reduced, the national energy conservation and emission reduction policy requirements are met, and the environmental pollution is reduced; the raw material of the reactor adopts high-purity monomethylamine, the transportation cost of unit raw materials is reduced, and the site selection of a factory is not limited; the process proportion is optimized to 1.06 from 1.11, and the material loss is reduced.
Drawings
Fig. 1 is a schematic structural diagram of an embodiment of the present invention.
Fig. 2 is a front view of a high pressure surge tank according to an embodiment of the present invention.
Detailed Description
The following is a further detailed description of the embodiments:
reference numerals in the drawings of the specification include: the device comprises an electric valve 1, a nitrogen inlet pipe 2, a feed pipe 3, a discharge pipe 4, a monomethylamine detector 5, a manhole 6, a hole cover 7, a GBL overhead tank 8, a monomethylamine overhead tank 9, a GBL metering pump 10, a monomethylamine metering pump 11, a static mixer 12, a reactor 13, an oil outlet 14, an oil inlet 15, a reject tank 16, a high-pressure nitrogen tank 17, a high-pressure buffer tank 18, a first branch pipe 19 and a second branch pipe 20.
Examples:
the scheme discloses a device for realizing the synthesis process:
as shown in figure 1, the synthetic production device for generating NMP by the reaction of GBL and high-purity monomethylamine comprises a GBL overhead tank 8, a monomethylamine overhead tank 9, a GBL metering pump 10, a monomethylamine metering pump 11 and a static mixer 12, wherein the GBL overhead tank 8 is communicated with the GBL metering pump 10, the monomethylamine overhead tank 9 is communicated with the monomethylamine metering pump 11, and the GBL metering pump 10 and the monomethylamine metering pump 11 are communicated with the static mixer 12. A methylamine mixer is arranged between the methylamine metering pump 11 and the static mixer 12; a GBL mixer is arranged between the GBL metering pump 10 and the static mixer 12; the monomethylamine mixer is used to provide stable feed to monomethylamine metering pump 11 while also providing a buffer for the feed of system material. The GBL mixer is used for providing stable materials for the GBL metering pump 10 and can buffer the supply of the system materials.
The reactor 13 comprises a coil pipe and a shell, wherein the coil pipe is fixedly arranged in the shell, a gap exists between the coil pipe and the shell, the coil pipe is communicated with the static mixer 12, the shell is provided with an oil inlet 15 and an oil outlet 14, the oil inlet 15 and the oil outlet 14 are both communicated with the coil pipe and the shell in a gap, the left end of the shell is also connected with four oil inlets 15, the four oil inlets 15 are uniformly distributed along the circumferential direction of the shell, the right end of the shell is connected with four oil outlets 14, and the four oil outlets 14 are uniformly distributed along the circumferential direction of the shell. The arrangement enables the heat conduction oil to be filled up rapidly and flow evenly distributed in the tank body. The coil is in communication with a high pressure buffer tank 18.
As shown in figure 2, a monomethylamine detector 5 and a PLC controller are arranged on the high-pressure buffer tank 18, a feed inlet is arranged on the side surface of the bottom of the high-pressure buffer tank 18, and a feed pipe 3 is communicated with the feed inlet. The bottom of the high-pressure buffer tank 18 is provided with a discharge port, the discharge port is communicated with a discharge pipe 4, and a control valve is arranged on the discharge pipe 4.
The high-pressure buffer tank 18 is provided with an exhaust hole, the exhaust hole is provided with an electric valve 1, the exhaust hole is communicated with a disqualified tank 16, the disqualified tank 16 is communicated with the static mixer 12, the monomethylamine detector 5 is arranged at the feed inlet of the high-pressure buffer tank 18, the monomethylamine detector 5 is positioned in the high-pressure buffer tank 18, the model of the amine detector 5 is RBT-6000-ZLG, and the measuring range is 0-100ppm. The PLC is electrically connected with the monomethylamine detector 5 and the switch of the electric valve 1. When the product in the coil pipe is discharged into the high-pressure buffer tank 18, and when the reaction is unqualified, a certain amount of monomethylamine remains in the high-pressure buffer tank 18, and when the monomethylamine detector 5 detects that the monomethylamine concentration exceeds a set value, the PLC controller controls the electric valve 1 to be opened, so that the high-temperature gas after the reaction is discharged into the unqualified tank and enters the static mixer 12 again for reaction. When the monomethylamine concentration is detected to be lower than the set value, the PLC controls the electric valve 1 to be closed. The prior art judges that the product is qualified according to experience or inspection when the product is finished, and the cost of the product is relatively high. Whether the finished product is qualified or not is detected by a monomethylamine detector 5, and the reaction is carried out again after the finished product is unqualified, so that the finished product is saved, and the product yield is improved.
Be equipped with the nitrogen gas air inlet on the high-pressure buffer tank 18, nitrogen gas air inlet intercommunication has high-pressure nitrogen gas jar 17, nitrogen gas air inlet intercommunication has nitrogen gas intake pipe 2, nitrogen gas intake pipe 2 is located the high-pressure buffer tank 18 inside, nitrogen gas intake pipe 2 intercommunication has first branch pipe 19 and second branch pipe 20, first branch pipe 19 and second branch pipe 20 are located the upper and lower extreme of monomethylamine detector 5 respectively, first branch pipe 19 export and second branch pipe 20 export all correspond with monomethylamine detector 5 detection mouth, be equipped with first electric valve in the first branch pipe 19, first electric valve switch is connected with the PLC controller electricity. A second electric valve is arranged in the second branch pipe 20, and a second electric valve switch is electrically connected with the PLC.
When the monomethylamine detector 5 detects that the monomethylamine concentration exceeds a set value, the PLC controller is enabled to intermittently switch and open the first electric valve or the second electric valve in a set time, so that high-pressure nitrogen enters the high-pressure buffer tank 18 from the first branch pipe 19 or the second branch pipe 20, the monomethylamine detector 5 is flushed by the nitrogen, the first branch pipe 19 or the second branch pipe 20 is intermittently started and opened to clean the monomethylamine detector 5 more comprehensively, and the sensitivity of the monomethylamine detector 5 is ensured; the high-pressure nitrogen completely enters the non-mixing tank to prevent the residual of the reaction product; the high-pressure nitrogen can accelerate the reaction speed of the reaction product (for chemical reactions involving gases, other conditions are unchanged (except for volume), the pressure is increased, namely the volume is reduced, the concentration of the reactant is increased, the number of activated molecules in unit volume is increased, the number of effective collisions in unit time is increased, and the reaction speed is accelerated), so that the raw materials are fully reacted.
The manhole 6 is arranged on the side wall of the lower end of the high-pressure buffer tank 18, the manhole 6 is provided with the hole cover 7, the manhole 6 is fixedly connected with the hole cover 7 through bolts, and when the manhole 6 is used for forming sharp overpressure or vacuum in the tank, the accident caused by damaging the storage tank is prevented, and the safety fire-retarding effect can be achieved.
An NMP synthesis process comprising the steps of:
step one: introducing GBL raw material into GBL overhead tank, and introducing high-purity monomethylamine raw material into monomethylamine overhead tank;
step two: feeding a GBL raw material with stable pressure from a GBL overhead tank into a static mixer, and feeding a high-purity monomethylamine raw material with stable pressure from a monomethylamine overhead tank into the static mixer;
adopts a monomethylamine metering pump and a GBL metering pump to mix the high-purity monomethylamine raw material and the GBL raw material. The ratio of the high-purity monomethylamine raw material to the GBL raw material can be accurately controlled;
the molar ratio of the high purity monomethylamine feed to the GBL feed in the static mixer was 1.06. The process proportion is optimized to 1.06 from 1.11, so that the material loss is reduced;
step three: feeding the mixed GBL raw material and the high-purity monomethylamine raw material into a reactor;
step four: adding heat conduction oil into the reactor shell to heat the raw materials, so that the raw materials react; the temperature of the heat conduction oil is 255-280 ℃;
step five: after the raw materials react for 2 to 6 hours, discharging the product from the reactor; the product is discharged into a high-pressure buffer tank 18, the monomethylamine concentration of the reaction product is detected by a monomethylamine detector 5, and when the monomethylamine concentration exceeds a set value of 1ppm, the PLC controller controls the reaction product to be discharged from an exhaust hole of the high-pressure buffer tank 18 into a disqualified tank 16 and then enter the static mixer 12 again for cyclic reaction. And repeating the step 5 until the concentration of the monomethylamine is lower than the set value of 1ppm, opening a control valve of the discharging pipe 4, and allowing the reaction products to enter the next process from the discharging pipe 4.
The scheme realizes continuous production, and the productivity reaches tens of thousands of tons per year, thereby being in line with large-scale industrial production; the water content in the reactor product is 15 percent, which is 27 percent of the prior art, so that the production energy consumption is effectively reduced, the sewage discharge amount is reduced, the national energy conservation and emission reduction policy requirements are met, and the environmental pollution is reduced; the raw material of the reactor adopts high-purity monomethylamine, the transportation cost of unit raw materials is reduced, and the site selection of a factory is not limited; the process proportion is optimized to 1.06 from 1.11, and the material loss is reduced.
The foregoing is merely exemplary embodiments of the present invention, and specific structures and features that are well known in the art are not described in detail herein. It should be noted that modifications and improvements can be made by those skilled in the art without departing from the structure of the present invention, and these should also be considered as the scope of the present invention, which does not affect the effect of the implementation of the present invention and the utility of the patent. The protection scope of the present application shall be subject to the content of the claims, and the description of the specific embodiments and the like in the specification can be used for explaining the content of the claims.
Claims (6)
1. An NMP synthesis process comprising the steps of:
step one: introducing GBL raw material into GBL overhead tank (8), and introducing high-purity monomethylamine raw material into monomethylamine overhead tank (9);
step two: feeding a GBL raw material with stable pressure from a GBL overhead tank (8) into a static mixer (12), and feeding a high-purity monomethylamine raw material with stable pressure from a monomethylamine overhead tank (9) into the static mixer (12);
step three: feeding the mixed GBL raw material and the high-purity monomethylamine raw material into a reactor (13);
step four: adding heat conduction oil into the shell of the reactor (13) to heat the raw materials, so that the raw materials react;
step five: after the raw materials react for 2 to 6 hours, discharging the product from the reactor (13) to a residual reaction device for cyclic reaction, and discharging the raw materials for the next procedure after the reaction reaches the set standard;
the reactor (13) in the third step comprises a coil pipe and a shell; the coil pipe is fixedly arranged in the shell; a gap exists between the coil pipe and the shell; an oil inlet (15) and an oil outlet (14) are respectively arranged at two ends of the shell;
the surplus reaction device comprises a high-pressure buffer tank (18), a PLC (programmable logic controller) and a monomethylamine detector (5), wherein the high-pressure buffer tank (18) is communicated with a coil pipe of a reactor (13), an exhaust hole is formed in the high-pressure buffer tank (18), an electric valve (1) is arranged at the exhaust hole, an unqualified tank (16) is communicated with the exhaust hole, the unqualified tank (16) is communicated with a static mixer (12), the monomethylamine detector (5) is arranged at a feed inlet of the high-pressure buffer tank (18), the monomethylamine detector (5) is positioned in the high-pressure buffer tank (18), the PLC is fixedly arranged on the high-pressure buffer tank (18), and the PLC is electrically connected with switches of the monomethylamine detector (5) and the electric valve (1);
be equipped with nitrogen gas air inlet on high-pressure buffer tank (18), nitrogen gas air inlet intercommunication has high-pressure nitrogen gas jar (17), nitrogen gas air inlet intercommunication has first branch pipe (19), and first branch pipe (19) export is corresponding with monomethylamine detector (5) detection mouth, be equipped with first electric valve in first branch pipe (19), first electric valve switch is connected with the PLC controller electricity.
2. The NMP synthesis process according to claim 1, characterized by: the molar ratio of the high-purity monomethylamine feed to the GBL feed in the step two static mixer (12) was 1.06.
3. The NMP synthesis process according to claim 1, characterized by: in the second step, a monomethylamine metering pump (11) and a GBL metering pump (10) are adopted to mix the high-purity monomethylamine raw material and the GBL raw material.
4. The NMP synthesis process according to claim 1, characterized by: and in the fourth step, the temperature of the heat conduction oil is 255-280 ℃.
5. The NMP synthesis process according to claim 1, characterized by: four oil inlets (15) and four oil outlets (14) are respectively arranged at two ends of the shell.
6. The NMP synthesis process according to claim 1, characterized by: the nitrogen gas air inlet is communicated with a second branch pipe (20), an outlet of the second branch pipe (20) corresponds to a detection port of the monomethylamine detector (5), a second electric valve is arranged in the second branch pipe (20), a second electric valve switch is electrically connected with the PLC, and the first branch pipe (19) and the second branch pipe (20) are respectively positioned at two ends of the monomethylamine detector (5).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110515521.0A CN113083204B (en) | 2021-05-12 | 2021-05-12 | NMP synthesis process |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110515521.0A CN113083204B (en) | 2021-05-12 | 2021-05-12 | NMP synthesis process |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN113083204A CN113083204A (en) | 2021-07-09 |
| CN113083204B true CN113083204B (en) | 2023-07-11 |
Family
ID=76665258
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202110515521.0A Active CN113083204B (en) | 2021-05-12 | 2021-05-12 | NMP synthesis process |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN113083204B (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115819313B (en) * | 2022-05-17 | 2024-04-02 | 重庆中润新材料股份有限公司 | NMP production process capable of realizing hydrogen recycling |
| CN115819312B (en) * | 2022-05-17 | 2023-11-07 | 重庆中润新材料股份有限公司 | Production method for preparing NMP (N-methyl pyrrolidone) from anhydrous monomethylamine |
Family Cites Families (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| BE1012946A6 (en) * | 1999-10-27 | 2001-06-05 | Pantochim Sa | METHOD FOR PRODUCING N-Methyl PYRROLIDONE USING THE GAMMA-BUTYROLACTONE METHYLAMINES AND MIXED AS STARTING MATERIALS. |
| CN103058910B (en) * | 2013-01-21 | 2014-09-17 | 郑州大学 | Separation method of organic amine impurity in N-methyl pyrrolidinone |
| CN103351321B (en) * | 2013-06-20 | 2015-08-26 | 滨州裕能化工有限公司 | The continuous production method of a kind of NMP |
| CN203602531U (en) * | 2013-12-17 | 2014-05-21 | 山东庆云长信化学科技有限公司 | N-methyl pyrrolidone production device |
| CN205035303U (en) * | 2015-10-12 | 2016-02-17 | 宿迁新亚科技有限公司 | Consecutive reaction device of N - methyl carboxamide |
| CN107297184A (en) * | 2017-07-03 | 2017-10-27 | 无锡科伦达化工热力装备有限公司 | A kind of reactor for producing N methyl pyrrolidones |
| CN208917104U (en) * | 2018-09-19 | 2019-05-31 | 赣州中能实业有限公司 | A kind of preparation facilities of N-Methyl pyrrolidone |
| CN209715906U (en) * | 2018-12-25 | 2019-12-03 | 江苏众智启澄环境工程技术有限公司 | Underwater water quality sensor automatic cleaning apparatus |
| CN210332195U (en) * | 2019-06-30 | 2020-04-17 | 载元派尔森新能源科技有限公司 | Excessive methylamine recovery and concentration device in NMP preparation |
| CN210815146U (en) * | 2019-08-28 | 2020-06-23 | 山东长信化学科技股份有限公司 | Stable NMP reaction feeding device |
| CN211035757U (en) * | 2019-11-26 | 2020-07-17 | 四川天华富邦化工有限责任公司 | Tubular system for preparing N-methyl pyrrolidone by condensation method of butyrolactone and methylamine |
| CN211771009U (en) * | 2019-12-26 | 2020-10-27 | 重庆市中润化学有限公司 | NMP continuous synthesis system |
| CN211863907U (en) * | 2020-03-18 | 2020-11-06 | 南通利奥化工科技有限公司 | Distillation tower for improving methanol content |
| CN212168314U (en) * | 2020-04-21 | 2020-12-18 | 常州捷卓智能科技有限公司 | A wash purifier for washing SF6 analyte tester sensor |
-
2021
- 2021-05-12 CN CN202110515521.0A patent/CN113083204B/en active Active
Also Published As
| Publication number | Publication date |
|---|---|
| CN113083204A (en) | 2021-07-09 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN113083204B (en) | NMP synthesis process | |
| CN109707992A (en) | A kind of multi-functional charging hydrogenation stations | |
| CN110975578A (en) | Three-waste zero-emission nanoparticle supercritical hydrothermal synthesis system and method | |
| CN104555958A (en) | Synthesis process of lithium hexafluorophosphate | |
| CN103803584A (en) | Ammonium bifluoride preparation method | |
| CN211754876U (en) | Micro-channel reactor | |
| CN103553004A (en) | Method for continuous preparation of sodium azide | |
| CN100391663C (en) | Process for preparing nano nickel powder | |
| CN1027809C (en) | Method for synthesizing paraffin chloride | |
| CN107089961B (en) | A kind of method that continuous hydrogenation produces methylhexahydrophthalic anhydride | |
| RU2690013C1 (en) | System and method of producing vanadium electrolyte with high purity and high activity | |
| CN113083205B (en) | NMP synthesizer | |
| CN110452264A (en) | A kind of preparation method of high optical selective essence glufosinate-ammonium ammonium salt | |
| CN209655011U (en) | A kind of multi-functional charging hydrogenation stations | |
| CN212113896U (en) | Novel low-temperature alcohol reforming fuel cell system | |
| CN212894326U (en) | Wet oxidation reaction system for water treatment | |
| CA2915364C (en) | Method and industrial process for continuous synthesis of different ionic liquids | |
| CN111668510A (en) | Novel low-temperature alcohol reforming fuel cell system | |
| CN111675423A (en) | Treatment method and system for nicotinic acid medical intermediate wastewater | |
| CN103131481A (en) | Biosynthetic fuel | |
| CN215028840U (en) | A device for green degradation of polyethylene glycol terephthalate | |
| CN105366642B (en) | A kind of rare earth synthesizes AlH3Method | |
| CN108003030A (en) | A kind of pipelineization continuously prepares the method and device of 5- nitro -1,4- dihydros -1,4- endo-methylene groups-naphthalene | |
| CN211688262U (en) | Rotary kiln type spray reaction device for preparing insoluble sulfur through closed cycle | |
| CN106995926A (en) | A kind of method that electrochemical catalysis deposition prepares the aluminum hydrides of α tri- |
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 | ||
| CB02 | Change of applicant information |
Address after: No.18, Huabei 2nd Road, Changshou District, Chongqing 401221 Applicant after: Chongqing Zhongrun New Materials Co.,Ltd. Address before: No.18, Huabei 2nd Road, Changshou District, Chongqing 401221 Applicant before: Chongqing Zhong run Chemical Co.,Ltd. |
|
| CB02 | Change of applicant information | ||
| CB03 | Change of inventor or designer information |
Inventor after: Ding Longqi Inventor after: Zhao Jianjun Inventor before: Lu Chuanxue Inventor before: Ding Longqi Inventor before: Lv Yucheng Inventor before: Zhao Jianjun Inventor before: You Lin |
|
| CB03 | Change of inventor or designer information | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |