CN111978184A - Retrieve device of methylamine in follow NMP crude - Google Patents
Retrieve device of methylamine in follow NMP crude Download PDFInfo
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- CN111978184A CN111978184A CN202010960276.XA CN202010960276A CN111978184A CN 111978184 A CN111978184 A CN 111978184A CN 202010960276 A CN202010960276 A CN 202010960276A CN 111978184 A CN111978184 A CN 111978184A
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- methylamine
- tower
- nmp
- recovery
- water
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- BAVYZALUXZFZLV-UHFFFAOYSA-N Methylamine Chemical compound NC BAVYZALUXZFZLV-UHFFFAOYSA-N 0.000 title claims abstract description 686
- SECXISVLQFMRJM-UHFFFAOYSA-N NMP Substances CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 claims abstract description 211
- 238000011084 recovery Methods 0.000 claims abstract description 194
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 88
- 238000000926 separation method Methods 0.000 claims abstract description 82
- LFETXMWECUPHJA-UHFFFAOYSA-N methanamine;hydrate Chemical compound O.NC LFETXMWECUPHJA-UHFFFAOYSA-N 0.000 claims abstract description 37
- 239000000047 product Substances 0.000 claims abstract description 35
- 239000012535 impurity Substances 0.000 claims abstract description 30
- 239000012043 crude product Substances 0.000 claims abstract description 22
- 238000012432 intermediate storage Methods 0.000 claims abstract description 20
- 238000000746 purification Methods 0.000 claims abstract description 10
- 238000010521 absorption reaction Methods 0.000 claims description 125
- 238000010438 heat treatment Methods 0.000 claims description 28
- 239000000463 material Substances 0.000 claims description 26
- 238000004519 manufacturing process Methods 0.000 claims description 18
- 238000006481 deamination reaction Methods 0.000 claims description 15
- 230000009615 deamination Effects 0.000 claims description 12
- 238000005576 amination reaction Methods 0.000 claims description 8
- 239000002253 acid Substances 0.000 claims description 7
- 238000004064 recycling Methods 0.000 claims description 6
- 238000005406 washing Methods 0.000 claims description 5
- 239000002351 wastewater Substances 0.000 claims description 4
- 238000002309 gasification Methods 0.000 claims description 2
- 238000006243 chemical reaction Methods 0.000 abstract description 3
- 230000009286 beneficial effect Effects 0.000 abstract description 2
- 238000007670 refining Methods 0.000 description 81
- YEJRWHAVMIAJKC-UHFFFAOYSA-N 4-Butyrolactone Chemical compound O=C1CCCO1 YEJRWHAVMIAJKC-UHFFFAOYSA-N 0.000 description 41
- 230000018044 dehydration Effects 0.000 description 25
- 238000006297 dehydration reaction Methods 0.000 description 25
- 230000009471 action Effects 0.000 description 17
- 150000001412 amines Chemical class 0.000 description 10
- 238000010586 diagram Methods 0.000 description 9
- 239000007789 gas Substances 0.000 description 8
- 239000001257 hydrogen Substances 0.000 description 5
- 229910052739 hydrogen Inorganic materials 0.000 description 5
- WERYXYBDKMZEQL-UHFFFAOYSA-N butane-1,4-diol Chemical compound OCCCCO WERYXYBDKMZEQL-UHFFFAOYSA-N 0.000 description 4
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 238000003860 storage Methods 0.000 description 3
- 239000006200 vaporizer Substances 0.000 description 3
- KAKZBPTYRLMSJV-UHFFFAOYSA-N Butadiene Chemical compound C=CC=C KAKZBPTYRLMSJV-UHFFFAOYSA-N 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000009833 condensation Methods 0.000 description 2
- 230000005494 condensation Effects 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 238000010992 reflux Methods 0.000 description 2
- 239000007921 spray Substances 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- FFEARJCKVFRZRR-BYPYZUCNSA-N L-methionine Chemical compound CSCC[C@H](N)C(O)=O FFEARJCKVFRZRR-BYPYZUCNSA-N 0.000 description 1
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 1
- 239000002033 PVDF binder Substances 0.000 description 1
- 150000001336 alkenes Chemical class 0.000 description 1
- HSFWRNGVRCDJHI-UHFFFAOYSA-N alpha-acetylene Natural products C#C HSFWRNGVRCDJHI-UHFFFAOYSA-N 0.000 description 1
- 150000004945 aromatic hydrocarbons Chemical class 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000013064 chemical raw material Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 150000001993 dienes Chemical class 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 229920006351 engineering plastic Polymers 0.000 description 1
- 125000002534 ethynyl group Chemical group [H]C#C* 0.000 description 1
- 239000002360 explosive Substances 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000004973 liquid crystal related substance Substances 0.000 description 1
- 229910001416 lithium ion Inorganic materials 0.000 description 1
- 231100000053 low toxicity Toxicity 0.000 description 1
- MROAQUNKLFXYQN-UHFFFAOYSA-N methanamine;sulfuric acid Chemical compound NC.OS(O)(=O)=O MROAQUNKLFXYQN-UHFFFAOYSA-N 0.000 description 1
- 229930182817 methionine Natural products 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- JRZJOMJEPLMPRA-UHFFFAOYSA-N olefin Natural products CCCCCCCC=C JRZJOMJEPLMPRA-UHFFFAOYSA-N 0.000 description 1
- 229920002120 photoresistant polymer Polymers 0.000 description 1
- 238000005554 pickling Methods 0.000 description 1
- 239000002798 polar solvent Substances 0.000 description 1
- 229920002981 polyvinylidene fluoride Polymers 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 238000011027 product recovery Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
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Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C209/00—Preparation of compounds containing amino groups bound to a carbon skeleton
- C07C209/82—Purification; Separation; Stabilisation; Use of additives
- C07C209/86—Separation
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C209/00—Preparation of compounds containing amino groups bound to a carbon skeleton
- C07C209/82—Purification; Separation; Stabilisation; Use of additives
- C07C209/84—Purification
-
- 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
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention belongs to the technical field of NMP purification, and particularly relates to a device for recovering methylamine from a crude NMP product, wherein the crude NMP product comprises methylamine, NMP, water and impurities, the device comprises a methylamine recovery unit, the methylamine recovery unit comprises a methylamine separation section, a methylamine recovery section and a methylamine recovery intermediate storage section, and the methylamine separation section, the methylamine recovery section and the methylamine recovery intermediate storage section are sequentially connected; after the NMP crude product is treated by a methylamine separation working section, methylamine and water enter a methylamine recovery working section, and then enter an intermediate storage working section for recovering methylamine. The invention has the beneficial effects that: after the treatment of a methylamine separation working section and a methylamine recovery working section, unreacted methylamine in the crude NMP product enters a methylamine water recovery intermediate tank, an outlet of a methylamine water high-level tank is connected with the methylamine water high-level tank, and the unreacted methylamine enters an NMP reactor to take part in the reaction, so that the circulation is realized, and the discharge of methylamine is avoided.
Description
Technical Field
The invention belongs to the technical field of NMP purification, and particularly relates to a device for recovering methylamine from a crude NMP product.
Background
N-methyl pyrrolidone (NMP) is a polar solvent and a chemical raw material with strong selectivity and good stability, and has the advantages of high boiling point, nonflammability, low toxicity, safe use, strong dissolving capacity, recoverability, biodegradability and the like. The method is mainly used for extracting agents such as butadiene and aromatic hydrocarbon, purifying acetylene, olefin and diene, solvents of a plurality of engineering plastics (polyvinylidene fluoride and the like), electrode auxiliary materials of lithium ion batteries, photoresist removing liquid, LCD liquid crystal material production, cleaning of circuit boards in the semiconductor industry and the like.
In the existing NMP industrial production process, a crude NMP product contains a large amount of unreacted methylamine, the unreacted methylamine is colorless gas at normal temperature and normal pressure, the specific gravity of the unreacted methylamine is 1.07 times of that of air, and the unreacted methylamine is inflammable, explosive and has strong ammonia-like odor, so that if the unreacted methylamine is directly discharged into the air, the environment pollution is caused, and the great waste is also caused. The existing methylamine recovery tower mainly aims at gas containing methylamine discharged by a factory to carry out acid liquor spray tower absorption, tail gas after absorption is directly emptied, however, the product methylamine sulfate generated after absorption by the equipment cannot be circularly applied to NMP preparation, and the existing acid liquor spray tower has poor absorption effect, tail gas also contains a certain amount of methylamine, the odor around the factory is obvious, and the surrounding working environment is influenced.
Disclosure of Invention
In order to solve the problems, the invention provides a device for recovering methylamine from a crude NMP product, which can absorb and recycle unreacted methylamine.
The invention provides the following technical scheme:
a device for recovering methylamine from a crude NMP product, wherein the crude NMP product comprises methylamine, NMP, water and impurities, the device comprises a methylamine recovery unit, the methylamine recovery unit comprises a methylamine separation section, a methylamine recovery section and a methylamine recovery intermediate storage section, and the methylamine separation section, the methylamine recovery section and the methylamine recovery intermediate storage section are sequentially connected;
after the NMP crude product is treated by a methylamine separation working section, methylamine and water enter a methylamine recovery working section, and then enter an intermediate storage working section for recovering methylamine.
Preferably, the methylamine separation section comprises a flash tank, an deamination tower, a deamination tower pump, a condenser at the top of the deamination tower, a reboiler of the deamination tower, a methylamine separation tower, a first-stage condenser at the top of the methylamine separation tower, a second-stage condenser at the top of the methylamine separation tower and a reboiler of the methylamine separation tower;
the top of the de-amination tower is provided with a de-amination tower top condenser, the bottom of the de-amination tower is provided with a de-amination tower reboiler, the top of the methylamine separation tower is provided with a methylamine separation tower top primary condenser and a methylamine separation tower top secondary condenser which are communicated with each other, the methylamine separation tower top secondary condenser is communicated with a methylamine primary absorption tower, the bottom of the methylamine separation tower is provided with a methylamine separation tower reboiler, and the bottom of the methylamine separation tower is communicated with a methylamine tertiary absorption tower in a methylamine recovery working section through a de-methylamine water pump;
an inlet of the flash tank is communicated with an NMP reactor of an NMP production unit so that a crude NMP product comprising NMP, methylamine, water and impurities enters the flash tank, an outlet of the flash tank is connected with an inlet in the middle of an amine removing tower, a reboiler of the amine removing tower is connected with the amine removing tower and used for heating the crude NMP product entering the amine removing tower, light components and heavy components are separated after heating, the light components comprising methylamine and water are gasified and enter a condenser at the top of the amine removing tower, the condenser at the top of the amine removing tower is provided with two outlets, an outlet I is communicated with the methylamine separating tower so that the methylamine and the water enter the methylamine separating tower, and an outlet II is communicated with a methylamine secondary absorption tower in a methylamine recovery section so that the methylamine; heavy components including NMP, impurities and water are extracted from the bottom of the deamination tower, one part of the heavy components enters a light component removal tower in the NMP purification unit, and the other part of the heavy components enters a light component removal tower in the NMP recovery unit.
A reboiler of the methylamine separation tower is connected with the methylamine separation tower and used for heating materials entering the methylamine separation tower, the reboiler comprises methylamine and water, the heated materials are light and heavy, the light components comprise a large amount of methylamine and a small amount of water, the gasified materials sequentially enter a first-level condenser at the top of the methylamine separation tower and a second-level condenser at the top of the methylamine separation tower, then the gasified materials enter a first-level absorption tower of the methylamine recovery section, the heavy components comprise a small amount of methylamine and a large amount of water, the heavy components are extracted from the bottom of the methylamine separation tower and are treated by a methylamine water pump, the methylamine is sent to a third-level absorption tower of the methylamine recovery section, and wastewater is collected and then treated in a centralized.
Preferably, the methylamine recovery section comprises a methylamine primary absorption tower, a methylamine secondary absorption tower, a methylamine tertiary absorption tower, a methylamine primary absorption circulation cooler, a methylamine secondary absorption circulation cooler, a methylamine tertiary absorption circulation cooler and a methionine washing tank;
the methylamine recovery section also comprises a methylamine primary absorption circulating cooler which forms a circulating loop with the methylamine primary absorption tower; the methylamine primary absorption tower is communicated with a methylamine secondary absorption tower, and the methylamine primary absorption circulating cooler is communicated with a methylamine water recovery intermediate tank;
the methylamine recovery section also comprises a methylamine secondary absorption circulating cooler which forms a circulating loop with the methylamine secondary absorption tower; the methylamine secondary absorption tower is communicated with a methylamine tertiary absorption tower, and the methylamine secondary absorption circulating cooler is connected with the methylamine primary absorption tower;
the methylamine recovery section also comprises a methylamine tertiary absorption circulation cooler which forms a circulation loop with the methylamine tertiary absorption tower; the methylamine tertiary absorption tower is communicated with a methylamine acid washing tank, and the methylamine tertiary absorption circulating cooler is communicated with a methylamine secondary absorption tower;
the materials entering the methylamine primary absorption tower comprise a large amount of methylamine and a small amount of water, the methylamine and the water are condensed in a methylamine primary absorption circulating cooler and flow into an intermediate tank for recovering methylamine water, and high-purity methylamine flows into a methylamine secondary absorption tower; the high-purity methylamine is further subjected to moisture removal in a methylamine secondary absorption circulating cooler and then flows into a methylamine tertiary absorption tower, the methylamine and water condensed in the methylamine secondary absorption circulating cooler flow back to the methylamine primary absorption tower, and the methylamine and water condensed in the methylamine tertiary absorption circulating cooler flow back to the methylamine secondary absorption tower.
Preferably, the intermediate methylamine recovery storage section comprises a methylamine water recovery intermediate tank and a methylamine water recovery pump;
the recycling methylamine water intermediate tank is at least provided with two inlets, wherein the inlet I is connected with the methylamine water high-level tank of the NMP production unit, the inlet II is communicated with the methylamine primary absorption circulation cooler, and the outlet on the recycling methylamine water intermediate tank is connected with the methylamine water high-level tank of the NMP production unit to form a circulation loop.
The invention has the beneficial effects that:
the device for recovering methylamine mainly comprises a methylamine separation section and a methylamine recovery section;
the methylamine separation engineering comprises an amine removing tower, wherein an NMP crude product (methylamine, water, NMP and impurities) in the amine removing tower is heated, light components and heavy components are separated after heating, the light components (methylamine and water) are gasified and enter a condenser at the top of the amine removing tower, the condenser at the top of the amine removing tower is provided with two outlets, the first outlet is communicated with the methylamine separating tower so that methylamine and water enter the methylamine separating tower, and the second outlet is communicated with a methylamine secondary absorption tower in a methylamine recovery working section so that methylamine enters a methylamine secondary absorption tower; heavy components (NMP, impurities and water) are extracted from the bottom of the deamination tower, one part of the heavy components enters a light component removal tower in an NMP purification unit, and the other part of the heavy components enters a light component removal tower in an NMP recovery unit.
Heating materials (methylamine and water) in a methylamine separation tower, separating light and heavy components after heating, gasifying the light components (a large amount of methylamine and a small amount of water), sequentially entering a first-stage condenser at the top of the methylamine separation tower and a second-stage condenser at the top of the methylamine separation tower, then entering a first-stage methylamine absorption tower in a methylamine recovery section, extracting the heavy components (a small amount of methylamine and a large amount of water) from the bottom of the methylamine separation tower, performing methylamine removing water pump treatment, sending the methylamine into a third-stage methylamine absorption tower in the methylamine recovery section, and performing centralized treatment after collecting wastewater;
after the treatment of a methylamine separation working section and a methylamine recovery working section, unreacted methylamine in the crude NMP product enters a methylamine water recovery intermediate tank, an outlet of a methylamine water high-level tank is connected with the methylamine water high-level tank, and the unreacted methylamine enters an NMP reactor to take part in the reaction, so that the circulation is realized, and the discharge of methylamine is avoided.
Drawings
FIG. 1 is a view of the GBL synthesis section;
FIG. 2 is a diagram of an NMP synthesis section;
FIG. 3 is a diagram of the methylamine separation section;
FIG. 4 is a diagram of the methylamine recovery section;
FIG. 5 is a diagram of an intermediate storage section for the recovery of methylamine;
FIG. 6 is a diagram of the NMP lightness-removing section;
FIG. 7 is a drawing of NMP refining section;
FIG. 8 is a diagram of an electronic grade NMP intermediate storage section;
FIG. 9 is a diagram of the lightness-removing section for recovering NMP;
FIG. 10 is a drawing of a refining section for recovering NMP;
FIG. 11 is a diagram of a tar treatment section;
FIG. 12 is a drawing of an NMP recovery section;
FIG. 13 is a drawing of a dehydration section for recovering NMP;
FIG. 14 is a diagram of an intermediate storage section of industrial grade NMP.
The designations in the drawings have the following meanings:
10-GBL production unit 11-BDO intermediate tank 12-BDO raw material pump 13-BDO vaporizer 14-BDO heater 15-GBL reactor 16-GBL heat exchanger 17-GBL condenser 18-GBL buffer tank 19-hydrogen buffer tank
20-NMP production unit 21-GBL elevated tank 22-methylamine water elevated tank 23-NMP reactor 24-methylamine elevated tank
30-methylamine recovery unit 31-methylamine separation section 311-flash drum 312-deamination tower 314-deamination tower overhead condenser 315-deamination tower reboiler 316-methylamine separation tower 317-methylamine separation tower overhead first-level condenser 318-methylamine separation tower overhead second-level condenser 319-methylamine separation tower reboiler
32-methylamine recovery section 321-methylamine primary absorption tower 322-methylamine secondary absorption tower 323-methylamine tertiary absorption tower 324-methylamine primary absorption circulating cooler 325-methylamine secondary absorption circulating cooler 326-methylamine tertiary absorption circulating cooler 327-methylamine pickling tank
33-intermediate methylamine recovery storage section 331-intermediate methylamine water recovery tank 332-methylamine water recovery pump
40-NMP purification unit 41-NMP lightness-removing section 411-lightness-removing tower 412-lightness-removing tower top condenser 413-lightness-removing tower top condensate tank 414-lightness-removing tower vacuum condenser 415-lightness-removing tower vacuum tank 416-lightness-removing tower reboiler
42-NMP refining section 421-refining tower 422-refining tower top condenser 423-refining tower top condensate tank 424-refining tower vacuum condenser 425-refining tower vacuum tank 426-refining tower reboiler
43-electronic grade NMP intermediate storage section 431-electronic grade NMP intermediate tank 432-NMP finished product cooler 433-NMP finished product pump 434-NMP crude product intermediate tank
50-NMP recovery unit 51-NMP recovery lightness-removing section 511-light-removing tower 512-light-removing tower top condenser 513-light-removing tower top condensate tank 514-light-removing tower vacuum condenser 515-light-removing tower vacuum tank 516-light-removing tower reboiler
52-NMP recovery refining section 521-recovery refining tower 522-recovery refining tower top condenser 523-recovery refining tower top condensate tank 524-recovery refining tower vacuum condenser 525-recovery refining tower vacuum tank 526-recovery refining tower reboiler
53-NMP recovery section 531-NMP recovery column 532-NMP recovery overhead condenser 533-NMP recovery column vacuum tank 534-NMP recovery column reboiler 535-recovery dehydration column 536-recovery dehydration column preheater 537-recovery dehydration column overhead condenser 538-recovery dehydration column overhead condensate tank 539-recovery dehydration column vacuum tank 5391-recovery dehydration column reboiler
54-tar processing section 541-tar tower 542-tar tower top condenser 543-tar tower vacuum tank 544-tar tower reboiler
55-technical grade NMP intermediate storage section 551-technical grade NMP intermediate tank 552-NMP product recovery cooler 553-technical grade NMP product pump
Detailed Description
The present invention will be described in detail with reference to the following examples.
BDO is 1, 4-butanediol, GBL is gamma-butyrolactone, NMP is N-methyl pyrrolidone
An NMP process package comprises a GBL production unit 10, an NMP production unit 20, a methylamine recovery unit 30, an NMP purification unit 40 and an NMP recovery unit 50. As will be explained in turn below, the following description,
GBL production unit
The GBL production unit 10 comprises a BDO intermediate tank 11, a BDO raw material pump 12, a BDO vaporizer 13, a BDO heater 14, a GBL reactor 15, a GBL heat exchanger 16, a GBL condenser 17, a GBL buffer tank 18 and a hydrogen buffer tank 19;
1, 4-Butanediol (BDO) flows out from a BDO intermediate tank 11 under the action of a BDO raw material pump 12, and sequentially enters a BDO vaporizer 13 and a BDO heater 14 for heating and gasification; then the mixed gas enters a GBL reactor 15 for reaction to generate mixed gas of a gamma-butyrolactone (GBL) crude product and hydrogen, the mixed gas exchanges heat through a GBL heat exchanger 16, then the mixed gas enters a GBL condenser 17 for condensation, after the condensation, the hydrogen is sent to a hydrogen buffer tank 18, and the gamma-butyrolactone crude product is sent to a GBL buffer tank 19.
Second, NMP production unit
The NMP production unit 20 comprises a GBL high-level tank 21, a methylamine water high-level tank 22, an NMP reactor 23 and a 24-methylamine high-level tank;
the gamma-butyrolactone crude product enters a GBL overhead tank 21 from a GBL buffer tank 19 and then enters an NMP reactor 23, methylamine water enters the NMP reactor 23 from a methylamine water overhead tank 22, the gamma-butyrolactone crude product reacts with the methylamine water in the NMP reactor 23 to obtain an NMP crude product, and the NMP crude product enters a flash tank 311 in a methylamine recovery unit 30 for subsequent treatment.
Methylamine recovery unit
The methylamine recovery unit comprises a methylamine separation section 31, a methylamine recovery section 32 and a methylamine recovery intermediate storage section 33;
the methylamine separation section 31 comprises a flash drum 311, a deamination tower 312, a deamination tower pump 313, a deamination tower top condenser 314, a deamination tower reboiler 315, a methylamine separation tower 316, a methylamine separation tower top primary condenser 317, a methylamine separation tower top secondary condenser 318 and a methylamine separation tower reboiler 319;
the methylamine recovery section 32 comprises a methylamine primary absorption tower 321, a methylamine secondary absorption tower 322, a methylamine tertiary absorption tower 323, a methylamine primary absorption circulating cooler 324, a methylamine secondary absorption circulating cooler 325, a methylamine tertiary absorption circulating cooler 326 and a methylamine acid washing tank 327;
the middle methylamine recovery storage section 33 comprises a methylamine water recovery middle tank 331 and a methylamine water recovery pump 332;
a de-aminating tower top condenser 313 is arranged at the top of the de-aminating tower 312, a de-aminating tower reboiler 315 is arranged at the bottom of the de-aminating tower 312, a methylamine separation tower top primary condenser 317 and a methylamine separation tower top secondary condenser 318 which are communicated with each other are arranged at the top of the methylamine separation tower 316, the methylamine separation tower top secondary condenser 318 is communicated with a methylamine primary absorption tower 321, a methylamine separation tower reboiler 319 is arranged at the bottom of the methylamine separation tower 316, and the bottom of the methylamine separation tower 316 is communicated with a methylamine tertiary absorption tower 326 through a de-aminating water pump;
an inlet of the flash tank 311 is communicated with an NMP reactor 23 of the NMP production unit 20, so that NMP crude products (NMP, methylamine, water and impurities) enter the flash tank 311, an outlet of the flash tank 311 is connected with an inlet in the middle of the deaminizing tower 312, a reboiler 314 of the deaminizing tower is connected with the deaminizing tower 312 and used for heating the NMP crude products entering the deaminizing tower 312, light and heavy components are separated after heating, light components (methylamine and water) are gasified and enter a condenser 314 at the top of the deaminizing tower, the condenser 314 at the top of the deaminizing tower is provided with two outlets, the first outlet is communicated with the methylamine separation tower 316, so that methylamine and water enter the methylamine separation tower 316, and the second outlet is communicated with the second methylamine absorption; heavy components (NMP, impurities, water) are extracted from the bottom of the deamination tower 312, one part of the heavy components enters a lightness-removing tower 411 in the NMP purification unit 40, and the other part of the heavy components enters a recovery lightness-removing tower 511 in the NMP recovery unit 50.
A methylamine separation tower reboiler 319 is connected with a methylamine separation tower 316 and used for heating materials (methylamine and water) entering the methylamine separation tower 316, light and heavy components are separated after heating, the light components (a large amount of methylamine and a small amount of water) are gasified and then sequentially enter a methylamine separation tower top primary condenser 317 and a methylamine separation tower top secondary condenser 318, and then enter a methylamine primary absorption tower 321, the heavy components (a small amount of methylamine and a large amount of water) are extracted from the bottom of the methylamine separation tower 316, after being treated by a methylamine removing water pump, the methylamine is sent to a methylamine tertiary absorption tower 323, and wastewater is collected and then is intensively treated;
the methylamine recovery section 32 further comprises a methylamine first-stage absorption circulation cooler 324 which forms a circulation loop with a methylamine first-stage absorption tower 321; the methylamine primary absorption tower 321 is communicated with a methylamine secondary absorption tower 322, and the methylamine primary absorption circulating cooler 324 is communicated with a recovered methylamine water intermediate tank 331;
the methylamine recovery section 32 further comprises a methylamine secondary absorption circulation cooler 325 which forms a circulation loop with a methylamine secondary absorption tower 322; the methylamine secondary absorption tower 322 is communicated with a methylamine tertiary absorption tower 323, and a methylamine secondary absorption circulating cooler 325 is connected with a methylamine primary absorption tower 321;
the methylamine recovery section 32 further comprises a methylamine tertiary absorption circulation cooler 326 which forms a circulation loop with the methylamine tertiary absorption tower 323; the methylamine tertiary absorption tower 323 is communicated with a methylamine acid washing tank 327, and a methylamine tertiary absorption circulating cooler 326 is communicated with a methylamine secondary absorption tower 322;
the materials (a large amount of methylamine and a small amount of water) entering the methylamine primary absorption tower 321 are condensed in a methylamine primary absorption circulating cooler 324, flow into a methylamine water recovery intermediate tank 331, and high-purity methylamine flows into a methylamine secondary absorption tower 322; further removing moisture from the high-purity methylamine in a methylamine secondary absorption circulating cooler 325, then flowing into a methylamine tertiary absorption tower 323, refluxing the methylamine and water condensed in the methylamine secondary absorption circulating cooler 325 to the methylamine primary absorption tower 321, and refluxing the methylamine and water condensed in the methylamine tertiary absorption circulating cooler 326 to the methylamine secondary absorption tower 322;
the intermediate tank 331 for recycling methylamine water is provided with at least two inlets, wherein the first inlet is connected with the high-level tank 22 for methylamine water of the NMP production unit 20, the second inlet is communicated with the primary methylamine absorption circulating cooler 324, and the outlet of the intermediate tank 331 for recycling methylamine water is connected with the high-level tank 22 for methylamine water of the NMP production unit 20 to form a circulating loop.
Fourth, NMP purification unit
The NMP purification unit 40 comprises an NMP lightness removing section 41, an NMP refining section 42 and an electronic grade NMP intermediate storage section 43;
the NMP lightness-removing section 41 comprises a lightness-removing tower 411, a lightness-removing tower top condenser 412, a lightness-removing tower top condensate tank 413, a lightness-removing tower vacuum condenser 414, a lightness-removing tower vacuum tank 415 and a lightness-removing tower reboiler 416;
the NMP refining section 42 comprises a refining tower 421, a refining tower top condenser 422, a refining tower top condensate tank 423, a refining tower vacuum condenser 424, a refining tower vacuum tank 425 and a refining tower reboiler 426;
the electronic grade NMP intermediate storage section 43 comprises an electronic grade NMP intermediate tank 431, an NMP finished product cooler 432, an NMP finished product pump 433 and an NMP crude product intermediate tank 434;
the top condenser 412 of the lightness-removing tower, the top condensate tank 413 of the lightness-removing tower, the vacuum condenser 414 of the lightness-removing tower and the vacuum tank 415 of the lightness-removing tower are sequentially connected, the inlet of the top condenser 412 of the lightness-removing tower is connected with the top of the lightness-removing tower 411, the middle part of the lightness-removing tower 411 is connected with the deaminizing tower 312, under the action of a pump of the deaminizing tower, a crude NMP (NMP, water and impurities) without methylamine is sent into the lightness-removing tower 411, a reboiler 416 of the lightness-removing tower is connected with the lightness-removing tower 411 and is used for heating materials (NMP, water and impurities) entering the lightness-removing tower 411, light and heavy components are separated after heating, light components (water, NMP and light impurities) are taken out from the top of the lightness-removing tower 411, and flow into the top condensate tank 413 of the lightness-removing tower after being condensed by the top condenser 412 of the top condensate tank 413 of the lightness-removing tower, water and light impurities flow out from, water and NMP flow out from the bottom of a condensate tank 413 at the top of the light component removing tower and enter an NMP recovery tower 531 in an NMP recovery unit 50 under the action of a pump at the top of the light component removing tower; heavy components (NMP, heavier impurities and water) flow out from the bottom of the lightness-removing tower 411, under the action of a pump at the bottom of the lightness-removing tower, one part (NMP, heavier impurities and water) enters the refining tower 421, and the other part (NMP and water) enters an NMP crude product intermediate tank 434;
the refining tower top condenser 422, the refining tower top condensate tank 423, the refining tower vacuum condenser 424 and the refining tower vacuum tank 425 are sequentially connected, the inlet of the refining tower top condenser 422 is connected with the top of the refining tower 421, the middle part of the refining tower 421 is connected with the lightness-removing tower 411, materials (NMP, heavier impurities and water) after lightness removal are sent into the refining tower 421 under the action of a lightness-removing tower bottom pump, a refining tower reboiler 426 is connected with the refining tower 421 and used for heating the materials (NMP, heavier impurities and water) entering the refining tower 421, light and heavy components are separated after heating, light components (NMP and water) are extracted from the top of the refining tower 421, condensed by the refining tower top condenser 422 and then flow into the refining tower top condensate tank 423, water flows out of the top condensate tank 423 and then enters the refining tower vacuum condenser 424 and finally enters the refining tower vacuum tank 425, and NMP and water flow out of the bottom of the refining tower top condensate tank 423, under the action of a pump at the top of the refining tower, one part (NMP) enters an NMP finished product cooler 432, the other part (NMP and water) enters an NMP crude product intermediate tank 434, heavy components (heavier impurities) flow out from the bottom of the refining tower 421, and enter a tar tower 541 in an NMP recovery unit 50 under the action of a pump at the bottom of the refining tower;
an outlet of the NMP finished product cooler 432 is connected with the electronic grade NMP intermediate tank 431, an inlet of the NMP finished product cooler 432 is connected with the refining tower top condensate tank 432 to receive NMP, an inlet of the electronic grade NMP intermediate tank 431 is connected with the recovered finished product NMP cooler 552 in the recovered NMP unit 50 to receive NMP, and the NMP entering the electronic grade NMP intermediate tank 431 enters the electronic grade NMP header pipe under the action of the NMP finished product pump 433;
the NMP crude product intermediate tank 434 is provided with a plurality of inlets which are respectively connected with an NMP recovery tower 531, a tar tower 541, a lightness-removing tower 411, a refining tower top condensate tank 423, a recovery lightness-removing tower 511 and a recovery refining tower top condensate tank 523 and used for receiving NMP and water, and the outlet of the NMP crude product intermediate tank 434 is connected with a recovery dehydrating tower preheater 536.
Fifth, NMP recovery unit
The NMP recovery unit 50 comprises a NMP recovery lightness removing section 51, a NMP recovery refining section 52, a NMP recovery section 53, a tar treatment section 54 and an industrial NMP intermediate storage section 55;
the NMP recovering and light component removing section 51 comprises a recovering and light component removing tower 511, a recovering and light component removing tower top condenser 512, a recovering and light component removing tower top condensate tank 513, a recovering and light component removing tower vacuum condenser 514, a recovering and light component removing tower vacuum tank 515 and a recovering and light component removing tower reboiler 516;
the NMP recovering and refining section 52 comprises a recovering and refining tower 521, a recovering and refining tower top condenser 522, a recovering and refining tower top condensate tank 523, a recovering and refining tower vacuum condenser 524, a recovering and refining tower vacuum tank 525 and a recovering and refining tower reboiler 526;
the NMP recovery section 53 comprises an NMP recovery tower 531, an NMP recovery tower top condenser 532, an NMP recovery tower vacuum tank 533 and an NMP recovery tower reboiler 534;
the tar treatment section 54 comprises a tar tower 541, a tar tower top condenser 542, a tar tower vacuum tank 543 and a tar tower reboiler 544;
the industrial grade NMP intermediate storage section 55 comprises an industrial grade NMP intermediate tank 551, a recovered NMP finished product cooler 552 and an industrial grade NMP finished product pump 553;
the recovery light component removal tower top condenser 512, the recovery light component removal tower top condensate tank 513, the recovery light component removal tower vacuum condenser 514 and the recovery light component removal tower vacuum tank 515 are sequentially connected, an inlet of the recovery light component removal tower top condenser 512 is connected with the top of the recovery light component removal tower 511, the middle part of the recovery light component removal tower 511 is connected with the deaminizing tower 312, materials (NMP, water and impurities) are sent into the recovery light component removal tower 511 under the action of the deaminizing tower pump, a recovery light component removal tower reboiler 526 is connected with the recovery light component removal tower 511 and is used for heating the materials (NMP, water and impurities) entering the recovery light component removal tower 511, light components (water, NMP and light impurities) are separated after heating, light components (water, NMP and light impurities) are collected from the top of the recovery light component removal tower 511, and flow into the recovery light component removal tower top condensate tank 513 after being condensed by the recovery light component removal tower top condenser 512, water and light impurities flow out from the top of the recovery light component removal tower top condensate, finally, the water and the NMP flow out from the bottom of a condensate tank 514 at the top of the recovery and lightness-removing tower and enter an NMP recovery tower 531 under the action of a pump at the top of the recovery and lightness-removing tower; heavy components (NMP, heavier impurities and water) flow out from the bottom of the recovery lightness-removing tower 511, under the action of a pump at the bottom of the recovery lightness-removing tower, one part (NMP, heavier impurities and water) enters a recovery refining tower 521, and the other part (NMP and water) enters an NMP crude product intermediate tank 434;
the recovery refining tower top condenser 522, the recovery refining tower top condensate tank 523, the recovery refining tower vacuum condenser 524 and the recovery refining tower vacuum tank 525 are sequentially connected, an inlet of the recovery refining tower top condenser 522 is connected with the top of the recovery refining tower 521, the middle part of the recovery refining tower 521 is connected with the recovery lightness-removing tower 511, materials (NMP, heavier impurities and water) after lightness removal are sent to the recovery refining tower 521 under the action of a recovery lightness-removing tower bottom pump, a recovery refining tower reboiler 526 is connected with the recovery refining tower 521 and used for heating the materials (NMP, heavier impurities and water) entering the recovery refining tower 521, light and heavy components are separated after heating, the light components (NMP and water) are extracted from the top of the recovery refining tower 521, flow into the recovery refining tower top condensate tank 523 after being condensed by the recovery refining tower top condenser 522, and flow out of the recovery refining tower top condensate tank 523 and then enter the recovery refining tower vacuum condenser 524, finally, the NMP and water flow out from the bottom of a condensate tank 523 at the top of the recovery refining tower, one part of the NMP enters a recovered NMP finished product cooler 552 under the action of a pump at the top of the recovery refining tower, the other part of the NMP and water enters an NMP crude product intermediate tank 434, and heavy components (heavier impurities) flow out from the bottom of the recovery refining tower 521 and enter a tar tower 541 under the action of the pump at the bottom of the recovery refining tower;
the top of the NMP recovery tower 531, a condenser 532 at the top of the NMP recovery tower and a vacuum tank 533 of the NMP recovery tower are sequentially connected, the middle part of the NMP recovery tower 531 is respectively connected with the lightness removing tower 411 and the recovery lightness removing tower 511, materials (NMP and water) are fed into the NMP recovery tower 531 under the action of a pump at the top of the lightness removing tower and a pump at the top of the recovery lightness removing tower, an NMP recovery tower reboiler 534 is connected with the NMP recovery tower 531 and used for heating the materials (NMP and water) entering the NMP recovery tower 531, light and heavy components are separated after heating, the light component (water) is extracted from the top of the NMP recovery tower 531, flows into the vacuum tank 533 of the NMP recovery tower after being cooled by the condenser 532 at the top of the NMP recovery tower, and the heavy component (NMP) enters an;
the middle part of the tar tower 541 is respectively connected with the refining tower 421 and the recovery refining tower 521, materials (tar, possibly containing a small amount of NMP and water) are sent into the tar tower 541 under the action of a refining tower bottom pump and a recovery refining tower bottom pump, a tar tower reboiler 544 is connected with the tar tower 541 and used for heating the materials (tar, NMP and water) entering the tar tower 541, light and heavy components are separated after heating, the light component (water) is extracted from the top of the tar tower 541, cooled by a tar tower top condenser 542 and then flows into a tar tower vacuum tank 543, and the light component (NMP and water) is extracted from the side line of the tar tower 541 and enters an NMP crude product intermediate tank 434;
the industrial grade NMP intermediate tank 551 is provided with two inlets, wherein the first inlet is connected with the NMP finished product cooler 432, the second inlet is connected with the recovered NMP finished product cooler 552, the inlet of the recovered NMP finished product cooler 552 is connected with the recovered dehydration tower 531 for receiving NMP, the recovered NMP finished product cooler 552 is provided with two outlets, the first outlet is connected with the electronic grade NMP intermediate tank 431, the second outlet is connected with the first inlet of the industrial grade NMP intermediate tank 551, and the NMP entering the industrial grade NMP intermediate tank 551 enters the industrial grade NMP main pipe under the action of the industrial grade NMP finished product pump 553.
The NMP recovery section 53 further comprises a recovery dehydration tower 535, a recovery dehydration tower preheater 536, a recovery dehydration tower top condenser 537, a recovery dehydration tower top condensate tank 538, a recovery dehydration tower vacuum tank 539, and a recovery dehydration tower reboiler 5391;
the recovery dehydration tower 535 is connected with the recovery dehydration tower preheater 536, the recovery dehydration tower preheater 536 is connected with an NMP crude product intermediate tank 434 and is used for receiving NMP and water, the recovery dehydration tower reboiler 5391 is connected with the recovery dehydration tower 535 and is used for heating the materials (NMP and water) entering the recovery dehydration tower 535, after heating, light and heavy components are separated, light phase (water) is extracted from the top of the recovery dehydration tower 535, and after cooling by a recovery dehydration tower top condenser 537, the light phase (water) flows into a recovery dehydration tower top condensate tank 538 and finally enters a recovery dehydration tower vacuum tank 539, and the heavy component (NMP) is extracted from the bottom of the recovery dehydration tower 535 and enters an industrial grade NMP intermediate tank 551.
Although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that changes may be made in the embodiments and/or equivalents thereof without departing from the spirit and scope of the invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (4)
1. The device for recovering the methylamine from the crude NMP product is characterized in that the crude NMP product comprises methylamine, NMP, water and impurities, the device comprises a methylamine recovery unit (30), the methylamine recovery unit comprises a methylamine separation section (31), a methylamine recovery section (32) and a methylamine recovery intermediate storage section (33), and the methylamine separation section (31), the methylamine recovery section (32) and the methylamine recovery intermediate storage section (33) are sequentially connected;
after the NMP crude product is treated by a methylamine separation section (31), methylamine and water enter a methylamine recovery section (32) and then enter a methylamine recovery intermediate storage section (33).
2. The apparatus for recovering methylamine from a crude NMP according to claim 1, wherein the methylamine separation section (31) comprises a flash drum (311), a de-amine column (312), a de-amine column pump (313), a de-amine overhead condenser (314), a de-amine column reboiler (315), a methylamine separation column (316), a methylamine separation column overhead primary condenser (317), a methylamine separation column overhead secondary condenser (318), a methylamine separation column reboiler (319);
the top of the de-amination tower (312) is provided with a de-amination tower top condenser (313), the bottom of the de-amination tower (312) is provided with a de-amination tower reboiler (315), the top of the methylamine separation tower (316) is provided with a methylamine separation tower top primary condenser (317) and a methylamine separation tower top secondary condenser (318) which are communicated with each other, the methylamine separation tower top secondary condenser (318) is communicated with a methylamine primary absorption tower (321), the bottom of the methylamine separation tower (316) is provided with a methylamine separation tower reboiler (319), and the bottom of the methylamine separation tower (316) is communicated with a methylamine tertiary absorption tower (326) in a methylamine recovery section (32) through a de-methylamine water pump;
an inlet of the flash tank (311) is communicated with an NMP reactor (23) of the NMP production unit (20) so that a crude NMP product comprising NMP, methylamine, water and impurities enters the flash tank (311), an outlet of the flash tank (311) is connected with an inlet in the middle of the deaminizing tower (312), a reboiler (314) of the deaminizing tower is connected with the deaminizing tower (312) and used for heating the crude NMP product entering the deaminizing tower (312), light and heavy components are separated after heating, the light components comprising methylamine and water are gasified and enter a condenser (314) at the top of the deaminizing tower, the condenser (314) at the top of the deaminizing tower is provided with two outlets, the first outlet is communicated with a methylamine separation tower (316) so that methylamine and water enter the methylamine separation tower (316), and the second outlet is communicated with a methylamine second absorption tower (322) in a methylamine recovery section (32) so that methylamine enters; heavy components including NMP, impurities and water are extracted from the bottom of the deamination tower (312), one part of the heavy components enters a lightness-removing tower (411) in the NMP purification unit (40), and the other part of the heavy components enters a recovery lightness-removing tower (511) in the NMP recovery unit (50).
A methylamine separation tower reboiler (319) is connected with a methylamine separation tower (316) and used for feeding materials into the methylamine separation tower (316), the materials comprise methylamine and water and are heated, light and heavy components are separated after heating, the light components comprise a large amount of methylamine and a small amount of water and enter a methylamine separation tower top primary condenser (317) and a methylamine separation tower top secondary condenser (318) in sequence after gasification, then the materials enter a methylamine primary absorption tower (321) in a methylamine recovery section (32), the heavy components comprise a small amount of methylamine and a large amount of water and are extracted from the bottom of the methylamine separation tower (316), the heavy components are treated by a methylamine water pump and then are fed into a methylamine tertiary absorption tower (323) in a methylamine recovery section (32), and wastewater is collected and then is treated in a centralized mode.
3. The apparatus for recovering methylamine from a crude NMP product according to claim 2, wherein the methylamine recovery section (32) comprises a methylamine primary absorption tower (321), a methylamine secondary absorption tower (322), a methylamine tertiary absorption tower (323), a methylamine primary absorption cycle cooler (324), a methylamine secondary absorption cycle cooler (325), a methylamine tertiary absorption cycle cooler (326) and a methylamine acid wash tank (327);
the methylamine recovery section (32) also comprises a methylamine primary absorption circulating cooler (324) which forms a circulating loop with the methylamine primary absorption tower (321); the methylamine primary absorption tower (321) is communicated with a methylamine secondary absorption tower (322), and the methylamine primary absorption circulating cooler (324) is communicated with a methylamine water recovery intermediate tank (331);
the methylamine recovery section (32) also comprises a methylamine secondary absorption circulating cooler (325) which forms a circulating loop with the methylamine secondary absorption tower (322); the methylamine secondary absorption tower (322) is communicated with a methylamine tertiary absorption tower (323), and the methylamine secondary absorption circulating cooler (325) is connected with a methylamine primary absorption tower (321);
the methylamine recovery section (32) also comprises a methylamine tertiary absorption circulating cooler (326) which forms a circulating loop with the methylamine tertiary absorption tower (323); the methylamine tertiary absorption tower (323) is communicated with a methylamine acid washing tank (327), and the methylamine tertiary absorption circulating cooler (326) is communicated with a methylamine secondary absorption tower (322);
the materials entering the methylamine primary absorption tower (321) comprise a large amount of methylamine and a small amount of water, the methylamine and the water are condensed in a methylamine primary absorption circulating cooler (324) and flow into a recovered methylamine water intermediate tank (331), and the high-purity methylamine flows into a methylamine secondary absorption tower (322); the high-purity methylamine further removes moisture in a methylamine secondary absorption circulating cooler (325), and then flows into a methylamine tertiary absorption tower (323), the methylamine and water condensed in the methylamine secondary absorption circulating cooler (325) flow back to the methylamine primary absorption tower (321), and the methylamine and water condensed in the methylamine tertiary absorption circulating cooler (326) flow back to the methylamine secondary absorption tower (322).
4. An apparatus for recovering methylamine from a crude NMP according to claim 3, wherein the recovered methylamine intermediate storage section (33) comprises a recovered methylamine water intermediate tank (331) and a recovered methylamine water pump (332);
the intermediate tank (331) for recycling the methylamine water is at least provided with two inlets, wherein the first inlet is connected with the methylamine water high-level tank (22) of the NMP production unit (20), the second inlet is communicated with the methylamine primary absorption circulating cooler (324), and the outlet of the intermediate tank (331) for recycling the methylamine water is connected with the methylamine water high-level tank (22) of the NMP production unit (20) to form a circulating loop.
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| CN202010960276.XA CN111978184A (en) | 2020-09-14 | 2020-09-14 | Retrieve device of methylamine in follow NMP crude |
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Cited By (1)
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