CN111978233B - Device for improving purity of NMP crude product after demethanization - Google Patents
Device for improving purity of NMP crude product after demethanization Download PDFInfo
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- CN111978233B CN111978233B CN202010967636.9A CN202010967636A CN111978233B CN 111978233 B CN111978233 B CN 111978233B CN 202010967636 A CN202010967636 A CN 202010967636A CN 111978233 B CN111978233 B CN 111978233B
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- 239000012043 crude product Substances 0.000 title claims abstract description 37
- SECXISVLQFMRJM-UHFFFAOYSA-N NMP Substances CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 claims abstract description 273
- BAVYZALUXZFZLV-UHFFFAOYSA-N Methylamine Chemical compound NC BAVYZALUXZFZLV-UHFFFAOYSA-N 0.000 claims abstract description 202
- 238000007670 refining Methods 0.000 claims abstract description 165
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 86
- 239000012535 impurity Substances 0.000 claims abstract description 46
- 238000012432 intermediate storage Methods 0.000 claims abstract description 25
- 238000000746 purification Methods 0.000 claims abstract description 17
- 238000011084 recovery Methods 0.000 claims description 139
- 239000000047 product Substances 0.000 claims description 35
- 230000009471 action Effects 0.000 claims description 31
- 238000010438 heat treatment Methods 0.000 claims description 27
- 239000000463 material Substances 0.000 claims description 24
- 238000009833 condensation Methods 0.000 claims description 4
- 230000005494 condensation Effects 0.000 claims description 4
- 230000009286 beneficial effect Effects 0.000 abstract description 2
- 238000010521 absorption reaction Methods 0.000 description 44
- 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
- 238000006481 deamination reaction Methods 0.000 description 22
- 238000000926 separation method Methods 0.000 description 21
- 230000009615 deamination Effects 0.000 description 19
- 238000010586 diagram Methods 0.000 description 14
- LFETXMWECUPHJA-UHFFFAOYSA-N methanamine;hydrate Chemical compound O.NC LFETXMWECUPHJA-UHFFFAOYSA-N 0.000 description 14
- 238000004519 manufacturing process Methods 0.000 description 12
- 239000001257 hydrogen Substances 0.000 description 5
- 229910052739 hydrogen Inorganic materials 0.000 description 5
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 4
- WERYXYBDKMZEQL-UHFFFAOYSA-N butane-1,4-diol Chemical compound OCCCCO WERYXYBDKMZEQL-UHFFFAOYSA-N 0.000 description 4
- 238000005554 pickling Methods 0.000 description 3
- 239000002994 raw material Substances 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
- 239000007789 gas Substances 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 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
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 150000001993 dienes Chemical class 0.000 description 1
- 229920006351 engineering plastic Polymers 0.000 description 1
- 125000002534 ethynyl group Chemical group [H]C#C* 0.000 description 1
- 238000002309 gasification Methods 0.000 description 1
- 230000006872 improvement Effects 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
- JRZJOMJEPLMPRA-UHFFFAOYSA-N olefin Natural products CCCCCCCC=C JRZJOMJEPLMPRA-UHFFFAOYSA-N 0.000 description 1
- 229920002120 photoresistant polymer Polymers 0.000 description 1
- 239000002798 polar solvent Substances 0.000 description 1
- 229920002981 polyvinylidene fluoride Polymers 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
Classifications
-
- 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 in particular relates to a device for improving the purity of an NMP crude product after demethanization, wherein the NMP crude product after demethanization comprises NMP, water and impurities, the device comprises an NMP purification unit, the NMP purification unit comprises an NMP light-off section, an NMP refining section and an electronic-grade NMP intermediate storage section, and the NMP light-off section, the NMP refining section and the electronic-grade NMP intermediate storage section are sequentially connected; after the NMP crude product is treated by an NMP light removal section, NMP, water and heavier impurities enter an NMP refining section, and after the NMP crude product is treated by the NMP refining section, NMP enters an electronic-grade NMP intermediate storage section. The invention has the beneficial effects that the NMP crude product (NMP, water and impurities) after the methylamine removal is treated by sequentially passing through an NMP light removal section and an NMP refining section, and enters an electronic grade NMP intermediate tank, and NMP in the electronic grade NMP intermediate tank is detected, wherein the methylamine content is less than or equal to 5ppm, the moisture content is less than or equal to 0.02%, the pH is between 7 and 9, the chromaticity is less than or equal to 10, and the requirements of the electronic grade NMP are completely met.
Description
Technical Field
The invention belongs to the technical field of NMP purification, and particularly relates to a device for improving the purity of an NMP crude product after demethanization.
Background
N-methyl pyrrolidone (NMP) is a polar solvent and 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, aromatic hydrocarbon and the like, 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.
At present, N-methyl pyrrolidone is mainly classified into a common grade, an industrial grade and an electronic grade, wherein the purity of the N-methyl pyrrolidone is required to be 99.5%, 99.8% and 99.9% respectively, the electronic grade also requires that the methylamine content in the product is less than or equal to 5ppm, the moisture content is less than or equal to 0.02%, the pH is between 7 and 9, and the chromaticity is less than or equal to 10.
In the prior art, when the N-methyl pyrrolidone product prepared by the conventional method is purified, the content of alkaline impurities such as methylamine and the like after purification is difficult to be reduced to below 5ppm, and the requirement of electronic grade products is difficult to be met.
Disclosure of Invention
In order to solve the problems, the invention provides a device for improving the purity of the crude NMP product after the methylamine removal, which can reduce the content of alkaline impurities in NMP to below 5ppm and meet the requirements of electronic grade products.
The invention provides the following technical scheme:
The device comprises an NMP purification unit, wherein the NMP purification unit comprises an NMP light removal section, an NMP refining section and an electronic grade NMP intermediate storage section, and the NMP light removal section, the NMP refining section and the electronic grade NMP intermediate storage section are sequentially connected;
After the NMP crude product is treated by an NMP light removal section, NMP, water and heavier impurities enter an NMP refining section, and after the NMP crude product is treated by the NMP refining section, NMP enters an electronic-grade NMP intermediate storage section.
Preferably, the NMP light component removing section comprises a light component removing tower, a light component removing tower top condenser, a light component removing tower top condensate tank, a light component removing tower vacuum condenser, a light component removing tower vacuum tank and a light component removing tower reboiler;
The device comprises a light component removing tower top condenser, a light component removing tower top condensate tank, a light component removing tower vacuum condenser and a light component removing tower vacuum tank, wherein an inlet of the light component removing tower top condenser is connected with a light component removing tower top, the middle part of the light component removing tower is used for receiving a crude NMP product after the methylamine is removed, a light component removing tower reboiler is connected with the light component removing tower and is used for heating materials which enter the light component removing tower, including NMP, water and impurities, light components and light components are separated after heating, the light components including water, NMP and lighter impurities are extracted from the light component removing tower top, condensed by the light component removing tower top condenser and flow into the light component removing tower top condensate tank, water and lighter impurities flow out from the top of the light component removing tower top condensate tank and flow out from the bottom of the light component removing tower vacuum condenser, and finally flow out from the bottom of the light component removing tower top condensate tank and enter an NMP recovery tower under the action of a light component removing tower pump; the heavy components including NMP, heavier impurities and water flow out from the bottom of the light component removal tower, and under the action of the light component removal tower bottom pump, the NMP, the heavier impurities and the water enter a refining tower in the NMP refining section.
Preferably, the NMP refining section comprises a refining tower, a refining tower top condenser, a refining tower top condensate tank, a refining tower vacuum condenser, a refining tower vacuum tank and a refining tower reboiler;
The device comprises a refining tower top condenser, a refining tower top condensate tank, a refining tower vacuum condenser and a refining tower vacuum tank, wherein an inlet of the refining tower top condenser is connected with the top of the refining tower, the middle part of the refining tower is connected with a light removal tower, light removal materials including NMP, impurities and water are sent into the refining tower under the action of a light removal tower bottom pump, a refining tower reboiler is connected with the refining tower and is used for heating the materials entering the refining tower, light and heavy components are separated after heating, light components including NMP and water are extracted from the refining tower top, condensed by the refining tower top condenser and flow into the refining tower top condensate tank, water flows out from the top of the refining tower top condensate tank and enters the refining tower vacuum condenser, finally enters the refining tower vacuum tank, NMP and water flow out from the bottom of the refining tower top condensate tank, a part of NMP enters a finished product cooler in an electronic grade intermediate storage section under the action of the refining tower top pump, and another part of NMP and water enters a crude product intermediate tank in the refining section under the action of the NMP tower bottom pump, and heavy components including impurities flow out from the bottom of the refining tower, NMP and NMP enters the NMP under the action of the NMP bottom of the refining tower bottom pump.
Preferably, the electronic grade NMP intermediate storage section comprises an electronic grade NMP intermediate tank, an NMP finished product cooler, an NMP finished product pump and an NMP crude product intermediate tank;
The outlet of the NMP finished product cooler is connected with the electronic-grade NMP intermediate tank, the inlet of the NMP finished product cooler is connected with the refined tower top condensate tank to receive NMP, and the NMP entering the electronic-grade NMP intermediate tank enters the electronic-grade NMP main pipe under the action of the NMP finished product pump;
the NMP crude product intermediate tank is provided with a plurality of inlets which are respectively connected with the light component removal tower and the refined tower top condensate tank and are used for receiving NMP and water.
The beneficial effects of the invention are as follows:
The purification device mainly comprises an NMP light removal section and an NMP refining section;
The NMP light component removing section comprises a light component removing tower, materials (NMP, water and impurities) in the light component removing tower are heated, light and heavy components are separated after heating, light components (water, NMP and lighter impurities) are extracted from the top of the light component removing tower, condensed by a condenser at the top of the light component removing tower and then flow into a condensate tank at the top of the light component removing tower, water and lighter impurities flow out from the top of the condensate tank at the top of the light component removing tower and then enter a vacuum condenser of the light component removing tower, finally enter a vacuum tank of the light component removing tower, water and NMP flow out from the bottom of the condensate tank at the top of the light component removing tower and enter an NMP recovery tower under the action of a pump at the top of the light component removing tower; the heavy components (NMP, heavier impurities and water) flow out from the bottom of the light component removal tower, and under the action of a light component removal tower bottom pump, the NMP, the heavier impurities and the water enter a refining tower in the NMP refining section;
The NMP refining section comprises a refining tower, materials (NMP, water and heavier impurities) in the refining tower are heated, light and heavy components are separated after heating, the light components comprising NMP and water are extracted from the refining tower, condensed by a condenser at the refining tower top and then flow into a condensate tank at the refining tower top, water flows out from the top of the condensate tank at the refining tower top and then enters a vacuum condenser at the refining tower, finally enters a vacuum tank at the refining tower, NMP and water flow out from the bottom of the condensate tank at the refining tower, under the action of a pump at the refining tower top, one part of NMP enters an NMP finished product cooler in an electronic grade NMP intermediate storage section, the other part of NMP and water enter an NMP crude product intermediate tank in the NMP refining section, and heavy components (impurities) flow out from the bottom of the refining tower and enter a tar tower under the action of the pump at the refining tower bottom;
After the methylamine is removed, NMP crude products (NMP, water and impurities) are sequentially treated by an NMP light removing section and an NMP refining section, and then enter an electronic-grade NMP intermediate tank, NMP in the electronic-grade NMP intermediate tank is detected, wherein the methylamine content is less than or equal to 5ppm, the moisture content is less than or equal to 0.02%, the pH is between 7 and 9, the chromaticity is less than or equal to 10, and the requirements of the electronic-grade NMP are completely met.
Drawings
FIG. 1 is a GBL synthesis section diagram;
FIG. 2 is a diagram of NMP synthesis section;
FIG. 3 is a diagram of a methylamine separation section;
FIG. 4 is a diagram of a methylamine recovery section;
FIG. 5 is a diagram of an intermediate storage section for recovering methylamine;
FIG. 6 is a diagram of NMP light ends section;
FIG. 7 is a diagram of NMP purification section;
FIG. 8 is a diagram of an electronic grade NMP intermediate storage section;
FIG. 9 is a diagram of a light section for NMP recovery;
FIG. 10 is a diagram of a purification section for NMP recovery;
FIG. 11 is a tar processing section diagram;
FIG. 12 is a diagram of NMP recovery section;
FIG. 13 is a diagram of a dehydration section for NMP recovery;
FIG. 14 is a diagram of an intermediate storage section for technical grade NMP.
The meaning of the symbols in the drawings is as follows:
10-GBL production unit 11-BDO middle 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 overhead tank 22-methylamine water overhead tank 23-NMP reactor 24-methylamine overhead tank
30-Methylamine recovery unit 31-methylamine separation section 311-flash tank 312-deamination tower 314-deamination tower top condenser 315-deamination tower reboiler 316-methylamine separation tower 317-methylamine separation tower top primary condenser 318-methylamine separation tower top secondary 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 recycle cooler 325-methylamine secondary absorption recycle cooler 326-methylamine tertiary absorption recycle cooler 327-methylamine pickling tank
33-Recovered methylamine intermediate storage section 331-recovered methylamine water intermediate tank 332-recovered methylamine water pump
40-NMP purification unit 41-NMP light ends section 411-light ends column 412-light ends column top condenser 413-light ends column top condensate tank 414-light ends column vacuum condenser 415-light ends column vacuum tank 416-light ends column 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 light ends section 511-NMP recovery light ends column 512-light ends recovery top condenser 513-light ends recovery top condensate tank 514-light ends recovery vacuum condenser 515-light ends recovery vacuum tank 516-light ends recovery 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 tower 532-NMP recovery tower condenser 533-NMP recovery tower vacuum tank 534-NMP recovery tower reboiler 535-recovery dehydration tower 536-recovery dehydration tower preheater 537-recovery dehydration tower condenser 538-recovery dehydration tower condensate tank 539-recovery dehydration tower vacuum tank 5391-recovery dehydration tower reboiler
54-Tar treatment section 541-tar tower 542-tar tower top condenser 543-tar tower vacuum tank 544-tar tower reboiler
55-Industrial grade NMP intermediate storage section 551-Industrial grade NMP intermediate tank 552-recovered NMP finished product cooler 553-Industrial grade NMP finished product pump
Detailed Description
The present invention will be specifically described with reference to the following examples.
BDO is 1, 4-butanediol, GBL is gamma-butyrolactone, NMP is N-methylpyrrolidone
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. In the following description it will be given in order,
1. GBL production unit
The GBL production unit 10 comprises a BDO middle 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 of the BDO middle tank 11 under the action of the BDO raw material pump 12, and sequentially enters the BDO vaporizer 13 and the BDO heater 14 for heating and gasification; then enters a GBL reactor 15 for reaction, the mixed gas of the gamma-butyrolactone (GBL) crude product and hydrogen is generated, the mixed gas is subjected to heat exchange through a GBL heat exchanger 16, then enters a GBL condenser 17 for condensation, the hydrogen is sent to a hydrogen buffer tank 18 after condensation, and the gamma-butyrolactone crude product is sent to the GBL buffer tank 19.
2. NMP production unit
The NMP production unit 20 comprises a GBL overhead tank 21, a methylamine water overhead tank 22, an NMP reactor 23 and a 24-methylamine overhead 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.
3. 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 tank 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 recycle cooler 324, a methylamine secondary absorption recycle cooler 325, a methylamine tertiary absorption recycle cooler 326 and a methylamine pickling tank 327;
the recovered methylamine intermediate storage section 33 comprises a recovered methylamine water intermediate tank 331 and a recovered methylamine water pump 332;
The top of the deamination tower 312 is provided with a deamination tower top condenser 313, the bottom of the deamination tower 312 is provided with a deamination 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 mutually communicated, 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 through a methylamine removal water pump;
The inlet of the flash tank 311 is communicated with the NMP reactor 23 of the NMP production unit 20 so that NMP crude products (NMP, methylamine, water and impurities) enter the flash tank 311, the outlet of the flash tank 311 is connected with the inlet of the middle part of the deamination tower 312, the deamination tower reboiler 314 is connected with the deamination tower 312 and is used for heating the NMP crude products entering the deamination tower 312, light and heavy components are separated after heating, light components (methylamine and water) are gasified and enter the deamination tower top condenser 314, the deamination tower top condenser 314 is provided with two outlets, the outlet I is communicated with the methylamine separation tower 316 so that methylamine and water enter the methylamine separation tower 316, and the outlet II is communicated with the methylamine secondary absorption tower 322 so that methylamine enters the methylamine secondary absorption tower 322; heavy components (NMP, impurities, water) are withdrawn from the bottom of the deamination column 312, one part is fed to the light component removal column 411 in the NMP purification unit 40, and the other part is fed to the recovery light component removal column 511 in the NMP recovery unit 50.
The methylamine separating tower reboiler 319 is connected with the methylamine separating tower 316 and is used for heating materials (methylamine and water) entering the methylamine separating tower 316, separating light components and heavy components after heating, gasifying the light components (a large amount of methylamine and a small amount of water), sequentially entering the first-stage condenser 317 at the top of the methylamine separating tower and the second-stage condenser 318 at the top of the methylamine separating tower, then entering the first-stage absorption tower 321 of the methylamine, extracting the heavy components (a small amount of methylamine and a large amount of water) from the bottom of the methylamine separating tower 316, pumping the methylamine into the third-stage absorption tower 323 of the methylamine after the methylamine is dehydrated, and collecting and then carrying out centralized treatment;
The methylamine recovery section 32 further comprises a methylamine primary absorption recycle cooler 324 which forms a recycle loop with the methylamine primary absorption tower 321; the methylamine primary absorption tower 321 is communicated with the methylamine secondary absorption tower 322, and the methylamine primary absorption recycle cooler 324 is communicated with the methylamine water recovery middle tank 331;
The methylamine recovery section 32 further comprises a methylamine secondary absorption recycle cooler 325 which forms a recycle loop with the methylamine secondary absorption tower 322; the methylamine secondary absorption tower 322 is communicated with the methylamine tertiary absorption tower 323, and the methylamine secondary absorption recycle cooler 325 is connected with the methylamine primary absorption tower 321;
The methylamine recovery section 32 further comprises a methylamine tertiary absorption recycle cooler 326 which forms a recycle loop with the methylamine tertiary absorption tower 323; the methylamine tertiary absorption tower 323 is communicated with a methylamine pickling tank 327, and the methylamine tertiary absorption recycle 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 the methylamine primary absorption recycle cooler 324, and flow into the methylamine water recovery intermediate tank 331, and the high-purity methylamine flows into the methylamine secondary absorption tower 322; the high-purity methylamine is further dehydrated in a methylamine secondary absorption circulation cooler 325, and then flows into a methylamine tertiary absorption tower 323, methylamine and water condensed in the methylamine secondary absorption circulation cooler 325 flow back to a methylamine primary absorption tower 321, and methylamine and water condensed in the methylamine tertiary absorption circulation cooler 326 flow back to the methylamine secondary absorption tower 322;
At least two inlets are arranged on the intermediate tank 331 for recovering the methylamine water, wherein the first inlet is connected with the high-level tank 22 of the methylamine water of the NMP production unit 20, the second inlet is communicated with the first-stage absorption and circulation cooler 324 of the methylamine, and the outlet on the intermediate tank 331 for recovering the methylamine water is connected with the high-level tank 22 of the methylamine water of the NMP production unit 20 to form a circulation loop.
4. NMP purification unit
The NMP purification unit 40 comprises an NMP light-off section 41, an NMP refining section 42 and an electronic grade NMP intermediate storage section 43;
The NMP light component 41 comprises a light component 411, a light component tower top condenser 412, a light component tower top condensate tank 413, a light component tower vacuum condenser 414, a light component tower vacuum tank 415 and a light component tower reboiler 416;
the NMP refining section 42 includes a refining column 421, a refining column top condenser 422, a refining column top condensate tank 423, a refining column vacuum condenser 424, a refining column vacuum tank 425, and a refining column 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 light component removing tower condenser 412, the light component removing tower condensate tank 413, the light component removing tower vacuum condenser 414 and the light component removing tower vacuum tank 415 are sequentially connected, an inlet of the light component removing tower condenser 412 is connected with the top of the light component removing tower 411, the middle part of the light component removing tower 411 is connected with the deamination tower 312, the NMP crude product (NMP, water and impurities) after methylamine removal is sent into the light component removing tower 411 under the action of the deamination tower pump, the light component removing tower reboiler 416 is connected with the light component removing tower 411 and is used for heating materials (NMP, water and impurities) entering the light component removing tower 411, light components (water, NMP and lighter impurities) are extracted from the top of the light component removing tower 411, condensed by the light component removing tower condenser 412 and then flow into the light component removing tower condensate tank 413, water and lighter impurities flow out from the top of the light component removing tower condensate tank 413 and finally flow into the light component removing tower vacuum condenser 415, water and NMP flow out from the bottom of the light component removing tower 411 and flow into the NMP recycling tower 531 of the NMP unit 50 under the action of the light component removing tower top pump; heavy components (NMP, heavier impurities and water) flow out from the bottom of the light component removal tower 411, one part (NMP, heavier impurities and water) enters the refining tower 421 under the action of a pump at the bottom of the light component removal tower, and the other part (NMP and water) enters the 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, an 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 light removal tower 411, the light removal materials (NMP, heavier impurities and water) are sent into the refining tower 421 under the action of the light removal tower bottom pump, the 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, the light and heavy components after heating are separated, the light components (NMP and water) are collected from the top of the refining tower 421, condensed by the refining tower top condenser 422 and flow into the refining tower top condensate tank 423, the water flows out from the top of the refining tower top condensate tank 423 and enters the refining tower vacuum condenser 411, finally enters the refining tower vacuum tank 425, NMP and water flow out from the bottom of the refining tower top condensate tank 423, one part (NMP and water) enters the NMP cooler 432, the other part (NMP and water) enters the NMP and the heavy impurities (NMP and water) enter the refining tower bottom unit 541 under the action of the refining tower bottom pump 50;
the outlet of the NMP finished product cooler 432 is connected with an electronic grade NMP intermediate tank 431, the inlet of the NMP finished product cooler 432 is connected with a refined tower top condensate tank 432 to receive NMP, the electronic grade NMP intermediate tank 431 is provided with an inlet connected with a recovered finished product NMP cooler 552 in a recovered NMP unit 50 to receive NMP, and the NMP entering the electronic grade NMP intermediate tank 431 enters an electronic grade NMP main pipe under the action of an 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 light component removal tower 411, a refined tower top condensate tank 423, a recovery light component removal tower 511 and a recovery refined tower top condensate tank 523 and are used for receiving NMP and water, and the outlet of the NMP crude product intermediate tank 434 is connected with a recovery dehydration tower preheater 536.
5. NMP recovery unit
The recovered NMP unit 50 comprises a recovered NMP light-off section 51, a recovered NMP refining section 52, an NMP recovery section 53, a tar treatment section 54 and an industrial-grade NMP intermediate storage section 55;
the recovered NMP light component 51 comprises a recovered light component tower 511, a recovered light component tower top condenser 512, a recovered light component tower top condensate tank 513, a recovered light component tower vacuum condenser 514, a recovered light component tower vacuum tank 515 and a recovered light component tower reboiler 516;
The recovered NMP refining section 52 comprises a recovered refining column 521, a recovered refining column top condenser 522, a recovered refining column top condensate tank 523, a recovered refining column vacuum condenser 524, a recovered refining column vacuum tank 525 and a recovered refining column 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 processing 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 NMP intermediate storage section 55 comprises an industrial NMP intermediate tank 551, a recovered NMP finished product cooler 552 and an industrial NMP finished product pump 553;
The recovery light removal tower top condenser 512, the recovery light removal tower top condensate tank 513, the recovery light removal tower vacuum condenser 514 and the recovery light removal tower vacuum tank 515 are sequentially connected, an inlet of the recovery light removal tower top condenser 512 is connected with the top of the recovery light removal tower 511, the middle part of the recovery light removal tower 511 is connected with the deamination tower 312, materials (NMP, water and impurities) are sent into the recovery light removal tower 511 under the action of a deamination tower pump, the recovery light removal tower reboiler 526 is connected with the recovery light removal tower 511 and is used for heating materials (NMP, water and impurities) entering the recovery light removal tower 511, light and heavy components are separated after heating, light components (water, NMP and lighter impurities) are extracted from the top of the recovery light removal tower 511, condensed by the recovery light removal tower condenser 512 and enter the recovery light removal tower top condensate tank 513, water and lighter impurities flow out of the top of the recovery light removal tower top condensate tank 513, enter the recovery light removal tower vacuum tank 514 and finally enter the recovery light removal tower vacuum tank 515 under the action of NMP top 514; the heavy components (NMP, heavier impurities and water) flow out from the bottom of the recovery light-removal tower 511, one part (NMP, heavier impurities and water) enters the recovery refining tower 521 under the action of the recovery light-removal tower bottom pump, and the other part (NMP and water) enters the 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, the 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 light removal tower 511, the light removal materials (NMP, heavier impurities and water) are sent into the recovery refining tower 521 under the action of the recovery light removal tower bottom pump, the recovery refining tower reboiler 526 is connected with the recovery refining tower 521 and is used for heating the materials (NMP, heavier impurities and water) entering the recovery refining tower 521, the heated light and heavy components are separated, the light components (NMP and water) are extracted from the top of the recovery refining tower 521, the light components flow into the recovery refining tower top condensate tank 523 after being condensed by the recovery refining tower top condenser 522, the water flows out from the top of the recovery refining tower condensate tank 524, finally flows into the recovery refining tower vacuum tank 525, NMP and water flows out from the bottom of the recovery refining tower condensate tank 523 under the action of the recovery refining tower top pump, one part (NMP) enters the NMP cooling device 552 and the other part enters the middle part of the recovery refined tower 521, and the heavy components enter the recovery tower 541 under the action of the recovery refined tower bottom 521;
the top of the NMP recovery tower 531, the NMP recovery tower top condenser 532 and the NMP recovery tower vacuum tank 533 are sequentially connected, the middle part of the NMP recovery tower 531 is respectively connected with the light component removing tower 411 and the recovery light component removing tower 511, materials (NMP and water) are sent into the NMP recovery tower 531 under the action of a light component removing tower top pump and a recovery light component removing tower top pump, the NMP recovery tower reboiler 534 is connected with the NMP recovery tower 531 and is used for heating the materials (NMP and water) entering the NMP recovery tower 531, light components and heavy components are separated after heating, light components (water) are extracted from the top of the NMP recovery tower 531, the light components are cooled by the NMP recovery tower top condenser 532 and then flow into the NMP recovery tower vacuum tank 533, and the heavy components (NMP) enter the NMP crude intermediate tank 434 under the action of the NMP recovery tower bottom pump;
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 is used for heating the materials (tar, NMP and water) entering the tar tower 541, light components and heavy components are separated after heating, light components (water) are extracted from the top of the tar tower 541, cooled by a tar tower top condenser 542 and then flow into a tar tower vacuum tank 543, light components (NMP and water) are extracted from the side line of the tar tower 541 and enter an NMP crude intermediate tank 434;
The industrial NMP intermediate tank 551 is provided with two inlets, 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 dehydrating 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 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 column 535, a recovery dehydration column preheater 536, a recovery dehydration column overhead condenser 537, a recovery dehydration column overhead condensate tank 538, a recovery dehydration column vacuum tank 539, and a recovery dehydration column 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 the 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 materials (NMP and water) entering the recovery dehydration tower 535, light and heavy components are separated after heating, light phases (water) are extracted from the top of the recovery dehydration tower 535, cooled by the recovery dehydration tower top condenser 537 and then flow into the recovery dehydration tower top condensate tank 538 and finally enter the recovery dehydration tower vacuum tank 539, and heavy components (NMP) are extracted from the bottom of the recovery dehydration tower 535 and enter the industrial NMP intermediate tank 551.
The foregoing description is only a preferred embodiment of the present invention, and the present invention is not limited thereto, but it is to be understood that modifications and equivalents of some of the technical features described in the foregoing embodiments may be made by those skilled in the art, although the present invention has been described in detail with reference to the foregoing embodiments. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (1)
1. The device for improving the purity of the NMP crude product after the demethanization is characterized by comprising an NMP purification unit (40), wherein the NMP purification unit (40) comprises an NMP light-off section (41), an NMP refining section (42) and an electronic-grade NMP intermediate storage section (43), and the NMP light-off section (41), the NMP refining section (42) and the electronic-grade NMP intermediate storage section (43) are sequentially connected;
after the NMP crude product is subjected to NMP light removal working section (41), NMP, water and heavier impurities enter NMP refining working section (42), after the NMP crude product is subjected to NMP refining working section (42), NMP enters electronic grade NMP intermediate storage working section (43);
The NMP light component removing section (41) comprises a light component removing tower (411), a light component removing tower top condenser (412), a light component removing tower top condensate tank (413), a light component removing tower vacuum condenser (414), a light component removing tower vacuum tank (415) and a light component removing tower reboiler (416);
The device comprises a light component removing tower top condenser (412), a light component removing tower top condensate tank (413), a light component removing tower vacuum condenser (414) and a light component removing tower vacuum tank (415), wherein an inlet of the light component removing tower top condenser (412) is connected with the top of the light component removing tower (411), an NMP crude product after methylamine removal is received in the middle of the light component removing tower (411), the light component removing tower reboiler (416) is connected with the light component removing tower (411) and is used for heating materials comprising NMP, water and impurities, separating light components and heavy components after heating, the light components comprising water, NMP and lighter impurities are extracted from the top of the light component removing tower (411), flow into the light component removing tower top condensate tank (413) after condensation of the light component removing tower top condenser (412), flow out of the top of the light component removing tower top condensate tank (413) and finally flow into the light component removing tower vacuum tank (415), and flow out of the top of the light component removing tower (413) and act on NMP to enter a recovery tower (531); the heavy components including NMP, heavier impurities and water flow out from the bottom of the light component removal tower (411), and under the action of a light component removal tower bottom pump, the NMP, the heavier impurities and the water enter a refining tower (421) in an NMP refining section (42);
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 refining tower condenser (422), the refining tower condensate tank (423), the refining tower vacuum condenser (424) and the refining tower vacuum tank (425) are sequentially connected, an inlet of the refining tower condenser (422) is connected with the top of the refining tower (421), the middle part of the refining tower (421) is connected with the light removal tower (411), the light removal materials including NMP and heavier impurities and water are sent into the refining tower (421) under the action of a light removal tower bottom pump, a refining tower reboiler (426) is connected with the refining tower (422) and used for heating the materials entering the refining tower, light and heavy components are separated after heating, light components including NMP and water are extracted from the top of the refining tower (421), flow into the refining tower condensate tank (423) after condensation of the refining tower condenser (422), flow out of the top of the refining tower condensate tank (423), flow into the refining tower vacuum condenser (424), finally flow into the refining tower vacuum tank (425), NMP and water flow out of the bottom of the refining tower condensate tank (423), NMP and NMP flow out of the bottom of the refining tower condensate tank (43), NMP and NMP flow out of the middle part of the refining tower condensate pump (43) enter the middle part of the NMP and enter the middle part of the NMP (43) and flow out of the middle part of the NMP pump;
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 outlet of the NMP finished product cooler (432) is connected with an electronic-grade NMP intermediate tank (431), the inlet of the NMP finished product cooler (432) is connected with a refined tower top condensate tank (423) to receive NMP, and NMP entering the electronic-grade NMP intermediate tank (431) enters an electronic-grade NMP main pipe under the action of an NMP finished product pump (433);
the NMP crude product intermediate tank (434) is provided with a plurality of inlets which are respectively connected with the light component removing tower (411) and the refined tower top condensate tank (423) and are used for receiving NMP and water.
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| CN113185441A (en) * | 2021-04-26 | 2021-07-30 | 宁波南大光电材料有限公司 | Purification method for reducing chroma of N-methyl pyrrolidone |
| CN114452669B (en) * | 2022-03-30 | 2023-05-19 | 派尔森环保科技有限公司 | Reclaimed material liquid rectifying and purifying system containing NMP |
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