CN220237804U - Crystallization vacuum operation system for producing ammonium sulfate from caprolactam - Google Patents
Crystallization vacuum operation system for producing ammonium sulfate from caprolactam Download PDFInfo
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- CN220237804U CN220237804U CN202321598650.1U CN202321598650U CN220237804U CN 220237804 U CN220237804 U CN 220237804U CN 202321598650 U CN202321598650 U CN 202321598650U CN 220237804 U CN220237804 U CN 220237804U
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- condenser
- ammonium sulfate
- unit
- dry
- vacuum
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- JBKVHLHDHHXQEQ-UHFFFAOYSA-N epsilon-caprolactam Chemical compound O=C1CCCCCN1 JBKVHLHDHHXQEQ-UHFFFAOYSA-N 0.000 title claims abstract description 30
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 title claims abstract description 24
- 229910052921 ammonium sulfate Inorganic materials 0.000 title claims abstract description 23
- 235000011130 ammonium sulphate Nutrition 0.000 title claims abstract description 23
- 238000002425 crystallisation Methods 0.000 title claims abstract description 9
- 230000008025 crystallization Effects 0.000 title claims abstract description 9
- 238000010793 Steam injection (oil industry) Methods 0.000 claims abstract description 10
- 239000012074 organic phase Substances 0.000 claims abstract description 5
- 238000011084 recovery Methods 0.000 claims abstract description 5
- 239000012071 phase Substances 0.000 claims description 6
- 229910001220 stainless steel Inorganic materials 0.000 claims description 4
- 239000010935 stainless steel Substances 0.000 claims description 4
- 239000013078 crystal Substances 0.000 claims description 3
- 239000007788 liquid Substances 0.000 claims description 3
- 238000000926 separation method Methods 0.000 claims description 3
- 239000000498 cooling water Substances 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 abstract description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 8
- 239000010865 sewage Substances 0.000 description 4
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- 210000000078 claw Anatomy 0.000 description 3
- 239000002826 coolant Substances 0.000 description 3
- 238000005265 energy consumption Methods 0.000 description 3
- 238000000034 method Methods 0.000 description 3
- 238000006386 neutralization reaction Methods 0.000 description 3
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 description 2
- HIGZEFHDFAMPND-UHFFFAOYSA-N azepan-2-one;sulfuric acid Chemical compound OS(O)(=O)=O.O=C1CCCCCN1 HIGZEFHDFAMPND-UHFFFAOYSA-N 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- VEZUQRBDRNJBJY-UHFFFAOYSA-N cyclohexanone oxime Chemical compound ON=C1CCCCC1 VEZUQRBDRNJBJY-UHFFFAOYSA-N 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 238000005192 partition Methods 0.000 description 2
- 238000006462 rearrangement reaction Methods 0.000 description 2
- 230000001105 regulatory effect Effects 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 1
- 229920002292 Nylon 6 Polymers 0.000 description 1
- AWSFEOSAIZJXLG-UHFFFAOYSA-N azepan-2-one;hydrate Chemical compound O.O=C1CCCCCN1 AWSFEOSAIZJXLG-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- ARJOQPDZEFWMDY-UHFFFAOYSA-N cyclohexane;n-cyclohexylidenehydroxylamine Chemical compound C1CCCCC1.ON=C1CCCCC1 ARJOQPDZEFWMDY-UHFFFAOYSA-N 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 229920006351 engineering plastic Polymers 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- HIFJUMGIHIZEPX-UHFFFAOYSA-N sulfuric acid;sulfur trioxide Chemical compound O=S(=O)=O.OS(O)(=O)=O HIFJUMGIHIZEPX-UHFFFAOYSA-N 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
Abstract
The utility model provides a be used for caprolactam production ammonium sulfate crystallization vacuum operating system, including the ammonium sulfate crystallizer, the ammonium sulfate crystallizer passes through the pipeline and communicates with first order condenser and second grade condenser in proper order, the second grade condenser passes through pipeline and steam injection unit and dry-type vacuum unit intercommunication, steam injection unit passes through pipeline intercommunication steam system, dry-type vacuum unit top is through pipeline intercommunication tail gas recovery system, steam injection unit, dry-type vacuum unit, first order condenser and second grade condenser bottom all communicate with the condensate collecting vat, the inside baffle that sets up of condensate collecting vat, the baffle separates into left and right two cavities with the condensate collecting vat, two cavity tops communicate each other, two cavities communicate with condensate delivery pump and organic phase delivery pump respectively.
Description
Technical Field
The utility model belongs to the technical field of vacuum process utilization, and particularly relates to a vacuum operation system for producing ammonium sulfate crystals by caprolactam.
Background
Caprolactam is an important raw material for producing nylon-6, engineering plastics, films and other chemical products, and a caprolactam production chain belongs to the category of high energy consumption, high pollution and high investment, and along with the tightening of national policies on enterprises of high energy consumption, high pollution and high investment, a series of technical improvements aim to continuously reduce the production material consumption and the energy consumption and reduce the emission of pollutants.
In the caprolactam production, the rearrangement reaction process is that a cyclohexane-cyclohexanone oxime solution of 20 percent of cyclohexanone oxime reacts under the catalysis of fuming sulfuric acid to generate caprolactam sulfate, the caprolactam sulfate reacts with ammonia gas in a saturated ammonium sulfate system to generate caprolactam and ammonium sulfate, the reaction is carried out under the conditions of vacuum degree of 80-90KPa and temperature of 60-70 ℃, and the ammonium sulfate crystals are generated by evaporating, concentrating and crystallizing through acid-base neutralization reaction heat, so that the solid-liquid layering is formed to achieve the separation effect.
In the crystallization reactor, the neutralization reaction provides a heat source, a large amount of gas phase is pumped away when the neutralization reaction is carried out under the vacuum degree of 80-90KPa, cyclohexane which is not completely vaporized exists in the rearrangement reaction and is brought into the crystallizer reaction, a caprolactam water solution containing a small amount of benzene is recycled, the pressure fluctuation of the crystallizer is large, the adjustment is difficult, a steam jet pump is adopted, a large amount of water enters the system and is finally discharged to a sewage system, so that the consumption is high, and the sewage treatment cost is increased.
Disclosure of Invention
The utility model solves the technical problems of large pressure fluctuation of a crystallizer, difficult regulation, high consumption and increased sewage treatment cost.
In order to solve the problems, the technical scheme of the utility model is as follows:
the utility model provides a be used for caprolactam production ammonium sulfate crystallization vacuum operating system, including the ammonium sulfate crystallizer, the ammonium sulfate crystallizer passes through the pipeline and communicates with first order condenser and second grade condenser in proper order, the second grade condenser passes through pipeline and steam injection unit and dry-type vacuum unit intercommunication, steam injection unit passes through pipeline intercommunication steam system, dry-type vacuum unit top is through pipeline intercommunication tail gas recovery system, steam injection unit, dry-type vacuum unit, first order condenser and second grade condenser bottom all communicate with the condensate collecting vat, the inside baffle that sets up of condensate collecting vat, the baffle separates into left and right two cavities with the condensate collecting vat, two cavity tops communicate each other, two cavities communicate with condensate delivery pump and organic phase delivery pump respectively.
The utility model has the beneficial effects that:
1. the steam flow of the steam jet unit and the circulating water flow of the condenser are automatically regulated, and the dry vacuum pump is automatically regulated according to the pressure of the crystallizer by adopting variable frequency regulation, so that the pressure stability of the crystallizer is maintained.
2. The crystallizer gas-phase primary condenser and the crystallizer gas-phase secondary condenser adopt high-efficiency heat exchangers, so that the equipment size is reduced, the heat exchange efficiency is improved, the consumption of cooling medium is reduced, and the occupied area is reduced.
3. The steam injection system is used as a standby, and once the dry vacuum pump is damaged and used in an emergency, the loss caused by long-time stopping of the system can be avoided.
4. The dry vacuum pump is adopted, steam is not consumed, the consumption reduction effect is achieved, and the sewage treatment cost is avoided.
5. The tail gas of the steam jet unit and the dry vacuum unit is discharged to a tail gas treatment system, so that the environment is improved, and the aim of environmental protection is fulfilled.
Drawings
The utility model is further illustrated by the following examples in conjunction with the accompanying drawings:
FIG. 1 is a schematic diagram of the present utility model.
In the figure: the device comprises an ammonium sulfate crystallizer 1, a primary condenser 2, a secondary condenser 3, a steam jet unit 4, a dry vacuum unit 5, a condensate collecting tank 6, an organic phase conveying pump 7, a condensate conveying pump 8, a steam system 9 and an exhaust gas recovery system 10.
Detailed Description
As shown in figure 1, the vacuum operation system for producing ammonium sulfate by caprolactam comprises an ammonium sulfate crystallizer 1, wherein the ammonium sulfate crystallizer 1 is sequentially communicated with a first-stage condenser 2 and a second-stage condenser 3 through pipelines, the second-stage condenser 3 is communicated with a steam jet unit 4 and a dry vacuum unit 5 through pipelines, the steam jet unit 4 is communicated with a steam system 9 through a pipeline, the top of the dry vacuum unit 5 is communicated with a tail gas recovery system 10 through a pipeline, the bottoms of the steam jet unit 4, the dry vacuum unit 5, the first-stage condenser 2 and the second-stage condenser 3 are all communicated with a condensate collecting tank 6, a partition plate is arranged in the condensate collecting tank 6, the partition plate divides the condensate collecting tank 6 into a left cavity and a right cavity, the tops of the two cavities are mutually communicated, and the two cavities are respectively communicated with a condensate conveying pump 8 and an organic phase conveying pump 7.
The bottom of the primary condenser 2 is provided with a gas-liquid separation bag, the orifice of the gas phase is provided with a baffle, and the heat exchange medium is circulating water with the temperature of 10-30 ℃.
The primary condenser 2 and the secondary condenser 3 are made of 316L stainless steel, and the heat exchange medium is chilled water at 5-7 ℃.
The steam jet unit 4 adopts two-stage steam jet, and the steam pressure is 1.2-2.0MPa;
the dry vacuum unit 5 adopts the form of an air-cooled Roots vacuum pump, a claw type vacuum pump or an air-cooled Roots vacuum pump, a screw vacuum pump, a vacuum pump motor adopts a variable frequency explosion-proof motor, a stator, a rotor, a shaft and a shaft sleeve of the vacuum pump are all made of 205 stainless steel, other overflowing parts in the dry vacuum unit are made of 316L stainless steel, and cooling media in the dry vacuum unit adopt chilled water at 5-7 ℃;
the working process of the utility model is as follows: the ammonium sulfate crystallizer runs under the vacuum condition, firstly passes through the first-stage condenser 2, the cooling medium is circulating water, then passes through the second-stage condenser 3, the cooling medium is chilled water, water vapor, cyclohexane and the like are cooled down through two-stage cooling, then gas phase is compressed and pumped away through the Roots blower, then gas is further compressed through the claw pump, after passing through the Roots blower and the claw pump, a condensable medium is condensed, noncondensable gas is pumped away, the purpose of vacuum is achieved, the condensed liquid phase returns to the system, and no waste water is generated, so that the purposes of energy conservation, consumption reduction and environmental protection are achieved.
Claims (5)
1. A vacuum operation system for producing ammonium sulfate crystals from caprolactam, which is characterized in that: including ammonium sulfate crystallizer (1), ammonium sulfate crystallizer (1) is in proper order with one-level condenser (2) and second grade condenser (3) through the pipeline intercommunication, second grade condenser (3) are through pipeline and steam injection unit (4) and dry-type vacuum unit (5) intercommunication, steam injection unit (4) are through pipeline intercommunication steam system (9), dry-type vacuum unit (5) top is through pipeline intercommunication tail gas recovery system (10), steam injection unit (4), dry-type vacuum unit (5), one-level condenser (2) and second grade condenser (3) bottom all communicate with condensate collecting vat (6), condensate collecting vat (6) are inside to set up the baffle, two cavities about the baffle separates condensate collecting vat (6), two cavity tops communicate each other, two cavities communicate with condensate delivery pump (8) and organic phase delivery pump (7) respectively.
2. A crystallization vacuum operating system for producing ammonium sulfate from caprolactam according to claim 1, wherein: the bottom of the first-stage condenser (2) is provided with a gas-liquid separation bag, and a gas-phase pipe orifice is provided with a baffle plate.
3. A crystallization vacuum operating system for producing ammonium sulfate from caprolactam according to claim 1, wherein: the primary condenser (2) and the secondary condenser (3) are made of 316L stainless steel, and the temperature of cooling water fed into the secondary condenser (3) is lower than that of the primary condenser (2).
4. A crystallization vacuum operating system for producing ammonium sulfate from caprolactam according to claim 1, wherein: the steam jet unit (4) adopts two-stage steam jet.
5. A crystallization vacuum operating system for producing ammonium sulfate from caprolactam according to claim 1, wherein: the vacuum pump motor in the dry vacuum unit (5) adopts a variable frequency explosion-proof motor.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202321598650.1U CN220237804U (en) | 2023-06-21 | 2023-06-21 | Crystallization vacuum operation system for producing ammonium sulfate from caprolactam |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202321598650.1U CN220237804U (en) | 2023-06-21 | 2023-06-21 | Crystallization vacuum operation system for producing ammonium sulfate from caprolactam |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN220237804U true CN220237804U (en) | 2023-12-26 |
Family
ID=89267951
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202321598650.1U Active CN220237804U (en) | 2023-06-21 | 2023-06-21 | Crystallization vacuum operation system for producing ammonium sulfate from caprolactam |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN220237804U (en) |
-
2023
- 2023-06-21 CN CN202321598650.1U patent/CN220237804U/en active Active
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