CN220194012U - Device for producing 6-aminocapronitrile by taking caprolactam as raw material - Google Patents
Device for producing 6-aminocapronitrile by taking caprolactam as raw material Download PDFInfo
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- CN220194012U CN220194012U CN202321587840.3U CN202321587840U CN220194012U CN 220194012 U CN220194012 U CN 220194012U CN 202321587840 U CN202321587840 U CN 202321587840U CN 220194012 U CN220194012 U CN 220194012U
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- caprolactam
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- aminocapronitrile
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- JBKVHLHDHHXQEQ-UHFFFAOYSA-N epsilon-caprolactam Chemical compound O=C1CCCCCN1 JBKVHLHDHHXQEQ-UHFFFAOYSA-N 0.000 title claims abstract description 454
- KBMSFJFLSXLIDJ-UHFFFAOYSA-N 6-aminohexanenitrile Chemical compound NCCCCCC#N KBMSFJFLSXLIDJ-UHFFFAOYSA-N 0.000 title claims abstract description 44
- 239000002994 raw material Substances 0.000 title claims abstract description 16
- 238000004821 distillation Methods 0.000 claims abstract description 52
- 238000006297 dehydration reaction Methods 0.000 claims abstract description 43
- 238000004176 ammonification Methods 0.000 claims abstract description 37
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 36
- 239000012071 phase Substances 0.000 claims abstract description 32
- 239000007791 liquid phase Substances 0.000 claims abstract description 22
- 230000018044 dehydration Effects 0.000 claims abstract description 16
- 238000011084 recovery Methods 0.000 claims abstract description 12
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 42
- 229910021529 ammonia Inorganic materials 0.000 claims description 16
- 239000003513 alkali Substances 0.000 claims description 10
- 239000000376 reactant Substances 0.000 claims description 10
- 238000007670 refining Methods 0.000 claims description 10
- 238000010992 reflux Methods 0.000 claims description 9
- 238000003860 storage Methods 0.000 claims description 3
- 238000007599 discharging Methods 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 9
- 238000005265 energy consumption Methods 0.000 abstract description 3
- 238000000926 separation method Methods 0.000 description 28
- 239000006227 byproduct Substances 0.000 description 16
- HEMHJVSKTPXQMS-UHFFFAOYSA-M sodium hydroxide Inorganic materials [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 14
- 239000003054 catalyst Substances 0.000 description 9
- 238000006243 chemical reaction Methods 0.000 description 9
- UNAQSRLBVVDYGP-UHFFFAOYSA-N hex-5-enenitrile Chemical compound C=CCCCC#N UNAQSRLBVVDYGP-UHFFFAOYSA-N 0.000 description 8
- 239000000463 material Substances 0.000 description 8
- 238000001704 evaporation Methods 0.000 description 7
- AWSFEOSAIZJXLG-UHFFFAOYSA-N azepan-2-one;hydrate Chemical compound O.O=C1CCCCCN1 AWSFEOSAIZJXLG-UHFFFAOYSA-N 0.000 description 6
- 238000000605 extraction Methods 0.000 description 5
- 238000000034 method Methods 0.000 description 5
- 238000002156 mixing Methods 0.000 description 5
- 239000000203 mixture Substances 0.000 description 5
- 238000009833 condensation Methods 0.000 description 4
- 230000005494 condensation Effects 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- NAQMVNRVTILPCV-UHFFFAOYSA-N hexane-1,6-diamine Chemical compound NCCCCCCN NAQMVNRVTILPCV-UHFFFAOYSA-N 0.000 description 4
- 238000004065 wastewater treatment Methods 0.000 description 4
- 239000004952 Polyamide Substances 0.000 description 2
- 238000005984 hydrogenation reaction Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 229920002647 polyamide Polymers 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- PWXIKGAMKWRXHD-UHFFFAOYSA-N 3-butylaziridin-2-one Chemical compound CCCCC1NC1=O PWXIKGAMKWRXHD-UHFFFAOYSA-N 0.000 description 1
- QPJCYJIZFCJYIR-UHFFFAOYSA-N 4-propylazetidin-2-one Chemical compound CCCC1CC(=O)N1 QPJCYJIZFCJYIR-UHFFFAOYSA-N 0.000 description 1
- QMXPTUUFGSTIKK-UHFFFAOYSA-N 5-ethylpyrrolidin-2-one Chemical compound CCC1CCC(=O)N1 QMXPTUUFGSTIKK-UHFFFAOYSA-N 0.000 description 1
- XPMMAKUHNMSONL-UHFFFAOYSA-N 6-methylpiperidin-2-one Chemical compound CC1CCCC(=O)N1 XPMMAKUHNMSONL-UHFFFAOYSA-N 0.000 description 1
- 229920002302 Nylon 6,6 Polymers 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000007037 hydroformylation reaction Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- ISBHMJZRKAFTGE-UHFFFAOYSA-N pent-2-enenitrile Chemical compound CCC=CC#N ISBHMJZRKAFTGE-UHFFFAOYSA-N 0.000 description 1
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- Other In-Based Heterocyclic Compounds (AREA)
Abstract
The utility model discloses a device for producing 6-aminocapronitrile by taking caprolactam as a raw material, wherein a crude caprolactam feeding pipeline is connected with a crude caprolactam evaporator, the crude caprolactam evaporator is connected with a caprolactam distillation tower, the caprolactam distillation tower is connected with a caprolactam distillation tower condenser, a gas phase outlet of the caprolactam distillation tower condenser is connected with a caprolactam capturing tower, and a liquid phase outlet is connected with a caprolactam tank; the upper part of the caprolactam trapping tower is connected with a vacuum pump, the bottom is connected with a water-containing caprolactam tank, the water-containing caprolactam tank is connected with a low-temperature cooler and a caprolactam recovery tower, and the low-temperature cooler is connected with caprolactam trapping; the caprolactam tank is connected with an ammonification and dehydration reaction feed evaporator which is connected with an ammonification and dehydration reactor. The utility model uses crude caprolactam to replace high-purity caprolactam as a raw material for producing 6-aminocapronitrile, thereby reducing the production cost of 6-aminocapronitrile and the energy consumption for producing caprolactam from the source.
Description
Technical Field
The utility model belongs to the technical field of organic chemical industry, relates to a device for producing 6-aminocapronitrile by taking caprolactam as a raw material, and in particular relates to a device for producing 6-aminocapronitrile by taking crude caprolactam as a raw material.
Background
6-aminocapronitrile is an important chemical intermediate that can be used to produce 1, 6-hexamethylenediamine by complete hydrogenation, while 1, 6-hexamethylenediamine can be used to produce polymeric nylon 66. The preparation of 6-aminocapronitrile is currently mainly obtained by partial hydrogenation of 1, 6-adiponitrile, as in patent CN 1238334C, CN 101309897B; or by hydroformylation of pentenenitrile, as described in patent CN1100752C.
The 6-aminocapronitrile can also be prepared from caprolactam by ammonification and dehydration, CN 107602416a discloses a method for preparing 6-aminocapronitrile by gas phase method, which uses caprolactam as raw material, comprising the following steps: mixing caprolactam steam and hot ammonia gas according to a certain mass ratio; carrying out ammonification and dehydration reaction on a mixture of caprolactam steam and hot ammonia under the condition of a catalyst to obtain an ammonification effluent; and separating and purifying the obtained ammoniated effluent to obtain the pure 6-aminocapronitrile. The production device is used for industrially producing the 6-aminocapronitrile by taking high-purity caprolactam as a raw material, and the production cost is higher.
Disclosure of Invention
The utility model provides a device for producing 6-aminocapronitrile by taking caprolactam as a raw material, which directly prepares 6-aminocapronitrile by taking crude caprolactam as a raw material, can reduce the production cost of 6-aminocapronitrile and reduce the energy consumption of caprolactam production from the source.
The technical scheme adopted by the utility model is as follows:
the device for producing the 6-aminocapronitrile by taking the crude caprolactam as the raw material comprises an ammonification dehydration reaction feed evaporator, an ammonification dehydration reactor, a crude caprolactam evaporator, a caprolactam distillation tower condenser, a caprolactam tank, a caprolactam capturing tower, a vacuum pump, an aqueous caprolactam tank and a low-temperature cooler, wherein a crude caprolactam feed pipeline is connected with the crude caprolactam evaporator, the crude caprolactam evaporator is connected with the caprolactam distillation tower, a gas phase outlet of the caprolactam distillation tower is connected with the caprolactam distillation tower condenser, a gas phase outlet of the caprolactam distillation tower condenser is connected with the caprolactam capturing tower, and a liquid phase outlet of the caprolactam distillation tower condenser is connected with the caprolactam tank; the upper part of the caprolactam trapping tower is connected with a vacuum pump, a liquid phase outlet at the bottom is connected with a water-containing caprolactam tank, the water-containing caprolactam tank is respectively connected with a low-temperature cooler and a caprolactam recovery tower of an ammoniation reactant refining system, and an outlet of the low-temperature cooler is connected with the top of the caprolactam trapping tower; the caprolactam tank is connected with an ammonification and dehydration reaction feed evaporator which is connected with an ammonification and dehydration reactor.
A crude caprolactam storage tank can be arranged in front of the crude caprolactam evaporator, and an alkali liquor feed inlet is arranged on a crude caprolactam feed pipe.
The caprolactam distillation column is provided with a liquid phase discharge port for discharging heavy components.
The water-containing caprolactam tank is connected with a reflux pump which is respectively connected with the cryocooler and a caprolactam recovery tower of the ammoniation reactant refining system.
The ammoniation dehydration reactor is provided with a feed mixer, and caprolactam steam and gas ammonia are mixed in the feed mixer.
The utility model adopts the method for producing 6-aminocapronitrile by taking crude caprolactam as raw material by the device, and the crude caprolactam and alkali liquor are mixed according to a proportion and enter a crude caprolactam evaporator for evaporation; steam enters a caprolactam distillation tower for distillation, heavy components are discharged through a liquid phase outlet, and a gas phase enters a caprolactam distillation tower condenser for partial condensation; the liquid phase caprolactam of the caprolactam distillation tower condenser enters a caprolactam tank, and the gas phase enters a caprolactam capturing tower; in a caprolactam capturing tower, after a gas phase is cooled and absorbed by a refluxing caprolactam water solution, part of the gas phase is sent into a caprolactam recovery tower of an ammoniation reactant refining system to recover caprolactam, and the other part of the gas phase is cooled by low temperature water and then flows back to the top of the caprolactam capturing tower; the caprolactam in the caprolactam tank is evaporated by an ammonification dehydration reaction evaporator and enters an ammonification dehydration reaction to react to prepare 6-aminocapronitrile. The utility model realizes the preparation of 6-aminocapronitrile by taking crude caprolactam as a raw material through heavy component removal, dehydration and caprolactam water solution recovery.
The crude caprolactam is a caprolactam water solution with the caprolactam mass content of more than 90 percent, can be a caprolactam extraction liquid recovered by a polyamide device, can be a raffinate distilled by a caprolactam production device, and can be crude caprolactam from other sources.
Lye NaOH, KOH, ca (OH) 2 、Ba(OH) 2 The alkali liquor accounts for 0.2 to 5.0 percent of the mass of the crude caprolactam.
Crude caprolactam evaporator operating conditions: the temperature is 130-180 ℃ and the pressure is 1-8 kPaA.
Caprolactam distillation column operating conditions: the temperature is 130-180 ℃ and the pressure is 1-8 kPaA.
The distillation tower condenser is partially condensed by hot water, and the outlet temperature of the gas phase and the liquid phase is 85-100 ℃.
Caprolactam capture column operating conditions: the temperature is 2-10 ℃, the pressure is 1-8 kPaA, and the reflux ratio is controlled to be 1-3.
Caprolactam is evaporated in an ammonification dehydration reaction feed evaporator and is mixed in a reaction feed mixer according to a mass ratio of 1: mixing 2-1:10 with 250-350 ℃ hot ammonia gas, entering a fixed bed reactor filled with a catalyst, controlling the reaction temperature to be 300-400 ℃, controlling the reaction pressure to be 0.1-0.5 MPa, and controlling the contact time of the mixture of caprolactam steam and hot ammonia gas with the catalyst to be 0.1-1 s.
Feeding the ammoniated dehydration reaction material into a first-stage separation rectifying tower, wherein the top of the tower is water-containing ammonia steam, the bottom of the tower is epsilon-caprolactam, and returning the epsilon-caprolactam to a caprolactam evaporator; the middle part of the primary separation rectifying tower mainly comprises 6-aminocapronitrile material flow which enters the secondary separation rectifying tower, light byproducts are adopted at the top of the secondary separation rectifying tower, and the purity of the 6-aminocapronitrile is more than 99.6 percent at the bottom of the secondary separation rectifying tower; in the three-stage separation rectifying tower, ammonia gas is returned to the ammonia heater for heating and returned to the ammonification dehydration reaction system, water is extracted from the tower, light byproducts are arranged at the bottom of the tower, HN (5-hexenenitrile) can be obtained by separating the light byproducts and the light byproducts of the two-stage separation rectifying tower, and after alkali is added to the water extracted from the tower for ammonia extraction, the water is neutralized and discharged into the wastewater treatment device.
The utility model has the characteristics and effects that:
the utility model uses the crude caprolactam with heavy components and water removed by a crude caprolactam evaporator and a caprolactam distillation tower to replace high-purity caprolactam as the raw material for producing 6-aminocapronitrile, thereby reducing the production cost of 6-aminocapronitrile and the energy consumption for producing source caprolactam.
Drawings
FIG. 1 is a schematic diagram of an apparatus for producing 6-aminocapronitrile from caprolactam according to the utility model;
in the figure: 1-a crude caprolactam evaporator; a 2-caprolactam distillation column; a 3-caprolactam distillation column condenser; a 4-caprolactam tank; a 5-caprolactam capturing tower; 6-a vacuum pump; 7-an aqueous caprolactam tank; 8-a cryocooler; 9-ammonification dehydration reaction feeding evaporator; 10-ammonification dehydration reactor.
A-crude caprolactam; b-alkali liquor; c-heavy component; d-noncondensable gas; e-aqueous caprolactam; f-refined caprolactam; g-recycle caprolactam; h-caprolactam vapor; i-ammonia gas; j-ammonification dehydration reaction product.
Detailed Description
The utility model will be further illustrated by the following examples, without however being limited thereto.
As can be seen from FIG. 1, the utility model is a device for producing 6-aminocapronitrile by using caprolactam as a raw material, which mainly comprises a crude caprolactam evaporator, a caprolactam distillation column condenser, a caprolactam tank, a caprolactam capturing column, a vacuum pump, a water-containing caprolactam tank, a cryocooler, an ammonification dehydration reaction feeding evaporator and an ammonification dehydration reactor, wherein a crude caprolactam feeding pipeline is connected with the crude caprolactam evaporator, the crude caprolactam evaporator is connected with the caprolactam distillation column, and a liquid phase outlet of the caprolactam distillation column discharges heavy components; the gas phase outlet of the caprolactam distillation tower is connected with a caprolactam distillation tower condenser, the gas phase outlet of the caprolactam distillation tower condenser is connected with a caprolactam capturing tower, and the liquid phase outlet of the caprolactam distillation tower condenser is connected with a caprolactam tank; the upper part of the caprolactam trapping tower is connected with a vacuum pump, a liquid phase outlet at the bottom is connected with a water-containing caprolactam tank, the water-containing caprolactam tank is respectively connected with a low-temperature cooler and a caprolactam recovery tower of an ammoniation reactant refining system, and an outlet of the low-temperature cooler is connected with the top of the caprolactam trapping tower; the caprolactam tank is connected with an ammonification and dehydration reaction feed evaporator which is connected with an ammonification and dehydration reactor.
Further, a crude caprolactam storage tank can be arranged in front of the crude caprolactam evaporator, and an alkali liquor feed inlet is arranged in a crude caprolactam feed pipe.
Further, the aqueous caprolactam tank is connected with a reflux pump which is respectively connected with the cryocooler and a caprolactam recovery tower of the ammoniated reactant refining system.
Further, the ammoniation dehydration reactor is provided with a feed mixer in which caprolactam steam and gaseous ammonia are mixed.
The utility model uses the apparatus of FIG. 1, and the specific examples of the production of 6-aminocapronitrile from crude caprolactam are as follows:
example 1
Adding sodium hydroxide into crude caprolactam with the caprolactam mass content of 93% according to the mass ratio of 1.5%, mixing, evaporating by a crude caprolactam evaporator, and controlling the evaporating temperature to be 130-180 ℃ and the pressure to be 1-8 kPaA; the steam enters a caprolactam distillation tower for distillation, the distillation temperature is controlled to be 130-180 ℃, the pressure is controlled to be 1-8 kPaA, heavy components are discharged through a liquid phase outlet, and a gas phase enters a caprolactam distillation tower condenser for condensation; the caprolactam distillation tower condenser is partially condensed by hot water, the outlet temperature of gas phase and liquid phase is 85-100 ℃, the liquid phase caprolactam of the distillation tower condenser enters a caprolactam tank, and the gas phase enters a caprolactam capturing tower; caprolactam capture column operating conditions: in a caprolactam trapping tower, after a gas phase is cooled and absorbed by a refluxing caprolactam water solution, part of the gas phase is fed into a caprolactam recovery tower of an ammoniation reactant refining system to recover caprolactam, and the other part of the gas phase is cooled by low temperature water and then flows back to the top of the caprolactam trapping tower; the caprolactam in the caprolactam tank is evaporated by an ammonification dehydration reaction evaporator and enters an ammonification dehydration reaction to react to prepare 6-aminocapronitrile.
The ammonification dehydration reactor is a fixed bed reactor filled with a catalyst, the reaction temperature is controlled to be 300-400 ℃, the reaction pressure is controlled to be 0.1-0.5 MPa, and the contact time of the mixture of caprolactam steam and hot ammonia gas and the catalyst is controlled to be 0.1-1 s.
Feeding the ammoniated dehydration reaction material into a first-stage separation rectifying tower, wherein the top of the tower is water-containing ammonia steam, the bottom of the tower is epsilon-caprolactam, and returning the epsilon-caprolactam to a caprolactam evaporator; the middle part of the primary separation rectifying tower mainly comprises 6-aminocapronitrile material flow which enters the secondary separation rectifying tower, light byproducts are adopted at the top of the secondary separation rectifying tower, and the purity of the 6-aminocapronitrile is more than 99.8 percent at the bottom of the secondary separation rectifying tower; in the three-stage separation rectifying tower, ammonia gas is returned to the ammonia heater for heating and returned to the ammonification dehydration reaction system, water is extracted from the tower, light byproducts are arranged at the bottom of the tower, HN (5-hexenenitrile) can be obtained by separating the light byproducts and the light byproducts of the two-stage separation rectifying tower, and after alkali is added to the water extracted from the tower for ammonia extraction, the water is neutralized and discharged into the wastewater treatment device.
In the whole process, the molar yield of 6-aminocapronitrile relative to caprolactam reaches 92.3 percent.
Example 2
Adding sodium hydroxide into polyamide device extract with 90 mass percent of caprolactam according to the mass ratio of 2.5 percent, mixing, evaporating by a crude caprolactam evaporator, controlling the evaporating temperature to be 130-180 ℃ and the pressure to be 1-8 kPaA; the steam enters a caprolactam distillation tower for distillation, the distillation temperature is controlled to be 130-180 ℃, the pressure is controlled to be 1-8 kPaA, heavy components are discharged through a liquid phase outlet, and a gas phase enters a caprolactam distillation tower condenser for condensation; the caprolactam distillation tower condenser is partially condensed by hot water, the outlet temperature of gas phase and liquid phase is 85-100 ℃, the liquid phase caprolactam of the distillation tower condenser enters a caprolactam tank, and the gas phase enters a caprolactam capturing tower; caprolactam capture column operating conditions: in a caprolactam trapping tower, after a gas phase is cooled and absorbed by a refluxing caprolactam water solution, part of the gas phase is fed into a caprolactam recovery tower of an ammoniation reactant refining system to recover caprolactam, and the other part of the gas phase is cooled by low temperature water and then flows back to the top of the caprolactam trapping tower; the caprolactam in the caprolactam tank is evaporated by an ammonification dehydration reaction evaporator and enters an ammonification dehydration reaction to react to prepare 6-aminocapronitrile.
The ammonification dehydration reactor is a fixed bed reactor filled with a catalyst, the reaction temperature is controlled to be 300-400 ℃, the reaction pressure is controlled to be 0.1-0.5 MPa, and the contact time of the mixture of caprolactam steam and hot ammonia gas and the catalyst is controlled to be 0.1-1 s.
Feeding the ammoniated dehydration reaction material into a first-stage separation rectifying tower, wherein the top of the tower is water-containing ammonia steam, the bottom of the tower is epsilon-caprolactam, and returning the epsilon-caprolactam to a caprolactam evaporator; the middle part of the primary separation rectifying tower mainly comprises 6-aminocapronitrile material flow which enters the secondary separation rectifying tower, light byproducts are adopted at the top of the secondary separation rectifying tower, and the purity of the 6-aminocapronitrile is more than 99.8 percent at the bottom of the secondary separation rectifying tower; in the three-stage separation rectifying tower, ammonia gas is returned to the ammonia heater for heating and returned to the ammonification dehydration reaction system, water is extracted from the tower, light byproducts are arranged at the bottom of the tower, HN (5-hexenenitrile) can be obtained by separating the light byproducts and the light byproducts of the two-stage separation rectifying tower, and after alkali is added to the water extracted from the tower for ammonia extraction, the water is neutralized and discharged into the wastewater treatment device.
In the whole process, the molar yield of 6-aminocapronitrile relative to caprolactam reaches 92.0%.
Example 3
Adding sodium hydroxide into the residual liquid of caprolactam with the caprolactam mass content of 98% according to the mass ratio of 1.0%, mixing, evaporating by a crude caprolactam evaporator, and controlling the evaporating temperature to be 130-180 ℃ and the pressure to be 1-8 kPaA; the steam enters a caprolactam distillation tower for distillation, the distillation temperature is controlled to be 130-180 ℃, the pressure is controlled to be 1-8 kPaA, heavy components are discharged through a liquid phase outlet, and a gas phase enters a caprolactam distillation tower condenser for condensation; the caprolactam distillation tower condenser is partially condensed by hot water, the outlet temperature of gas phase and liquid phase is 85-100 ℃, the liquid phase caprolactam of the distillation tower condenser enters a caprolactam tank, and the gas phase enters a caprolactam capturing tower; caprolactam capture column operating conditions: in a caprolactam trapping tower, after a gas phase is cooled and absorbed by a refluxing caprolactam water solution, part of the gas phase is fed into a caprolactam recovery tower of an ammoniation reactant refining system to recover caprolactam, and the other part of the gas phase is cooled by low temperature water and then flows back to the top of the caprolactam trapping tower; the caprolactam in the caprolactam tank is evaporated by an ammonification dehydration reaction evaporator and enters an ammonification dehydration reaction to react to prepare 6-aminocapronitrile.
The ammonification dehydration reactor is a fixed bed reactor filled with a catalyst, the reaction temperature is controlled to be 300-400 ℃, the reaction pressure is controlled to be 0.1-0.5 MPa, and the contact time of the mixture of caprolactam steam and hot ammonia gas and the catalyst is controlled to be 0.1-1 s.
Feeding the ammoniated dehydration reaction material into a first-stage separation rectifying tower, wherein the top of the tower is water-containing ammonia steam, the bottom of the tower is epsilon-caprolactam, and returning the epsilon-caprolactam to a caprolactam evaporator; the middle part of the primary separation rectifying tower mainly comprises 6-aminocapronitrile material flow which enters the secondary separation rectifying tower, light byproducts are adopted at the top of the secondary separation rectifying tower, and the purity of the 6-aminocapronitrile is more than 99.8 percent at the bottom of the secondary separation rectifying tower; in the three-stage separation rectifying tower, ammonia gas is returned to the ammonia heater for heating and returned to the ammonification dehydration reaction system, water is extracted from the tower, light byproducts are arranged at the bottom of the tower, HN (5-hexenenitrile) can be obtained by separating the light byproducts and the light byproducts of the two-stage separation rectifying tower, and after alkali is added to the water extracted from the tower for ammonia extraction, the water is neutralized and discharged into the wastewater treatment device.
In the whole process, the molar yield of 6-aminocapronitrile relative to caprolactam reaches 96.5%.
The foregoing examples illustrate only a few embodiments of the utility model and are described in detail herein without thereby limiting the scope of the utility model. It should be noted that it will be apparent to those skilled in the art that several variations and modifications can be made without departing from the spirit of the utility model, which are all within the scope of the utility model. Accordingly, the scope of protection of the present utility model is to be determined by the appended claims.
Claims (5)
1. The device for producing the 6-aminocapronitrile by taking the caprolactam as the raw material comprises an ammonification dehydration reaction feed evaporator and an ammonification dehydration reactor, and is characterized by further comprising a crude caprolactam evaporator, a caprolactam distillation tower condenser, a caprolactam tank, a caprolactam trapping tower, a vacuum pump, a water-containing caprolactam tank and a low-temperature cooler, wherein a crude caprolactam feed pipeline is connected with the crude caprolactam evaporator, the crude caprolactam evaporator is connected with the caprolactam distillation tower, a gas phase outlet of the caprolactam distillation tower is connected with the caprolactam distillation tower condenser, a gas phase outlet of the caprolactam distillation tower condenser is connected with the caprolactam trapping tower, and a liquid phase outlet of the caprolactam distillation tower condenser is connected with the caprolactam tank; the upper part of the caprolactam trapping tower is connected with a vacuum pump, a liquid phase outlet at the bottom is connected with a water-containing caprolactam tank, the water-containing caprolactam tank is respectively connected with a low-temperature cooler and a caprolactam recovery tower of an ammoniation reactant refining system, and an outlet of the low-temperature cooler is connected with the top of the caprolactam trapping tower; the caprolactam tank is connected with an ammonification and dehydration reaction feed evaporator which is connected with an ammonification and dehydration reactor.
2. The apparatus for producing 6-aminocapronitrile from caprolactam according to claim 1, wherein a crude caprolactam storage tank is arranged in front of the crude caprolactam evaporator, and an alkali liquor feed inlet is arranged in the crude caprolactam feed pipe.
3. The apparatus for producing 6-aminocapronitrile from caprolactam according to claim 1, wherein the caprolactam distillation column is provided with a liquid phase discharge port for discharging the heavy components.
4. The apparatus for producing 6-aminocapronitrile from caprolactam according to claim 1, wherein the aqueous caprolactam tank is connected to a reflux pump, and the reflux pump outlet is connected to a cryocooler and a caprolactam recovery column of an ammoniated reactant refining system, respectively.
5. The apparatus for producing 6-aminocapronitrile from caprolactam according to claim 1, wherein the ammonification and dehydration reactor is provided with a feed mixer, and caprolactam steam and gaseous ammonia are mixed in the feed mixer.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202321587840.3U CN220194012U (en) | 2023-06-21 | 2023-06-21 | Device for producing 6-aminocapronitrile by taking caprolactam as raw material |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202321587840.3U CN220194012U (en) | 2023-06-21 | 2023-06-21 | Device for producing 6-aminocapronitrile by taking caprolactam as raw material |
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| CN202321587840.3U Active CN220194012U (en) | 2023-06-21 | 2023-06-21 | Device for producing 6-aminocapronitrile by taking caprolactam as raw material |
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