CN112979496A - Method and device for preparing 4-aminobutyronitrile by adopting pyrrolidone liquid phase method - Google Patents
Method and device for preparing 4-aminobutyronitrile by adopting pyrrolidone liquid phase method Download PDFInfo
- Publication number
- CN112979496A CN112979496A CN202110299864.8A CN202110299864A CN112979496A CN 112979496 A CN112979496 A CN 112979496A CN 202110299864 A CN202110299864 A CN 202110299864A CN 112979496 A CN112979496 A CN 112979496A
- Authority
- CN
- China
- Prior art keywords
- gas
- pyrrolidone
- aminobutyronitrile
- reaction
- ammonia
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- HNJBEVLQSNELDL-UHFFFAOYSA-N pyrrolidin-2-one Chemical compound O=C1CCCN1 HNJBEVLQSNELDL-UHFFFAOYSA-N 0.000 title claims abstract description 49
- 238000000034 method Methods 0.000 title claims abstract description 45
- XGYKKVTZDQDYJQ-UHFFFAOYSA-N 4-aminobutanenitrile Chemical compound NCCCC#N XGYKKVTZDQDYJQ-UHFFFAOYSA-N 0.000 title claims abstract description 36
- 239000007791 liquid phase Substances 0.000 title claims abstract description 23
- 238000006243 chemical reaction Methods 0.000 claims abstract description 69
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims abstract description 62
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims abstract description 27
- 235000011114 ammonium hydroxide Nutrition 0.000 claims abstract description 26
- 239000007788 liquid Substances 0.000 claims abstract description 19
- 238000002360 preparation method Methods 0.000 claims abstract description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000000047 product Substances 0.000 claims abstract description 13
- 239000003960 organic solvent Substances 0.000 claims abstract description 10
- 238000004821 distillation Methods 0.000 claims abstract description 7
- 239000003054 catalyst Substances 0.000 claims abstract description 6
- 238000010438 heat treatment Methods 0.000 claims abstract description 6
- 238000002156 mixing Methods 0.000 claims abstract description 6
- 239000007795 chemical reaction product Substances 0.000 claims abstract description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical group [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 19
- IAHFWCOBPZCAEA-UHFFFAOYSA-N succinonitrile Chemical group N#CCCC#N IAHFWCOBPZCAEA-UHFFFAOYSA-N 0.000 claims description 11
- 239000003463 adsorbent Substances 0.000 claims description 7
- 239000000945 filler Substances 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- BTGRAWJCKBQKAO-UHFFFAOYSA-N adiponitrile Chemical compound N#CCCCCC#N BTGRAWJCKBQKAO-UHFFFAOYSA-N 0.000 claims description 4
- ZTOMUSMDRMJOTH-UHFFFAOYSA-N glutaronitrile Chemical compound N#CCCCC#N ZTOMUSMDRMJOTH-UHFFFAOYSA-N 0.000 claims description 4
- 239000002808 molecular sieve Substances 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims description 2
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 1
- 238000005265 energy consumption Methods 0.000 abstract description 3
- 239000002994 raw material Substances 0.000 description 4
- DQQIUVCNBOJDGF-UHFFFAOYSA-N 2-aminobutanenitrile Chemical compound CCC(N)C#N DQQIUVCNBOJDGF-UHFFFAOYSA-N 0.000 description 3
- YZYDPPZYDIRSJT-UHFFFAOYSA-K boron phosphate Chemical compound [B+3].[O-]P([O-])([O-])=O YZYDPPZYDIRSJT-UHFFFAOYSA-K 0.000 description 3
- 229910000149 boron phosphate Inorganic materials 0.000 description 3
- 239000006227 byproduct Substances 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 3
- FHKPTEOFUHYQFY-UHFFFAOYSA-N 2-aminohexanenitrile Chemical compound CCCCC(N)C#N FHKPTEOFUHYQFY-UHFFFAOYSA-N 0.000 description 2
- NBBJYMSMWIIQGU-UHFFFAOYSA-N Propionic aldehyde Chemical compound CCC=O NBBJYMSMWIIQGU-UHFFFAOYSA-N 0.000 description 2
- 229910021529 ammonia Inorganic materials 0.000 description 2
- 208000012839 conversion disease Diseases 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 238000005292 vacuum distillation Methods 0.000 description 2
- NGUGWHFIVAQVMN-UHFFFAOYSA-N 4-aminobut-3-en-2-one Chemical compound CC(=O)C=CN NGUGWHFIVAQVMN-UHFFFAOYSA-N 0.000 description 1
- XFXPMWWXUTWYJX-UHFFFAOYSA-N Cyanide Chemical compound N#[C-] XFXPMWWXUTWYJX-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 229910000069 nitrogen hydride Inorganic materials 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C253/00—Preparation of carboxylic acid nitriles
- C07C253/20—Preparation of carboxylic acid nitriles by dehydration of carboxylic acid amides
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01C—AMMONIA; CYANOGEN; COMPOUNDS THEREOF
- C01C1/00—Ammonia; Compounds thereof
- C01C1/02—Preparation, purification or separation of ammonia
- C01C1/024—Purification
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C253/00—Preparation of carboxylic acid nitriles
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/52—Improvements relating to the production of bulk chemicals using catalysts, e.g. selective catalysts
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Analytical Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a method and a device for preparing 4-aminobutyronitrile by adopting a pyrrolidone liquid phase method, wherein the preparation method comprises the following steps: mixing pyrrolidone and an organic solvent, and preheating at the temperature of 90-110 ℃; purifying and preheating ammonia gas, wherein the preheating temperature is 90-110 ℃; fully mixing the pyrrolidone, the organic solvent and the catalyst, heating to a certain temperature, and introducing ammonia gas into the reaction kettle for reaction; after the reaction is finished, carrying out reduced pressure distillation on the reaction product to obtain the product 4-aminobutyronitrile. The preparation device comprises an ammonia gas pretreatment device, a reaction kettle, an ammonia water separator, a condenser and a gas-liquid separator, wherein a gas outlet of the reaction kettle is communicated with a gas inlet of the ammonia water separator, a gas outlet of the ammonia water separator is communicated with a gas inlet of the condenser, a gas outlet of the condenser is communicated with a gas inlet of the gas-liquid separator, a gas outlet of the gas-liquid separator is communicated with a gas inlet of the reaction kettle, and a water outlet is arranged on the gas-liquid separator. The invention has the advantages of low energy consumption, easy reaction, high conversion rate and stable product quality.
Description
Technical Field
The invention belongs to the technical field of preparation of aminobutyronitrile, and particularly relates to a method and a device for preparing 4-aminobutyronitrile by adopting a pyrrolidone liquid phase method.
Background
The aminobutyronitrile is an important chemical intermediate, and is an important intermediate for organic synthesis and medical synthesis. Currently, the preparation of the aminobutyronitrile is mainly prepared by reacting n-propionaldehyde with excessive cyanide and then carrying out vacuum rectification, for example, the patent number CN 201911196336.9. However, the patents for preparing aminocapronitrile by taking pyrrolidone as a raw material are few, and the existing method for preparing 2-aminocapronitrile by taking pyrrolidone as a raw material can be divided into a gas phase method and a liquid phase method according to the reaction state of the pyrrolidone, wherein the gas phase method has high temperature, large reaction energy consumption and more reaction byproducts; the liquid phase method has low temperature, mild reaction condition, few by-products and high reaction conversion rate.
Disclosure of Invention
The invention aims to provide a method for preparing 4-aminobutyronitrile by adopting a pyrrolidone liquid phase method, wherein pyrrolidone and ammonia gas are used as raw materials, the reaction is simple, byproducts are few, and the reaction conversion rate is high.
In order to achieve the purpose, the technical scheme of the invention is realized as follows:
a method for preparing 4-aminobutyronitrile by adopting a pyrrolidone liquid phase method comprises the following steps:
step S1, mixing pyrrolidone and an organic solvent, and then preheating at the temperature of 90-110 ℃;
step S2, purifying and preheating ammonia gas by using an adsorbent, wherein the preheating temperature is 90-110 ℃;
step S3, sufficiently and uniformly mixing pyrrolidone, an organic solvent and a catalyst in a reactor, heating to a certain temperature, and introducing ammonia gas into a reaction kettle for reaction;
and step S4, after the reaction is finished, carrying out reduced pressure distillation on the reaction product to obtain the product 4-aminobutyronitrile.
In step S1, the organic solvent is succinonitrile, glutaronitrile or adiponitrile or a mixture of succinonitrile, glutaronitrile and adiponitrile.
Preferably, in step S1, the organic solvent is succinonitrile.
In step S2, the adsorbent is activated carbon or molecular sieve.
Preferably, in step S2, the adsorbent is activated carbon.
In step S3, the molar ratio of the pyrrolidone, the catalyst, and the ammonia gas is 1: (0.01-0.1): (1-10).
In step S4, the vacuum rectification conditions are that the kettle temperature is 130-150 ℃, the top temperature is 110-130 ℃, and the vacuum degree is-0.08-0.095 MPa.
In step S3, the reaction temperature is 200-230 ℃, the reaction stirring speed is 800-1200RPM, and the reaction time is 1.0-3.0 h.
In step S3, when the temperature reaches 160-220 ℃, ammonia gas is introduced, and the molar ratio of the ammonia gas to the pyrrolidone is (10-30): 1.
In step S3, the reaction kettle is a reaction kettle communicated with an ammonia water separator, wherein: the ammonia water separator is filled with filler.
The invention also aims to provide a preparation device used in the method for preparing 4-aminobutyronitrile by adopting the pyrrolidone liquid phase method, so as to prepare the 4-aminobutyronitrile.
A preparation device used in a method for preparing 4-aminobutyronitrile by adopting a pyrrolidone liquid phase method comprises an ammonia gas pretreatment device, a reaction kettle, an ammonia water separator, a condenser and a gas-liquid separator; the new ammonia gas and the recovered ammonia gas in the ammonia gas pre-processor are connected in series and enter a reaction kettle; the gas outlet of the reaction kettle is communicated with the gas inlet of an ammonia water separator, and the gas outlet of the ammonia water separator is communicated with the gas inlet of a condenser; the air outlet of the condenser is communicated with the air inlet of a gas-liquid separator, and the air outlet of the gas-liquid separator is communicated with the air inlet of the reaction kettle; and a water outlet is formed in the gas-liquid separator.
The adsorbent used by the ammonia gas pre-processor is activated carbon; the ammonia water separator is filled with filler to separate ammonia water; the circulating water of the condenser is cold water with the temperature lower than 100 ℃.
The invention takes pyrrolidone and ammonia gas as raw materials to prepare 4-aminobutyronitrile by a liquid phase method, and the pyrrolidone is aminated and dehydrated to prepare the 4-aminobutyronitrile, and the reaction principle is as follows:
C4H7NO+NH3=C4H8N2+H20
compared with the prior art, the method and the device for preparing 4-aminobutyronitrile have the following advantages:
(1) in the method for preparing 4-aminobutyronitrile, ammonia gas can be removed of ammonia gas impurities after passing through an ammonia gas pre-processor, so that the product quality is improved.
(2) The reaction of the invention is carried out in a reaction kettle provided with an ammonia water separator filled with filler, water and excessive ammonia gas generated in the reaction can be removed from the reaction kettle in time, the reaction is promoted to be carried out in the positive direction, and simultaneously, the 4-aminobutyronitrile, the pyrrolidone and the organic solvent are refluxed into the reaction kettle.
(3) The invention has low energy consumption, simple reaction and high product conversion rate.
Drawings
FIG. 1 is a schematic structural diagram of the apparatus for preparing 4-aminobutyronitrile according to the invention.
Wherein: 1-ammonia pre-processor; 2- - -a reaction kettle; 3- -an ammonia separator; 4-condenser; 5-a gas-liquid separator.
In FIG. 1, NMP is pyrrolidone and SN is succinonitrile.
Detailed Description
The technical solution of the present invention will be described in detail with reference to specific examples.
Example 1
As shown in fig. 1, a preparation apparatus for preparing 4-aminobutyronitrile by utilizing a pyrrolidone liquid phase method, comprises an ammonia gas pretreatment device 1, a reaction kettle 2, an ammonia water separator 3, a condenser 4 and a gas-liquid separator 5; the new ammonia gas and the recovered ammonia gas in the ammonia gas pretreatment device 1 are connected in series and enter a reaction kettle 2, a gas outlet of the reaction kettle 2 is communicated with a gas inlet of an ammonia water separator 3, and a gas outlet of the ammonia water separator 3 is communicated with a gas inlet of a condenser 4; an air outlet of the condenser 4 is communicated with an air inlet of the gas-liquid separator 5, and an air outlet of the gas-liquid separator 5 is communicated with an air inlet of the reaction kettle 1; a water outlet is arranged on the gas-liquid separator 5, and unreacted ammonia gas and new ammonia gas are connected in series and enter the reaction kettle 2 for continuous reaction.
Wherein: the ammonia water separator 3 is filled with filler, and the circulating water in the condenser 4 is circulating water condensate with the temperature lower than 100 ℃.
The use principle of the preparation device is as follows:
when the pyrrolidone liquid phase method is adopted to prepare the 4-aminobutyronitrile, ammonia gas and recovered ammonia gas which pass through the ammonia gas filter 1 are mixed and enter the reaction kettle 2 to react with the pyrrolidone, the catalyst and the succinonitrile in the reaction kettle, generated water and excessive ammonia gas pass through the ammonia water separator 3 to enter the cooling condenser 4, part of the pyrrolidone and a small amount of the succinonitrile flow back to the reaction kettle 2 to continue to react, ammonia gas and water pass through the cooling condenser 4 to enter the gas-liquid separator 5, water is discharged through the liquid outlet, and the ammonia gas flows back to the reaction kettle 2 to continue to react.
Examples 2-4 below are illustrative of the preparation of 4-aminobutyronitrile by the liquid phase pyrrolidone process under experimental conditions, and the vacuum distillation conditions are typical of laboratory vacuum distillation operations. The reduced pressure distillation conditions are that the temperature of the tower bottom is 130 ℃ plus 140 ℃, the temperature of the tower top is 110 ℃ plus 130 ℃, and the negative pressure is-0.085 to-0.095 MPA.
Example 2
Heating 100g of pyrrolidone, 1000g of succinonitrile and 1g of boron phosphate to 100 ℃ in a reaction kettle communicated with an ammonia water separator, preheating ammonia gas treated by an ammonia gas preprocessor to 100 ℃, starting stirring at 1000RPM, introducing ammonia gas when the temperature reaches 200 ℃, and reacting for 2 hours, wherein the molar ratio of the ammonia gas to the pyrrolidone is 10:1 in the reaction process. After the reaction is finished, the mixture is subjected to reduced pressure distillation in a tower, the temperature of a tower kettle is 130 ℃, the temperature of a tower top is 110 ℃, and the negative pressure is minus 0.095MPA, so that the 4-aminobutyronitrile with the purity of 99.7 percent is obtained.
Through product metering and analysis, the selectivity of the pyrrolidone in the example is 98.50%, and the conversion rate is 65.00%.
The technical indexes before and after the ammonia gas is adsorbed by the active carbon are shown in the following table:
| index (I) | Unit of | Before the adsorption of active carbon | After the activated carbon is absorbed |
| Content of Ammonia gas | Wt% | 99.10 | 99.90 |
| Oil content | ppm(wt) | 10.0 | 5.08 |
| Moisture content | Wt% | 0.20 | 0.05 |
As can be seen from the table above, the purity of the ammonia gas after being adsorbed by the active carbon is close to 100%, and the oil content and the moisture content are extremely low, so that the purpose of improving the content and the quality of the 4-aminobutyronitrile product is finally achieved.
In the embodiment, after the ammonia gas is treated by the activated carbon, the purity of the product is greatly improved, the purity of the 4-aminobutyronitrile obtained by the reaction of the purified ammonia gas is higher, and the content of impurities and moisture and the chromaticity are lower.
Example 3
Heating 100g of pyrrolidone, 800g of succinonitrile and 2g of boron phosphate in a reaction kettle with an ammonia-water separator to 110 ℃, preheating ammonia gas treated by an ammonia gas preprocessor to 110 ℃, starting stirring at 1200RPM, introducing ammonia gas when the temperature reaches 230 ℃, and reacting for 2 hours, wherein the molar ratio of the ammonia gas to the pyrrolidone is 20:1 in the reaction process. After the reaction is finished, the mixture is put into a tower for reduced pressure distillation, the temperature of the kettle of the tower is 150 ℃, the temperature of the top of the tower is 125 ℃, and the negative pressure is minus 0.085MPA, so that the 4-aminobutyronitrile with the purity of 99.6 percent is obtained.
Through product metering and analysis, the selectivity of the pyrrolidone in the example is 98.80%, and the conversion rate is 68.50%.
Example 4
Heating 100g of pyrrolidone, 1200g of succinonitrile and 3g of boron phosphate in a reaction kettle with an ammonia-water separator to 90 ℃, preheating ammonia gas treated by an ammonia gas preprocessor to 90 ℃, starting stirring at 800RPM, introducing ammonia gas when the temperature reaches 220 ℃, and reacting for 1 hour, wherein the molar ratio of the ammonia gas to the pyrrolidone is 30:1 in the reaction process. After the reaction is finished, the mixture is subjected to reduced pressure distillation in a tower, the temperature of a tower kettle is 140 ℃, the temperature of a tower top is 120 ℃, and the negative pressure is-0.090 MPA, so that the 4-aminobutyronitrile with the purity of 99.5 percent is obtained.
Through product metering and analysis, the selectivity of the pyrrolidone in the example is 98.1%, and the conversion rate is 59.50%.
The analysis of the products obtained in examples 2 to 4 is shown in the following table:
| content (%) | Chroma (Hazen) | Moisture (ppm) | Yield (%) | |
| Example 2 | 99.7 | 15 | 220 | 65.00 |
| Example 3 | 99.6 | 12 | 240 | 68.50 |
| Example 4 | 99.5 | 13 | 230 | 59.50 |
As can be seen from the above table, the 4-aminobutyronitrile prepared by the reaction of ammonia gas treated by activated carbon has the advantages of excellent performance, low chroma and moisture content, high product purity, simple process and simple operation.
The above description is only a preferred embodiment of the present invention and should not be taken as limiting the invention, and the technical solutions and technical suggestions made by equivalent replacement and obvious changes in the description and the drawings of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. A method for preparing 4-aminobutyronitrile by adopting a pyrrolidone liquid phase method is characterized by comprising the following steps:
step S1, mixing pyrrolidone and an organic solvent, and then preheating at the temperature of 90-110 ℃;
step S2, purifying and preheating ammonia gas by using an adsorbent, wherein the preheating temperature is 90-110 ℃;
step S3, sufficiently and uniformly mixing pyrrolidone, an organic solvent and a catalyst in a reactor, heating to a certain temperature, and introducing ammonia gas into a reaction kettle for reaction;
and step S4, after the reaction is finished, carrying out reduced pressure distillation on the reaction product to obtain the product 4-aminobutyronitrile.
2. A process according to claim 1 for the preparation of 4-aminobutyronitrile by liquid phase pyrrolidone process, wherein: in step S1, the organic solvent is succinonitrile, glutaronitrile or adiponitrile or a mixture of succinonitrile, glutaronitrile and adiponitrile.
3. A process according to claim 1 for the preparation of 4-aminobutyronitrile by liquid phase pyrrolidone process, wherein: in step S2, the adsorbent is activated carbon or molecular sieve.
4. A process according to claim 1 for the preparation of 4-aminobutyronitrile by liquid phase pyrrolidone process, wherein: in step S3, the molar ratio of the pyrrolidone, the catalyst, and the ammonia gas is 1: (0.01-0.1): (1-10).
5. A process according to claim 1 for the preparation of 4-aminobutyronitrile by liquid phase pyrrolidone process, wherein: in step S4, the vacuum rectification conditions are that the kettle temperature is 130-150 ℃, the top temperature is 110-130 ℃, and the vacuum degree is-0.08-0.095 MPa.
6. A process according to claim 1 for the preparation of 4-aminobutyronitrile by liquid phase pyrrolidone process, wherein: in step S3, the reaction temperature is 200-230 ℃, the reaction stirring speed is 800-1200RPM, and the reaction time is 1.0-3.0 h.
7. A process according to claim 1 for the preparation of 4-aminobutyronitrile by liquid phase pyrrolidone process, wherein: in step S3, when the temperature reaches 160-220 ℃, ammonia gas is introduced, and the molar ratio of the ammonia gas to the pyrrolidone is (10-30): 1.
8. A process according to claim 1 for the preparation of 4-aminobutyronitrile by liquid phase pyrrolidone process, wherein: in step S3, the reaction kettle is a reaction kettle communicated with an ammonia water separator, wherein: the ammonia water separator is filled with filler.
9. The apparatus for producing 4-aminobutyronitrile by a liquid phase process using pyrrolidone as defined in claim 1, wherein: the preparation device comprises an ammonia gas pretreatment device (1), a reaction kettle (2), an ammonia water separator (3), a condenser (4) and a gas-liquid separator (5); the new ammonia gas and the recovered ammonia gas in the ammonia gas pretreatment device (1) are connected in series and enter a reaction kettle (2); the gas outlet of the reaction kettle (2) is communicated with the gas inlet of the ammonia water separator (3), and the gas outlet of the ammonia water separator (3) is communicated with the gas inlet of the condenser (4); an air outlet of the condenser (4) is communicated with an air inlet of a gas-liquid separator (5), and an air outlet of the gas-liquid separator (5) is communicated with an air inlet of the reaction kettle (2); a water outlet is arranged on the gas-liquid separator (5).
10. The manufacturing apparatus according to claim 9, characterized in that: the adsorbent used by the ammonia gas pretreatment device (1) is activated carbon; the ammonia water separator (3) is filled with filler to separate ammonia water; the circulating water of the condenser (4) is cold water with the temperature lower than 100 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110299864.8A CN112979496A (en) | 2021-03-22 | 2021-03-22 | Method and device for preparing 4-aminobutyronitrile by adopting pyrrolidone liquid phase method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110299864.8A CN112979496A (en) | 2021-03-22 | 2021-03-22 | Method and device for preparing 4-aminobutyronitrile by adopting pyrrolidone liquid phase method |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN112979496A true CN112979496A (en) | 2021-06-18 |
Family
ID=76332691
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202110299864.8A Pending CN112979496A (en) | 2021-03-22 | 2021-03-22 | Method and device for preparing 4-aminobutyronitrile by adopting pyrrolidone liquid phase method |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN112979496A (en) |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107739318A (en) * | 2017-10-11 | 2018-02-27 | 中国天辰工程有限公司 | A kind of caprolactam liquid phase method prepares the method and device of 6 amino-capronitriles |
| CN112341339A (en) * | 2020-11-30 | 2021-02-09 | 江苏凯美普瑞工程技术有限公司 | Method and device for synthesizing 1, 4-butanediamine |
-
2021
- 2021-03-22 CN CN202110299864.8A patent/CN112979496A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107739318A (en) * | 2017-10-11 | 2018-02-27 | 中国天辰工程有限公司 | A kind of caprolactam liquid phase method prepares the method and device of 6 amino-capronitriles |
| CN112341339A (en) * | 2020-11-30 | 2021-02-09 | 江苏凯美普瑞工程技术有限公司 | Method and device for synthesizing 1, 4-butanediamine |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN110835311A (en) | Method for preparing 6-aminocapronitrile from cyclohexanone oxime | |
| CN101429139B (en) | Process for producing dicyclohexyl methyl hydride diisocyanate and its midbody | |
| ZA200605556B (en) | Process for the purification of olefinically unsaturated nitriles | |
| CN109456200B (en) | Preparation method of m-xylylenediamine | |
| CN100349839C (en) | Method for synthesising mixture of methanol and dimethyl ether from syngas | |
| CN113501770B (en) | Acetonitrile refining method | |
| CN114105818B (en) | Catalyst for preparing succinonitrile from butyrolactone and synthesis method | |
| CN1440963A (en) | Ethanol ammoxidizing process to synthesize high-purity acetonitrile | |
| CN112979496A (en) | Method and device for preparing 4-aminobutyronitrile by adopting pyrrolidone liquid phase method | |
| CN107445786B (en) | Method for preparing biphenyl by hydrogenation of dibenzofuran | |
| CN108927203B (en) | Regeneration method of phenol hydrogenation Pd @ CN catalyst | |
| CN115073343B (en) | Caprolactam synthesis method without by-product ammonium sulfate | |
| CN105367450B (en) | The efficient absorption method of acrylonitrile | |
| CN101443310A (en) | Process for continuously preparing n- ethyl-2-pyrrolidone (NEP) | |
| CN116082172B (en) | Method for producing isopropanolamine | |
| CN220478146U (en) | Device for producing caprolactam and co-producing 6-aminocapronitrile | |
| CN116003350B (en) | Preparation method of tetrahydrofuran | |
| CN116621674B (en) | Purification method of crude chlorobutane | |
| CN221085572U (en) | System for preparing acetaldehyde by ethanol dehydrogenation | |
| CN220835483U (en) | System for preparing tetrahydrofuran from 1, 4-butanediol | |
| CN215975599U (en) | Acrylonitrile and acetonitrile coproduction device | |
| KR102721330B1 (en) | Method for preparing acrylic acid | |
| CN101508683B (en) | Dehydrogenation ammoniation method for producing pyrrolidine with 1,4butanediol | |
| CN115228119B (en) | Dimethyl carbonate purification system and method | |
| CN102381930B (en) | Method for producing p-chorotoluene by using element selenium as catalyst |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20210618 |