CN210506157U - Reaction device for continuously preparing 1, 6-hexamethylene diamine - Google Patents
Reaction device for continuously preparing 1, 6-hexamethylene diamine Download PDFInfo
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- CN210506157U CN210506157U CN201921369033.8U CN201921369033U CN210506157U CN 210506157 U CN210506157 U CN 210506157U CN 201921369033 U CN201921369033 U CN 201921369033U CN 210506157 U CN210506157 U CN 210506157U
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Abstract
The utility model discloses a reaction unit for continuously preparing 1, 6-hexamethylene diamine, which mainly comprises a liquid ammonia tank, an ammonia buffer tank, an ammonia gas and caprolactam preheater, a caprolactam ammonolysis reactor, a feed liquid condenser after ammonolysis, a feed liquid-gas separator after ammonolysis, a caprolactam and 6-aminocapronitrile liquid receiving tank, a caprolactam and 6-aminocapronitrile rectifying tower, a hydrogen and 6-aminocapronitrile preheater, a 6-aminocapronitrile hydrogenation reactor, a feed liquid condenser after hydrogenation, a feed liquid-gas separator after hydrogenation, a hydrogen refining tower, a hydrogen compressor, a hydrogen tank or a hydrogen recovery tank which are connected in sequence; the ammonia and the inlet of the caprolactam preheater are connected with a caprolactam raw material tank; the bottom of the hydrogenated feed liquid-gas-liquid separator is connected with a 1, 6-hexamethylenediamine product tank; and the inlets of the hydrogen and 6-aminocapronitrile preheater are sequentially connected with a hydrogen buffer tank and a hydrogen tank. The device can be operated continuously, and has the characteristics of low cost and high reactant utilization rate.
Description
Technical Field
The utility model relates to a continuous preparation 1, 6-hexanediamine's reaction unit belongs to the chemical plant field.
Background
The melting point of caprolactam is 68-71 ℃, and the boiling point is 270 ℃. The melting point of the 6-aminocapronitrile is-31.3 ℃, and the boiling point is 200.13 ℃. The melting point of the 1, 6-hexamethylene diamine is 42-45 ℃, and the boiling point is 205 ℃. 6-aminocapronitrile is an important chemical intermediate, and hydrogenation thereof can prepare 1, 6-hexanediamine. 1, 6-hexamethylenediamine is used for the most part for the synthesis of nylon 66 and 610 resins, and also for the synthesis of polyurethane resins, ion exchange resins and hexamethylene diisocyanate, and is used as a curing agent for urea resins, epoxy resins and the like, an organic crosslinking agent and the like, and also as a stabilizer, a bleaching agent for textile and paper industries, an anticorrosive agent for aluminum alloys, an emulsifier for chloroprene rubber and the like.
The prior preparation of 6-aminocapronitrile mainly comprises partial hydrogenation of 1, 6-adiponitrile, and the preparation of 6-aminocapronitrile from caprolactam is rare. Meanwhile, the hexamethylene diamine is mainly obtained by hydrogenation of adiponitrile at present, such as patents CN 107805203A and CN 106810454A. Patent CN 107739318A introduces a device for preparing 6-aminocapronitrile by a caprolactam liquid phase method, the device is a batch reaction device, the utilization rate of raw materials is low, the production efficiency is low, and the continuous reaction has the characteristics of high utilization rate of raw materials and high production efficiency. Patent CN 109261085A describes a system for synthesizing hexamethylene diamine, but relates to a system for preparing hexamethylene diamine by hydrogenation of adiponitrile. Therefore, it is necessary to develop a reaction apparatus for continuously preparing 1, 6-hexamethylenediamine by a series of reactions using caprolactam as a starting material.
SUMMERY OF THE UTILITY MODEL
The utility model provides a reaction device for continuously preparing 1, 6-hexanediamine. The method aims to solve a series of problems of low production efficiency and the like caused by the current batch reaction for preparing 6-aminocapronitrile, and enrich the content of a device for preparing 1, 6-hexamethylenediamine.
A reaction device for continuously preparing 1, 6-hexamethylene diamine mainly comprises a liquid ammonia tank, an ammonia buffer tank, an ammonia and caprolactam preheater, a caprolactam ammonolysis reactor, a feed liquid condenser after ammonolysis, a feed liquid and gas-liquid separator after ammonolysis, a caprolactam and 6-aminocapronitrile liquid receiving tank, a caprolactam and 6-aminocapronitrile rectifying tower, a hydrogen and 6-aminocapronitrile preheater, a 6-aminocapronitrile hydrogenation reactor, a feed liquid condenser after hydrogenation, a feed liquid and gas-liquid separator after hydrogenation, a hydrogen refining tower, a hydrogen compressor, a hydrogen tank or a hydrogen recovery tank which are connected in sequence;
the ammonia and the inlet of the caprolactam preheater are connected with a caprolactam raw material tank;
the top of the material liquid gas-liquid separator after ammonolysis is sequentially connected with an ammonia refining tower, an ammonia compressor, a liquid ammonia tank or a liquid ammonia recovery tank;
the bottom of the hydrogenated feed liquid-gas-liquid separator is connected with a 1, 6-hexamethylenediamine product tank;
and the inlets of the hydrogen and 6-aminocapronitrile preheater are sequentially connected with a hydrogen buffer tank and a hydrogen tank.
Further, in the above technical solution, the number of devices included in each unit is at least one.
Further, in the technical scheme, an outlet of the caprolactam raw material tank is connected with an inlet of the ammonia gas and a caprolactam preheater; the outlet of the liquid ammonia tank is connected with the inlet of the ammonia buffer tank; an outlet of the ammonia buffer tank is connected with an inlet of the ammonia gas and caprolactam preheater; the outlet of the ammonia gas and caprolactam preheater is connected with the inlet of the caprolactam ammonolysis reactor; the outlet of the caprolactam ammonolysis reactor is connected with the inlet of the feed liquid condenser after ammonolysis; the outlet of the feed liquid condenser after ammonolysis is connected with the inlet of the feed liquid gas-liquid separator after ammonolysis; a liquid outlet of the material liquid gas-liquid separator after ammonolysis is connected with an inlet of a caprolactam and 6-aminocapronitrile liquid receiving tank; the outlet of the caprolactam and 6-aminocapronitrile liquid receiving tank is connected with the inlet of a caprolactam and 6-aminocapronitrile rectifying tower, the bottom of the caprolactam and 6-aminocapronitrile rectifying tower is connected with a caprolactam raw material tank, and the gas outlet of the ammonolysis feed liquid-gas separator is connected with the inlet of an ammonia refining tower; the outlet of the ammonia refining tower is connected with the inlet of an ammonia compressor; the outlet of the ammonia compressor is connected with a liquid ammonia recovery tank of the liquid ammonia tank;
the upper part of the rectifying tower of caprolactam and 6-aminocapronitrile is connected with the inlet of a preheater of hydrogen and 6-aminocapronitrile; the outlet of the hydrogen and 6-aminocapronitrile preheater is connected with the inlet of the 6-aminocapronitrile hydrogenation reactor; the outlet of the 6-aminocapronitrile hydrogenation reactor is connected with the inlet of a hydrogenated feed liquid condenser; the outlet of the hydrogenated feed liquid condenser is connected with the inlet of the hydrogenated feed liquid gas-liquid separator; the liquid outlet of the hydrogenated feed liquid-gas-liquid separator is connected with a 1, 6-hexamethylenediamine product tank; the gas outlet of the hydrogenated feed liquid-gas-liquid separator is connected with the inlet of the hydrogen refining tower; the outlet of the hydrogen refining tower is connected with the inlet of a hydrogen compressor; the outlet of the hydrogen compressor is connected with the hydrogen tank, and the hydrogen is recycled.
The device can achieve the effect of continuous feeding and continuous discharging in the process of preparing the 1, 6-hexamethylene diamine, and improves the production efficiency.
The utility model discloses a have following effect:
(1) compared with the batch reaction for preparing 6-aminocapronitrile, the device has continuous operation and improves the production efficiency;
(2) the device has high utilization rate of different raw materials in the operation process, and can reduce the production cost.
Drawings
FIG. 1: a reaction device for continuously preparing 1, 6-hexamethylene diamine.
In fig. 1, the structures represented by the respective reference numerals are as follows:
1. a caprolactam raw material tank, a is a caprolactam raw material pipeline; 2. a liquid ammonia tank, b is an ammonia pipeline; 3. the ammonia buffer tank is a mixing pipeline before caprolactam and ammonia are preheated; 4. ammonia and caprolactam preheater, d is a mixing tube after preheating caprolactam and ammonia; 5. a caprolactam ammonolysis reactor, e is a mixed material liquid pipeline after reaction; 6. feed liquid condenser after ammonolysis, f is mixture liquid pipeline after feed liquid condensation after ammonolysis; 7. a feed liquid gas-liquid separator after ammonolysis, g is a mixed pipeline of caprolactam and 6-aminocapronitrile; 8. a caprolactam and 6-aminocapronitrile liquid receiving tank; 9. a caprolactam and 6-aminocapronitrile rectifying tower, wherein h is a 6-aminocapronitrile pipeline, i is an unreacted caprolactam pipeline, and caprolactam is recycled; j is an ammonia pipeline after gas-liquid separation of feed liquid after ammonolysis; 10. an ammonia refining tower, wherein k is a refined ammonia pipeline; 11. the ammonia compressor, m is a liquid ammonia pipeline, and is conveyed to a liquid ammonia tank for recycling; 12. a hydrogen tank, n is a hydrogen pipeline; 13. a hydrogen buffer tank, wherein o is a mixing pipeline before preheating of hydrogen and 6-aminocapronitrile; 14. a hydrogen and 6-aminocapronitrile preheater, wherein p is a mixing pipeline after the hydrogen and 6-aminocapronitrile are preheated; 15. a 6-aminocapronitrile hydrogenation reactor, wherein q is a mixed material liquid pipeline after 6-aminocapronitrile hydrogenation reaction; 16. a hydrogenated feed liquid condenser, wherein r is a mixed material liquid pipeline after the hydrogenated feed liquid is condensed; 17. a hydrogenated feed liquid gas-liquid separator; 18. a 1, 6-hexanediamine product tank; s is a 1, 6-hexamethylene diamine pipeline separated by a gas-liquid separator and connected with a 1, 6-hexamethylene diamine product tank; t is a hydrogen pipeline after the gas-liquid separator separates; 19. a hydrogen refining tower, wherein u is a refined hydrogen pipeline; 20. and v is a hydrogen pipeline after compression, and hydrogen is recycled.
Detailed Description
The principles and features of the present invention will be described with reference to the accompanying drawings, which are provided for illustration only and are not intended to limit the scope of the invention.
Example 1
As shown in fig. 1, a reaction apparatus for continuously preparing 1, 6-hexanediamine mainly comprises a liquid ammonia tank 2, an ammonia buffer tank 3, an ammonia and caprolactam preheater 4, a caprolactam ammonolysis reactor 5, a post-ammonolysis feed liquid condenser 6, a post-ammonolysis feed liquid-gas separator 7, a caprolactam and 6-aminocapronitrile liquid receiving tank 8, a caprolactam and 6-aminocapronitrile rectifying tower, a hydrogen and 6-aminocapronitrile preheater 14, a 6-aminocapronitrile hydrogenation reactor 15, a post-hydrogenation feed liquid condenser 16, a post-hydrogenation feed liquid-gas separator 17, a hydrogen refining tower 19, a hydrogen compressor 20, a hydrogen tank 12 or a hydrogen recovery tank which are connected in sequence;
the ammonia gas and the inlet of a caprolactam preheater 4 are connected with a caprolactam raw material tank 1;
the top of the material liquid gas-liquid separator 7 after ammonolysis is sequentially connected with an ammonia refining tower 10, an ammonia compressor 11, a liquid ammonia tank 2 or a liquid ammonia recovery tank;
the bottom of the hydrogenated feed liquid-gas-liquid separator 17 is connected with a 1, 6-hexamethylenediamine product tank 18;
the hydrogen and the inlet of the 6-aminocapronitrile preheater 14 are sequentially connected with a hydrogen buffer tank 13 and a hydrogen tank 12.
The number of devices contained in each unit is at least one.
An outlet of the caprolactam raw material tank 1 is connected with an inlet of an ammonia gas and caprolactam preheater 4; the outlet of the liquid ammonia tank 2 is connected with the inlet of the ammonia buffer tank 3; an outlet of the ammonia buffer tank 3 is connected with an inlet of an ammonia preheater 4 for caprolactam; the outlet of the ammonia gas and caprolactam preheater 4 is connected with the inlet of the caprolactam ammonolysis reactor 5; an outlet of the caprolactam ammonolysis reactor 5 is connected with an inlet of a feed liquid condenser 6 after ammonolysis; an outlet of the feed liquid condenser 6 after ammonolysis is connected with an inlet of the feed liquid gas-liquid separator 7 after ammonolysis; a liquid outlet of the material liquid gas-liquid separator 7 after ammonolysis is connected with an inlet of a caprolactam and 6-aminocapronitrile liquid receiving tank 8; an outlet of a caprolactam and 6-aminocapronitrile liquid receiving tank 8 is connected with an inlet of a caprolactam and 6-aminocapronitrile rectifying tower 9, the bottom of the caprolactam and 6-aminocapronitrile rectifying tower 9 is connected with a caprolactam raw material tank 1, and a gas outlet of a material liquid gas-liquid separator 7 after ammonolysis is connected with an inlet of an ammonia refining tower 10; the outlet of the ammonia refining tower 10 is connected with the inlet of an ammonia compressor 11; the outlet of the ammonia gas compressor 11 is connected with the liquid ammonia tank 2 or the liquid ammonia recovery tank;
the upper part of the rectifying tower 9 for caprolactam and 6-aminocapronitrile is connected with the inlet of a preheater 14 for 6-aminocapronitrile; the outlet of the hydrogen and 6-aminocapronitrile preheater 14 is connected with the inlet of the 6-aminocapronitrile hydrogenation reactor 15; an outlet of the 6-aminocapronitrile hydrogenation reactor 15 is connected with an inlet of a hydrogenated feed liquid condenser 16; an outlet of the hydrogenated feed liquid condenser 16 is connected with an inlet of a hydrogenated feed liquid gas-liquid separator 17; a liquid outlet of the hydrogenated feed liquid-gas-liquid separator 17 is connected with a 1, 6-hexanediamine product tank 18; the gas outlet of the hydrogenated feed liquid-gas liquid separator 17 is connected with the inlet of a hydrogen refining tower 19; the outlet of the hydrogen refining tower 19 is connected with the inlet of a hydrogen compressor 20; the outlet of the hydrogen compressor 20 is connected to the hydrogen tank 12. .
The caprolactam raw material tank 1 is provided with a feed inlet which is connected with caprolactam participating in the reaction; the ammonia refining tower 10 removes water possibly contained in the ammonia and entrained liquid feed liquid; the hydrogen refining column 19 removes liquid feed entrained in the hydrogen gas.
The above description is only for the preferred embodiment of the present invention, and is not intended to limit the present invention, and any modifications, equivalent replacements, improvements, etc. made within the spirit and principle of the present invention should be included within the protection scope of the present invention.
Claims (3)
1. A reaction device for continuously preparing 1, 6-hexamethylene diamine mainly comprises a liquid ammonia tank, an ammonia buffer tank, an ammonia and caprolactam preheater, a caprolactam ammonolysis reactor, a feed liquid condenser after ammonolysis, a feed liquid and gas-liquid separator after ammonolysis, a caprolactam and 6-aminocapronitrile liquid receiving tank, a caprolactam and 6-aminocapronitrile rectifying tower, a hydrogen and 6-aminocapronitrile preheater, a 6-aminocapronitrile hydrogenation reactor, a feed liquid condenser after hydrogenation, a feed liquid and gas-liquid separator after hydrogenation, a hydrogen refining tower, a hydrogen compressor, a hydrogen tank or a hydrogen recovery tank which are connected in sequence;
the ammonia and the inlet of the caprolactam preheater are connected with a caprolactam raw material tank;
the top of the material liquid gas-liquid separator after ammonolysis is sequentially connected with an ammonia refining tower, an ammonia compressor, a liquid ammonia tank or a liquid ammonia recovery tank;
the bottom of the hydrogenated feed liquid-gas-liquid separator is connected with a 1, 6-hexamethylenediamine product tank;
and the inlets of the hydrogen and 6-aminocapronitrile preheater are sequentially connected with a hydrogen buffer tank and a hydrogen tank.
2. The reactor apparatus of claim 1, wherein: the ammonia liquid tank, the ammonia gas buffer tank, the ammonia gas and caprolactam preheater, the caprolactam ammonolysis reactor, the feed liquid condenser after ammonolysis, the feed liquid gas-liquid separator after ammonolysis, the caprolactam and 6-aminocapronitrile liquid receiving tank, the caprolactam and 6-aminocapronitrile rectifying tower, the hydrogen gas and 6-aminocapronitrile preheater, the 6-aminocapronitrile hydrogenation reactor, the feed liquid condenser after hydrogenation, the feed liquid gas-liquid separator after hydrogenation, the hydrogen refining tower, the hydrogen compressor, the hydrogen tank or hydrogen recovery tank, the caprolactam raw material tank, the ammonia refining tower, the ammonia compressor, the liquid ammonia tank or liquid ammonia recovery tank, the hydrogen buffer tank are respectively at least one.
3. The reactor apparatus of claim 1, wherein: the outlet of the caprolactam raw material tank is connected with the inlet of the ammonia gas and the caprolactam preheater; the outlet of the liquid ammonia tank is connected with the inlet of the ammonia buffer tank; an outlet of the ammonia buffer tank is connected with an inlet of the ammonia gas and caprolactam preheater; the outlet of the ammonia gas and caprolactam preheater is connected with the inlet of the caprolactam ammonolysis reactor; the outlet of the caprolactam ammonolysis reactor is connected with the inlet of the feed liquid condenser after ammonolysis; the outlet of the feed liquid condenser after ammonolysis is connected with the inlet of the feed liquid gas-liquid separator after ammonolysis; a liquid outlet of the material liquid gas-liquid separator after ammonolysis is connected with an inlet of a caprolactam and 6-aminocapronitrile liquid receiving tank; the outlet of the caprolactam and 6-aminocapronitrile liquid receiving tank is connected with the inlet of a caprolactam and 6-aminocapronitrile rectifying tower, the bottom of the caprolactam and 6-aminocapronitrile rectifying tower is connected with a caprolactam raw material tank, and the gas outlet of the ammonolysis feed liquid-gas separator is connected with the inlet of an ammonia refining tower; the outlet of the ammonia refining tower is connected with the inlet of an ammonia compressor; the outlet of the ammonia compressor is connected with a liquid ammonia recovery tank of the liquid ammonia tank;
the upper part of the rectifying tower of caprolactam and 6-aminocapronitrile is connected with the inlet of a preheater of hydrogen and 6-aminocapronitrile; the outlet of the hydrogen and 6-aminocapronitrile preheater is connected with the inlet of the 6-aminocapronitrile hydrogenation reactor; the outlet of the 6-aminocapronitrile hydrogenation reactor is connected with the inlet of a hydrogenated feed liquid condenser; the outlet of the hydrogenated feed liquid condenser is connected with the inlet of the hydrogenated feed liquid gas-liquid separator; the liquid outlet of the hydrogenated feed liquid-gas-liquid separator is connected with a 1, 6-hexamethylenediamine product tank; the gas outlet of the hydrogenated feed liquid-gas-liquid separator is connected with the inlet of the hydrogen refining tower; the outlet of the hydrogen refining tower is connected with the inlet of a hydrogen compressor; the outlet of the hydrogen compressor is connected with the hydrogen tank.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111978206A (en) * | 2020-09-22 | 2020-11-24 | 江苏扬农化工集团有限公司 | Process system for synthesizing hexamethylene diamine key intermediate |
| 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 |
| CN112812020A (en) * | 2021-02-08 | 2021-05-18 | 陈天然 | Method and device for producing hexamethylene diamine from caprolactam |
| CN113398857A (en) * | 2021-08-02 | 2021-09-17 | 江苏扬农化工集团有限公司 | Magnetically stable reaction device and preparation method of hexamethylenediamine by using same |
| CN113797929A (en) * | 2020-06-17 | 2021-12-17 | 中国科学院过程工程研究所 | Solid catalyst for catalyzing synthesis of butanediamine, method for preparing butanediamine by using solid catalyst and system device |
| CN114011468A (en) * | 2021-11-17 | 2022-02-08 | 江苏凯美普瑞工程技术有限公司 | Copper carbene catalyst and preparation method and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113797929A (en) * | 2020-06-17 | 2021-12-17 | 中国科学院过程工程研究所 | Solid catalyst for catalyzing synthesis of butanediamine, method for preparing butanediamine by using solid catalyst and system device |
| CN111978206A (en) * | 2020-09-22 | 2020-11-24 | 江苏扬农化工集团有限公司 | Process system for synthesizing hexamethylene diamine key intermediate |
| CN111978206B (en) * | 2020-09-22 | 2023-03-14 | 江苏扬农化工集团有限公司 | Process system for synthesizing hexamethylene diamine key intermediate |
| 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 |
| CN112812020A (en) * | 2021-02-08 | 2021-05-18 | 陈天然 | Method and device for producing hexamethylene diamine from caprolactam |
| CN113398857A (en) * | 2021-08-02 | 2021-09-17 | 江苏扬农化工集团有限公司 | Magnetically stable reaction device and preparation method of hexamethylenediamine by using same |
| CN113398857B (en) * | 2021-08-02 | 2024-04-30 | 江苏扬农化工集团有限公司 | Magnetic stabilization reaction device and preparation method of hexamethylenediamine by using same |
| CN114011468A (en) * | 2021-11-17 | 2022-02-08 | 江苏凯美普瑞工程技术有限公司 | Copper carbene catalyst and preparation method and application thereof |
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