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A kind of preparation method of long carbon chain cyano acid

A technology of carbon chain cyano acid and cyano acid, which is applied in the direction of carboxylate preparation, carboxylate preparation, carboxylic acid amide preparation, etc., and can solve the problem that there is no process route for synthesizing nylon 9 and nylon 10

Active Publication Date: 2021-06-18
WUXI YINDA NYLON
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, there are no reports of nylon 9 and nylon 10 in the market, the main reason is that there is no monomer and mature process route for synthesizing nylon 9 and nylon 10

Method used

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  • A kind of preparation method of long carbon chain cyano acid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] Put 2kg of azelaic acid and 60g of self-made composite catalyst into the reaction kettle, heat it to a molten state, close the valve, and after checking the air tightness, start the cooling liquid circulation pump of the packed tower (jacket temperature is 120-130°C), Ammonia gas was introduced slowly (mass flow meter control); then the gas circulation pump was started, nitrogen was automatically replenished during the process, and the pressure was maintained at 0.3 MPa.

[0039] The ammonia flow rate in the early stage is kept at 50cm 3 / h, heating to keep the temperature of the kettle at 165°C, and the pressure of the kettle at a constant 0.3MPa. After the reaction time is 2 hours, the temperature is gradually raised to 285°C. By adjusting the opening of the valve, the flow rate of ammonia is maintained at 20cm 3 / h, the pressure in the kettle was maintained at 0.2MPa, and the reaction time was 6 hours.

[0040] Stop the gas pump after the reaction is finished, take ...

Embodiment 2

[0042] Put 2kg of azelaic acid and 60g of self-made composite catalyst into the high-pressure reactor, heat it to a molten state, close the valve, and after checking the air tightness, start the cooling liquid circulation pump of the packed tower (jacket temperature is 120-130°C) , slowly feed ammonia gas (mass flow meter control); then start the gas circulation pump, automatically replenish nitrogen during the process, and maintain the pressure at 0.3MPa.

[0043] The ammonia flow rate in the early stage is kept at 50cm 3 / h, heating to keep the temperature of the kettle at 170°C, and the pressure of the kettle to be constant at 0.3MPa. After the reaction time is 2 hours, the temperature is gradually raised to 290°C, and the ammonia flow rate is maintained at 20cm by adjusting the opening of the valve. 3 / h, the pressure in the kettle was maintained at 0.2MPa, and the reaction time was 4.5 hours.

[0044] Stop the air pump after the reaction is finished, take out the crude p...

Embodiment 3

[0046]Put 2kg of sebacic acid and 60g of self-made composite catalyst into the high-pressure reactor, heat it to a molten state, close the valve, and after passing the air tightness inspection, start the cooling liquid circulation pump of the packed tower (jacket temperature is 120-130°C) , slowly feed ammonia gas (mass flow meter control); then start the gas circulation pump, automatically replenish nitrogen during the process, and maintain the pressure at 0.3MPa.

[0047] The ammonia flow rate in the early stage is kept at 50cm 3 / h, heating to keep the temperature of the kettle at 175°C, and the pressure of the kettle at a constant 0.2MPa. After the reaction time is 2 hours, the temperature is gradually raised to 295°C, and the ammonia flow rate is maintained at 20cm by adjusting the opening of the valve. 3 / h, the pressure in the kettle was maintained at 0.2MPa, and the reaction time was 5 hours.

[0048] Stop the air pump after the reaction is finished, take out the crud...

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Abstract

The invention relates to a preparation method of long carbon chain cyano acid, which belongs to the technical field of organic synthesis. First put the dibasic acid and catalyst into the reaction kettle, replace it with nitrogen, heat it to a molten state, start the cooling liquid of the packed tower, and slowly feed ammonia gas; then start the gas circulation pump, and automatically replenish nitrogen during the process, and the reaction time is 1 ~3 hours, and then quantitatively complete the required ammonia gas. The present invention adopts specific equipment, a specific process flow, and sets strict process conditions to prepare cyanoacid products, especially like 8-cyanoctanoic acid and 9-cyano nonanoic acid, which are synthetic nylon 9 and Front intermediate of nylon 10.

Description

technical field [0001] The invention relates to a preparation method of long carbon chain cyano acid, in particular to the application of 8-cyanoctanoic acid and 9-cyano nonanoic acid in the preparation of single-gauge nylon, which belongs to the technical field of organic synthesis. Background technique [0002] Polyamide resin is an important variety of polyamide engineering plastics. It has the characteristics of good flexibility, high mechanical strength, low density, acid and alkali corrosion resistance, and excellent electrical insulation properties. Because of its excellent performance, it is widely used in many fields such as automobile industry, medical equipment, electronic appliances, military industry and so on. [0003] At present, there are many varieties of nylon for production and industrial application, such as double-number nylon 66, nylon 610, nylon 612, nylon 1010, nylon 1012, nylon 1212, etc., single-number nylon 6, nylon 11, nylon 12, etc. And there ar...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C255/19C07C253/20C07C51/41C07C55/18C07C55/20C07C231/10C07C233/05
CPCC07C51/412C07C231/10C07C253/20C07C55/18C07C55/20C07C233/05C07C255/19
Inventor 陈尚标沈俊毅胡瑞莉殷炼伟
Owner WUXI YINDA NYLON
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