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Method for purifying long-carbon-chain cyanic acid products

A cyano acid and long carbon chain technology, applied in the field of separation, can solve the problem of no synthetic process route of nylon 9 and nylon 10, and achieve the effect of strong repeatability, simple and reliable process

Active Publication Date: 2017-12-08
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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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Weigh 200g of the ammoniated product containing cyano acid, add 600mL of deionized water at a temperature of about 30~50℃, slowly add ammonia water with a concentration of 25%, stir well, and adjust the pH of the system to 9~12 ; Pour it into a 1500mL separatory funnel and let it stand to separate layers. Pour out the upper oil layer containing dinitriles, ie component A.

[0023] The aqueous solution of the water layer was added dropwise to it with a concentration of 50% H 2 SO 4 , keep stirring, let it fully mix, adjust the pH value of the system, and maintain it at 6.6~6.7. After the pH value is stable, let it stand for stratification, and use the same method to pour out the upper layer containing cyano acids, that is, the oil layer of component B. .

[0024] The aqueous solution of the water layer is continuously added dropwise to it with a concentration of 50% H 2 SO 4 , until the pH is 2~3, fully stirred and then cooled and centrifuged to obtain dibasic acid-...

Embodiment 2

[0027] Weigh 200g of the ammoniated product containing cyano acid, add 600mL of deionized water at a temperature of about 30~50℃, slowly add ammonia water with a concentration of 20%, stir well, and adjust the pH of the system to 9~12 ,. Pour it into a 1500mL separatory funnel, and let it stand to separate layers. Pour out the upper oil layer containing dinitriles, ie component A.

[0028] The aqueous solution of the water layer was added dropwise to it with a concentration of 50% H 2 SO 4 , keep stirring, let it fully mix, adjust the pH value of the system, and maintain it at 6.8~6.9. After the pH value is stable, let it stand for stratification, and use the same method to pour out the upper layer containing cyano acids, that is, the oil layer of component B. .

[0029] The aqueous solution of the water layer is continuously added dropwise to it with a concentration of 50% H 2 SO 4 , until the pH is 2~3, fully stirred and then cooled and centrifuged to obtain dibasic ac...

Embodiment 3

[0032] Weigh 200g of the ammoniated product containing cyano acid, add 800mL of deionized water at a temperature of about 40~50℃, slowly add ammonia water with a concentration of 25%, stir well, and adjust the pH of the system to 9~12 ,. Pour it into a 1500mL separatory funnel, and let it stand to separate layers. Pour out the upper oil layer containing dinitriles, ie component A.

[0033] The aqueous solution of the water layer was added dropwise to it with a concentration of 50% H 2 SO 4 , Stir constantly, let it fully mix, adjust the pH value of the system, maintain it at 6.9, wait for the pH value to stabilize and then separate into layers, use the same method to pour out the upper layer containing cyano acid substances, that is, the oil layer of component B.

[0034] The aqueous solution of the water layer is continuously added dropwise to it with a concentration of 50% H 2 SO 4 , until the pH is 2~3, fully stirred and then cooled and centrifuged to obtain dibasic ac...

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Abstract

The invention relates to a method for purifying long-carbon-chain cyanic acid products, belonging to the technical field of separation. The method comprises the following steps: mixing ammoniated products and water, then regulating pH value by using alkali, fully stirring, and standing for layering to obtain an upper oil layer as a component A, namely NC-R-CN; continuously dropwise adding dilute-acid solution into the remaining lower-layer aqueous solution, regulating PH of the solution, fully stirring, standing for layering, and collecting an upper-layer oil phase which is a component B, namely HOOC-R-CN; continuously dropwise adding dilute acid into the remaining lower-layer aqueous phase, regulating PH, fully stirring to fully precipitate all solids, cooling, and carrying out centrifugal separation to obtain a component C, namely HOOC-R-COOH. According to the separation method provided by the invention, long-carbon-chain cyanic acid product can be separated, especially 8-cyanooctanoic acid and 9-cyanononyl acid which are front intermediates of nylon 9 and nylon 10; and According to the method, the process is simple and reliable the repeatability is strong and the method is applicable to large-scale industrial application.

Description

technical field [0001] The invention relates to a separation method, in particular to a method for purifying long carbon chain cyano acid products, and belongs to the field of separation technology. 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 are no reports of nylon 9 and nylon 10 on the market at present, and its main reason is ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C253/34C07C255/19
CPCC07C253/34C07C255/19
Inventor 陈尚标沈俊毅胡瑞莉殷炼伟
Owner WUXI YINDA NYLON