Preparation method for N-vinyl caprolactam capable of recycling raw materials

A technology of vinyl caprolactam and caprolactam, which is applied in the direction of organic chemistry, can solve the problems of difficult industrialization, low product purity, and numerous process steps, and achieve the effects of reducing solvent consumption, good solubility, and shortening reaction time

Active Publication Date: 2014-02-12
BEIJING THTD PHARMA TECH JOINT CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] In order to overcome the problems existing in the above-mentioned prior art, the present invention provides a kind of N-vinyl caprolactam preparation, purification and recycling of raw materials recycling preparation method, to solve the existing problems in the synthesis of N-vinyl caprolactam In the process of caprolactam, the material is easy to solidify, the reaction time is too long, the process operation is dangerous, and it is difficult to realize industrialization and solve the problems of many process steps, difficult control and low product purity in the existing purification of N-vinyl caprolactam. A method for recovering and reusing raw material caprolactam is provided

Method used

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  • Preparation method for N-vinyl caprolactam capable of recycling raw materials
  • Preparation method for N-vinyl caprolactam capable of recycling raw materials

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] 1. Take 800 kg of dried caprolactam (purity > 95%) and 16 kg of potassium hydroxide in the jet loop reactor, pass nitrogen at 90°C for 2 hours to discharge the air and moisture in the reactor, and close Reactor (keep a certain amount of nitrogen in the kettle), feed acetylene, the temperature is controlled at 130 ± 3 ° C, the reaction stops after 10 hours, and 906 kg of N-vinyl caprolactam with a content of 58% (GC) is obtained mother liquor.

[0039] 2. 906 kilograms of N-vinyl caprolactam mother liquors with a content of 58% (GC) obtained in step 1 are placed in a rectifying still of 1.5 tons, start rectifying after the closed system, and set the still temperature to be 150°C. The vacuum degree is 30mmHg, adjust the reflux ratio of the rectifying tower, and after the reflux at the top of the rectifying tower is stable for one hour, the distillate tends to be stable and start to collect products, GC monitoring, after collecting 355 kg of products with a purity of more ...

Embodiment 2

[0043] 1. Take 800 kilograms of dry raw material caprolactam (purity > 95%) and 16 kilograms of potassium hydroxide in the jet loop reactor, pass nitrogen at 100 ° C for 2 hours to discharge the air and moisture in the reactor, and close the reaction Still (keep a certain amount of nitrogen in the still), feed acetylene, the temperature is controlled at 100 ± 3 ° C, the reaction stops after 16 hours, and 902 kg of N-vinyl caprolactam crude product with a content of 56.6% (GC) is obtained mother liquor.

[0044] 2. Place 902 kilograms of N-vinyl caprolactam crude product mother liquor with a content of 56.6% (GC) obtained in step 1 in a 1.5-ton rectification kettle, start rectification after the closed system, and set the kettle temperature to 150°C , the vacuum degree is 30mmHg, adjust the reflux ratio of the rectifying tower, and after the reflux at the top of the rectifying tower is stable for one hour, the fraction tends to be stable and begins to collect products, GC monit...

Embodiment 3

[0048] 1. Take dry 800 kilograms of raw material caprolactam (purity > 95%) and 16 kilograms of potassium methylate in the jet loop reactor, pass nitrogen at 90 ° C for 2 hours to discharge the air and moisture in the reactor, and close the reactor (keep a certain amount of nitrogen in the still), feed acetylene, and the temperature is controlled at 150 ± 3° C., and the reaction stops in 8 hours to obtain 912 kg of N-vinyl caprolactam mother liquor with a content of 58.9% (GC).

[0049] 2. 912 kilograms of N-vinyl caprolactam mother liquors with a content of 58.9% (GC) obtained in step 1 are placed in a rectifying still of 1.5 tons, start rectifying after the airtight embodiment, and set the temperature of the still to be 150°C. The vacuum degree is 20mmHg, after one hour of reflux at the top of the kettle, the distillate tends to be stable and begins to collect products. GC monitors and collects 377 kg of products with a purity of more than 98.5%. After the purity is lower tha...

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Abstract

The invention relates to a preparation method for N-vinyl caprolactam capable of recycling raw materials, wherein the method for preparing high-purity N-vinyl caprolactam can save cost, is high in productivity and efficiency, is eco-friendly, and is suitable for large-scale industrialized production by the steps of synthesis, rectification, simple distillation and recovery.

Description

technical field [0001] The invention relates to a production method of N-vinyl caprolactam, in particular to a method for preparing high-purity N-vinyl caprolactam by recycling recycled raw materials, rectifying and washing. Background technique [0002] Both N-vinylpyrrolidone and N-vinylcaprolactam belong to vinyl compounds, such as N-vinylcaprolactam (NVCL) (cas#: 2235-00-9) shown in (1) due to its molecular The presence of active vinyl makes it an important organic intermediate. [0003] [0004] N-vinylcaprolactam homopolymer or graft copolymerization with other monomers such as glucose or dextran can obtain water-soluble temperature-sensitive polymer materials. When the ambient temperature is higher than its phase transition temperature, its aqueous solution will undergo thermal settlement, and the structure of polymer aggregates will change. Studies have shown that poly N-vinyl caprolactam (PNVCL) is a temperature sensitive polymer with low critical phase transit...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D223/10
Inventor 王红平
Owner BEIJING THTD PHARMA TECH JOINT CO LTD
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