Preparation method of anti-yellowing agent HN-150

An anti-yellowing agent and solvent technology, which is applied in the field of chemical intermediate technology, can solve the problems of low product purity, difficult recovery of solvents, and easy environmental pollution, and achieve the effects of high purity, low equipment requirements, and low price

Inactive Publication Date: 2014-11-19
SHAOXING UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the synthesis process of spandex anti-yellowing agent is costly, the solvent is difficult to recycle, it is easy to pollute the environment, and the purity of the obtained product is not high

Method used

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  • Preparation method of anti-yellowing agent HN-150

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preparation example Construction

[0020] The invention provides a preparation method of spandex anti-yellowing agent HN-150, comprising the following steps:

[0021] a. respectively dissolve unsymmetrical dimethylhydrazine and diphenylmethane diisocyanate in the organic solvent under the state of stirring; then mix the two and continue to stir the reaction;

[0022] b. After the reaction finishes, filter the mixed solution in a;

[0023] c. Dry the solid obtained by filtering in b.

[0024]

Embodiment 1

[0027] In a 2L three-necked flask, mix 66.0g of unsymmetrical dimethylhydrazine in 1000mL of ethyl acetate. Slowly add 125.0 g of diphenylmethane diisocyanate into the three-necked flask in batches. After the addition was complete, stirring was continued for 2 hours. The reaction solution was suction-filtered to obtain a crude product with a wet weight of about 360 g. The crude product obtained above was dried in an oven to obtain about 175.0 g of white powder with a yield of 92% (the purity was 97% as detected by HPLC).

[0028] The ethyl acetate in the above-mentioned filtrate is distilled again, and the ethyl acetate obtained can continue to be reused.

Embodiment 2

[0030] In a 1000mL three-necked flask, mix 100.0g of diphenylmethane diisocyanate in 600mL of ethyl acetate. Mix 53.0g of unsymmetrical dimethylhydrazine in 160mL of ethyl acetate, and slowly add it into the three-necked flask. After the addition was complete, stirring was continued for 2 hours. The reaction solution was suction-filtered to obtain a crude product with a wet weight of about 280 g. The crude product obtained above was dried in an oven to obtain about 140.0 g of white powder with a yield of 92% (the purity was 97% as detected by HPLC).

[0031] The ethyl acetate in the above-mentioned filtrate is distilled again, and the ethyl acetate obtained can continue to be reused.

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PUM

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Abstract

The invention provides a preparation method of an anti-yellowing agent HN-150. The preparation method comprises the following steps: respectively dissolving unsymmetrical dimethylhydrazine and diphenyl methane diisocyanate in an organic solvent while stirring, mixing, filtering, washing, drying and the like to obtain a final product. The preparation method provided by the invention has the advantages that the operation is simple, raw materials are low in price, a process is simple and convenient, the environmental pressure is small, the product is high in yield and purity, and the like.

Description

technical field [0001] The invention relates to a preparation method of an anti-yellowing agent HN-150, which belongs to the technical field of chemical intermediates. Background technique [0002] The full name of polyurethane is polyurethane. It has a wide range of uses and is closely related to our lives. For example, it is widely used in industries such as footwear, clothing, plastics, adhesives and coatings. The spandex anti-yellowing agent is an indispensable auxiliary material in the production of polyurethane. It can be used to prevent the yellowing of polyurethane. For example, it is necessary to add anti-yellowing agent in the production of polyurethane such as spandex fiber, synthetic leather and artificial leather. At present, the main anti-yellowing agents for spandex mainly include anti-yellowing agent 1,6-hexamethylene-bis(N,N-dimethylsemicarbazide) (HN-130) and anti-yellowing agent bis(N,N-di Methylhydrazideamino-4-phenyl)methane (HN-150), etc., are also use...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C281/06
Inventor 齐陈泽杨震
Owner SHAOXING UNIVERSITY
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