Process for synthesizing hindered amine light stabilizer 944

A hindered amine light stabilizer and synthetic process technology, applied in the direction of organic chemistry, can solve the problems of rising cost, increasing post-processing difficulty, and reducing product quality, so as to reduce the possibility, reduce post-processing difficulty, and reduce by-products Effect

Inactive Publication Date: 2018-10-09
宿迁联盛科技股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

These two methods all need to add excessive hexamethylenediamine piperidine to terminate the polymerization during the polymerization reaction, so a large amount of cyclic insolubles and small molecule products will be produced, which increases the difficulty of post-processing, reduces product quality, and increases costs

Method used

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  • Process for synthesizing hindered amine light stabilizer 944
  • Process for synthesizing hindered amine light stabilizer 944
  • Process for synthesizing hindered amine light stabilizer 944

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] A kind of concrete steps of the synthesis technique of hindered amine light stabilizer 944 are as follows:

[0034] (1) Pour 92.3g of cyanuric chloride into the flask, add 185g of xylene, and drop 64.5g of tert-octylamine solution at 10°C for 6 hours. After 5 hours of heat preservation, slowly add 100g of 20% sodium hydroxide solution, the temperature is controlled at about 10°C, the dropwise addition is completed in 2 hours, and then kept for 6 hours. After the reaction was finished, 322g of Intermediate 1 solution (containing 137g of Intermediate 1) was obtained by cooling down and washing with water.

[0035] (2) Take 129g of Intermediate 1 solution (containing 54.8g of Intermediate 1) and pour it into a flask, add 5.5g of water, react at 40°C for 6h, cool down, separate water, filter, and precipitate to obtain 50g of Intermediate 2.

[0036] (3) Take 193g of intermediate 1 solution (containing 82.2g of intermediate 1) and pour it into the autoclave, and add 82.2g o...

Embodiment 2

[0039] A kind of concrete steps of the synthesis technique of hindered amine light stabilizer 944 are as follows:

[0040] (1) Pour 92.3g of cyanuric chloride into the flask, add 370g of toluene, drop 68g of tert-octylamine solution at 30°C for 11 hours, and slowly add 120g of 32 % sodium hydroxide solution, the temperature is controlled at about 30°C, the dropwise addition is completed in 6 hours, and then kept for 4 hours. After the reaction, the intermediate 1 solution was obtained by lowering the temperature and washing with water.

[0041] (2) Pour 200g of Intermediate 1 solution (containing 55.2g of Intermediate 1) into a flask, add 50g of water, react at 60°C for 4 hours, cool down, separate water, filter, and remove solvent to obtain 50.3g of Intermediate 2.

[0042] (3) Take 300g of intermediate 1 solution (containing 82.8g of intermediate 1) and pour it into the autoclave, add 200g of 15% sodium hydroxide solution and 158g of hexamethylenediamine piperidine in seque...

Embodiment 3

[0045] A kind of concrete steps of the synthesis technique of hindered amine light stabilizer 944 are as follows:

[0046] (1) Pour 92.3g of cyanuric chloride into the flask, add 554g of toluene, and drop 71g of tert-octylamine solution at 50°C for 15 hours. After 1 hour of heat preservation, slowly add 150g of concentration It is a 40% sodium hydroxide solution, the temperature is controlled at about 50°C, the dropwise addition is completed in 8 hours, and then kept for 2 hours. After the reaction, the intermediate 1 solution was obtained by lowering the temperature and washing with water.

[0047] (2) Take 276.5g of Intermediate 1 solution (containing 54.2g of Intermediate 1) and pour it into a flask, add 271g of water, react at 80°C for 2 hours, cool down, separate water, filter, and precipitate to obtain 50g of Intermediate 2.

[0048] (3) Take 417.7g of intermediate 1 solution (including 83g of intermediate 1) and pour it into the autoclave, add 415g of 5% sodium hydroxi...

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Abstract

The invention relates to a process for synthesizing a hindered amine light stabilizer 944. The process comprises the following specific steps: adding cyanuric chloride into a solvent to be stirred anddissolved, dropping a tert-octylamine solution and stirring, maintaining the temperature after dropping completion, dropping a sodium hydroxide solution, maintaining the temperature after dropping completion, washing and filtering to obtain an intermediate 1 solution; mixing the intermediate 1 solution and water, maintaining the temperature, cooling, filtering and desolventizing to obtain an intermediate 2; sequentially adding a sodium hydroxide solution and hexamethylendiamine piperidine into the intermediate 1 solution, raising the temperature to 90-120 DEG C, maintaining the temperature for 0.5-2 hours, continuously heating, maintaining the temperature for 0.5-2 hours while raising the temperature by 5-15 DEG C each time, and maintaining the temperature for 5-15 hours after the solution is heated to 130-160 DEG C so as to obtain an intermediate 3 solution; adding the intermediate 2 into the intermediate 3 solution for stirring, maintaining the temperature, washing, filtering and desolventizing the reaction solution, thereby obtaining the hindered amine light stabilizer 944. According to the method disclosed by the invention, production of small-molecule products is reduced, by-products are reduced, and the product quality and yield are improved.

Description

technical field [0001] The invention relates to a synthesis process of hindered amine light stabilizer 944, which belongs to the field of light stabilizer preparation. Background technique [0002] The hindered amine light stabilizer 944 is one of the varieties with the best application performance among the light stabilizers in the world. It has low volatility, high thermal stability, good extraction resistance, good compatibility with resin and not easy to migrate, easy plastic molding and non-irritating use and other hot spots. [0003] Among the currently disclosed synthesis methods of hindered amine light stabilizer 944, there are mainly two kinds: two-step method and three-step method. The two-step method is to react cyanuric chloride with tert-octylamine to obtain intermediate 2-tert-octylamino-4,6-dichloro-1,3,5 triazine, which is intermediate 1, and then react with hexamethylenediamine Pyridine was subjected to high-pressure polymerization, and the temperature was...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D401/14
CPCC07D401/14
Inventor 娄凯项瞻波项瞻峰胡新利
Owner 宿迁联盛科技股份有限公司
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