Low-polymerization type hindered amine light stabilizer and preparation method thereof

A technology of hindered amine light stabilizer and light stabilizer, which is applied in the manufacture of rayon, one-component polyolefin rayon, chemical characteristics of fibers, etc., can solve the problem of easy failure of effective groups, poor light stability and low volatility and other problems, to achieve the effect of low volatility, good compatibility and good purity

Active Publication Date: 2020-06-19
XIAN TECHNOLOGICAL UNIV
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  • Claims
  • Application Information

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Problems solved by technology

[0004] The object of the present invention is to provide a low-polymerization hindered amine light stabilizer and its preparation method, which overcomes the problems of poor light stability, easy volatilization and easy failure of effective groups in the prior art hindered amine light stabilizer. Products with better UV and thermal stability, low volatility, and better compatibility with polymer materials

Method used

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  • Low-polymerization type hindered amine light stabilizer and preparation method thereof
  • Low-polymerization type hindered amine light stabilizer and preparation method thereof
  • Low-polymerization type hindered amine light stabilizer and preparation method thereof

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preparation example Construction

[0029] The preparation method of above-mentioned hindered amine light stabilizer, synthetic route is:

[0030]

[0031] where R 1 for C 1 -C 18 straight-chain alkanes, C 5 -C 7 Naphthenic.

[0032] The preparation method of hindered amine light stabilizer of the present invention comprises the following steps:

[0033] Step 1, add light stabilizer 944, 2,4-bis(di-n-butylamino)-6-chloro-1,3,5-s-triazine, strong base and solvent to the autoclave; Stabilizer 944, 2,4-bis(di-n-butylamino)-6-chloro-1,3,5-s-triazine, strong base, solvent feed ratio is 1:0.2-0.3:0.3-0.6:0.8- 1.2.

[0034] Step 2, pressurize nitrogen to 1.5-2.0MPa, heat to 160-200°C for 3-8h.

[0035] Step 3: lower the temperature, filter, wash, and evaporate the solvent under reduced pressure to obtain intermediate 1.

[0036] Step 4, intermediate 1, water, catalyst (I), 30% hydrogen peroxide solution are mixed; Intermediate 1: 30% hydrogen peroxide feed ratio is 1:0.8-1.2; Catalyst (I) is stannous sulfat...

Embodiment 1

[0042] Put 280g of light stabilizer 944, 74g of 2,4-bis(di-n-butylamino)-6-chloro-1,3,5-s-triazine, 300mL of xylene and 100g of 20% sodium hydroxide solution into the autoclave , replaced with nitrogen several times, pressurized to 2MPa, stirred, and heated to 160°C for 3h. Cool down, filter the reaction solution, wash the organic phase several times with 10% sodium chloride solution, evaporate the solvent under reduced pressure, and obtain intermediate 1.

[0043] Mix 340g of intermediate 1 with 500mL of water, stir at 15°C for 10min, add 20g of sodium tungstate, add dropwise 340g of 30% aqueous hydrogen peroxide, control the temperature between 20°C and 25°C, and continue the heat preservation reaction for 24h. After the reaction, it was extracted three times with 1000 mL of ethyl acetate, and the solvent was removed in vacuo to obtain intermediate 2, which was stored at low temperature until use.

[0044] Dissolve 380g of intermediate 2 in 500mL of ethanol, add 116g of n-p...

Embodiment 2

[0046]Put 280g of light stabilizer 944, 74g of 2,4-di(di-n-butylamino)-6-chloro-1,3,5-s-triazine, 300mL of toluene and 100g of 20% sodium hydroxide solution into the autoclave, Nitrogen was replaced several times, pressurized to 2MPa, stirred, and heated to 160°C for 3h. Cool down, filter the reaction solution, wash the organic phase several times with 10% sodium chloride solution, evaporate the solvent under reduced pressure, and obtain intermediate 1.

[0047] Mix 340g of intermediate 1 with 500mL of water, stir at 15°C for 10min, add 18g of stannous sulfate, add dropwise 340g of 30% aqueous hydrogen peroxide, control the temperature between 20°C and 25°C, and continue the heat preservation reaction for 24h. After the reaction, it was extracted three times with 1000 mL of ethyl acetate, and the solvent was removed in vacuo to obtain intermediate 2, which was stored at low temperature until use.

[0048] Take 380g of intermediate 2 and dissolve in 500mL of ethanol, then add ...

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Abstract

The invention relates to a low-polymerization type hindered amine light stabilizer and a preparation method thereof, which overcome the problems of poor light stability, easy volatilization and easy failure of effective groups of hindered amine light stabilizers in the prior art, and the prepared product has better ultraviolet and thermal stability, low volatility and better compatibility with high polymer materials. The invention provides a mixed type low-alkalinity hindered amine light stabilizer. The structure of the mixed type low-alkalinity hindered amine light stabilizer is shown in thespecification, wherein R1 is C1-C18 straight-chain alkane and C5-C7 cycloalkane. The synthetic route of the preparation method of the hindered amine light stabilizer is as follows that: in the formula, R1 is C1-C18 straight-chain alkane and C5-C7 cycloalkane.

Description

Technical field: [0001] The invention relates to a light stabilizer and a preparation method thereof, in particular to an oligomerized hindered amine light stabilizer and a preparation method thereof. Background technique: [0002] Since its appearance in the 1970s, hindered amine light stabilizers have the characteristics of high efficiency, low toxicity, and low cost, and have become one of the best performance light stabilizers today. At the same time, they have good compatibility with polymer materials. Therefore, it is widely used in various polymer materials. A lot of research has been done on the development of new hindered amine light stabilizers at home and abroad. The performance and function of hindered amine light stabilizers have become more and more perfect, and the production cost has become cheaper. Many new high-performance hindered amine light stabilizers The agent was developed and put into the market, and its development mainly showed the development tre...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08K5/3492C07D401/14D01F6/46D01F1/10
CPCC07D401/14C08K5/34926D01F1/10D01F6/46
Inventor 金洗郎陈卫星周宏伟项瞻峰谢胜利刘旭
Owner XIAN TECHNOLOGICAL UNIV
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