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Preparation method of light stabilizer intermediate

A technology for light stabilizers and intermediates, applied in the field of preparation of light stabilizer intermediates, can solve the problems of easy migration of hindered amine molecules, poor compatibility with industrial solvents, intolerant of pesticides, etc., and achieve excellent polymer compatibility, Good compatibility, slow down aging and decomposition effect

Active Publication Date: 2019-12-24
宿迁联盛科技股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The invention solves the technical problems in the prior art that hindered amine molecules are easy to migrate, has poor compatibility with industrial solvents, is not resistant to pesticides, and is toxic, and provides a preparation method for a light stabilizer intermediate to solve the problems in the prior art. problems in

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  • Preparation method of light stabilizer intermediate
  • Preparation method of light stabilizer intermediate

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Experimental program
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Effect test

Embodiment 1

[0026] A preparation method of light stabilizer intermediate, comprising the following steps:

[0027] Add 100g of dichloromethane to the reaction flask, cool down to -20°C, add 11.3g of chloroacetyl chloride and 10.1g of triethylamine, add 1-octyloxy-2,2,6, 28.5g of 6-tetramethyl-4-piperidinol, after dropping, react at a temperature of 0-5°C for 2 hours. After the reaction, wash with water, separate the liquids, evaporate the organic layer to remove the solvent, and obtain a light yellow solid 2-chloro - (1-octyloxy-2,2,6,6-tetramethyl-4-oxy) acetate.

[0028] Add 100g of dichloromethane into the reaction flask, add the above solid 2-chloro-acetic acid (1-octyloxy-2,2,6,6-tetramethyl-4-oxyl) ester and 10.1g of triethylamine, Stir to dissolve the solid, and add 14.8 g of 4-amino-2,2,6,6-tetramethylpiperidine dropwise at a temperature of 15-20°C. After the drop, keep warm at 30-35°C for 2 hours. After the reaction, Wash with water, cool down, crystallize and centrifuge to obt...

Embodiment 2

[0030] A preparation method of light stabilizer intermediate, comprising the following steps:

[0031] Add 150g of dichloromethane to the reaction bottle, lower the temperature to -20°C, add 17.8g of chloroacetyl chloride and 16.0g of triethylamine, and add 1-octyloxy-2,2,6, 42.7g of 6-tetramethyl-4-piperidinol, after dropping, react at a temperature of 0-5°C for 3 hours. After the reaction, wash with water, separate the liquids, and evaporate the organic layer to remove the solvent to obtain a light yellow solid 2-chloro - (1-octyloxy-2,2,6,6-tetramethyl-4-oxy) acetate.

[0032] Add 150g of dichloromethane into the reaction flask, add the above-mentioned solid 2-chloro-acetic acid (1-octyloxy-2,2,6,6-tetramethyl-4-oxyl) ester and 16.0g of triethylamine, Stir to dissolve the solid, add 23.4g of 4-amino-2,2,6,6-tetramethylpiperidine dropwise under temperature control at 15-20°C, and keep warm at 35-40°C for 3 hours. After the reaction, Wash with water, cool down, crystallize ...

Embodiment 3

[0034] A preparation method of light stabilizer intermediate, comprising the following steps:

[0035] Add 200g of dichloromethane to the reaction flask, cool down to -15°C, add 29.4g of chloroacetyl chloride and 25.0g of triethylamine, add 1-octyloxy-2,2,6, 57.0g of 6-tetramethyl-4-piperidinol, after dropping, react at a temperature of 0-5°C for 3 hours. After the reaction, wash with water, separate the liquids, evaporate the organic layer to remove the solvent, and obtain a light yellow solid 2-chloro - (1-octyloxy-2,2,6,6-tetramethyl-4-oxy) acetate.

[0036] Add 200g of dichloromethane into the reaction flask, add the above solid 2-chloro-acetic acid (1-octyloxy-2,2,6,6-tetramethyl-4-oxyl) ester and 25.0g of triethylamine, Stir to dissolve the solid, add 31.2 g of 4-amino-2,2,6,6-tetramethylpiperidine dropwise under temperature control at 15-20°C, and keep warm at 40-45°C for 3 hours. After the reaction, Wash with water, cool down, crystallize and centrifuge to obtain a w...

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Abstract

The invention discloses a preparation method of a light stabilizer intermediate. The preparation method comprises the following steps: firstly, performing a reaction on 1-octyloxy-2,2,6,6-tetramethyl-4-piperidinol with chloroacetyl chloride under the action of a catalyst to generate (1-octyloxy-2,2,6,6-tetramethyl-4-oxy) 2-chloroacetate; then performing a reaction a reaction on the (1-octyloxy-2,2,6,6-tetramethyl-4-oxy) 2-chloroacetate with 4-amino-2,2,6,6-tetramethylpiperidine, and performing crystallization and centrifugation after the reaction product is qualified, thereby finally obtaining the solid (1- octyloxy-2,2,6,6-tetramethyl-4-oxy) 2-(2,2,6,6-tetramethyl-4-piperidineamino)-acetate; the preparation process of the light stabilizer intermediate is simple, the separation and purification process is simple and convenient, the reaction time is short, and the product yield can reach about 93%.

Description

technical field [0001] The invention relates to a preparation method of a light stabilizer intermediate, belonging to the field of preparation of light stabilizer intermediates. Background technique [0002] Light stabilizer is an additive of polymer products, it can shield or absorb the energy of ultraviolet rays, quench singlet oxygen and decompose hydroperoxide into inactive substances, etc. , can eliminate or slow down the possibility of photochemical reaction, prevent or delay the process of photoaging, so as to achieve the purpose of prolonging the service life of polymer products. [0003] Hindered amines are a class of organic amine compounds with steric hindrance, which have a good inhibitory effect on the photo-oxidative degradation of polymers and organic compounds, and are a class of light stabilizers with excellent performance. [0004] There are many hindered amine light stabilizers in the prior art. Traditional hindered amines have low molecular weight and ar...

Claims

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Application Information

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IPC IPC(8): C07D211/94C08K5/3435
CPCC07D211/94C08K5/3435
Inventor 祝君威杨光袁开锋
Owner 宿迁联盛科技股份有限公司