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Synthesis method for ultraviolet absorber UV-P

A UV-P and synthetic method technology, applied in the direction of organic chemistry, etc., can solve the problems of high cost, pollute the environment, etc., and achieve the effects of easy separation, economic benefits, and yield improvement.

Inactive Publication Date: 2012-05-02
淮安嘉诚高新化工股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, there are still problems such as polluting the environment and high cost

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Embodiment 1: Synthesize ultraviolet absorber UV-P according to the following steps

[0023] (1) Synthesis of 4-methyl-2-nitrosophenol

[0024] Add p-cresol (108 g, 1mol) and 500 mL each of toluene and ethanol to a 5 L three-necked flask, stir to dissolve, add 500 mL of 6 N hydrochloric acid, and cool to 0 in an ice bath. o C. Slowly add an aqueous solution (200 mL) of sodium nitrite (90 g, 1.3 mol) dropwise, keeping the temperature below 5 o C, the dropwise addition was completed and reacted for 1 hour. After the reaction was detected by TLC, the organic solvent was spin-dried, 500 mL of water was added, and extracted three times with 500 mL of ethyl acetate, the organic phases were combined, and spin-dried to obtain 4-methyl-2-methoxide Nitrophenol 123 g, yield 90%;

[0025] (2) Synthesis of 2-(1H-benzo[d][1,2,3]triazole-2(3H))-4-methylphenol

[0026] Add 4-methyl-2-nitrosophenol (123 g, 0.9 mol) into a 5 L three-necked flask, add 500 mL each of toluene and ethanol...

Embodiment 2

[0029] Example 2: Same as Example 1, wherein the molar ratio of p-cresol: sodium nitrite: o-phenylenediamine: sodium tungstate monohydrate is 1: 1.4: 1.0: 0.9, and the final yield is 82%.

Embodiment 3

[0030] Example 3: Same as Example 1, wherein the molar ratio of p-cresol: sodium nitrite: o-phenylenediamine: sodium tungstate monohydrate is 1:1.2:0.8:0.7, and the final yield is 80%.

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Abstract

The invention discloses a synthesis method for an ultraviolet absorber UV-P. According to the synthesis method, methylphenol, sodium nitrite, o-phenylenediamine, sodium tungstate monohydrate and a reaction solvent are taken as raw materials and are used to synthesize the ultraviolet absorber UV-P in a normal-pressure homogeneous phase system. By adopting a method for first cyclization and then oxidative dehydrogenation of 4-methyl-2-nitrosophenol and the o-phenylenediamine, the traditional azo intermediate mode is jumped out, the synthesis method is reasonable in process and easiness for separation, low-value resources are fully utilized to produce products with high economic value, the economic benefit of enterprises is improved, and environmental pollution is reduced.

Description

technical field [0001] The present invention relates to taking p-cresol, sodium nitrite, o-phenylenediamine and catalysts as raw materials to synthesize ultraviolet absorber UV-P [full name 2-(2′-hydroxyl-5′-methanol) in homogeneous system at normal pressure. phenyl) benzotriazole] method. [0002] The structural formula of the ultraviolet absorber UV-P compound is as follows: [0003] . Background technique [0004] With the expansion of the application field of polymer materials, the position of ultraviolet absorbers in the whole polymer additives has become more and more prominent. It is always the goal of the industry to seek new varieties and new structures of ultraviolet absorbers that are efficient, hygienic, cheap, and meet harsh processing and application conditions. UV-P raw materials have a wide range of sources and low prices. In addition to being directly used as a polymer stabilizer, this product is also widely used as a higher-grade stabilizer. UV-P is a...

Claims

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Application Information

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IPC IPC(8): C07D487/04
Inventor 石祖嘉曹建常夏士朋
Owner 淮安嘉诚高新化工股份有限公司
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