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Preparing method of ultraviolet absorber UV-329

A technology of UV-329 and absorbent, applied in the field of preparation of ultraviolet absorbent UV-329, can solve the problems of environmental pollution, high cost, low yield, etc., and achieve the effects of reducing the generation of impurities, low cost, and low three wastes

Active Publication Date: 2019-07-30
XIANGYANG JINDACHENG FINE CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0008] The purpose of the present invention is to solve the problems of low yield, high cost and environmental pollution in the prior art, and provide a 2-(2' with high yield, high purity, low cost, safe production process, and low discharge of three wastes. -Hydroxy-5'-tertoctylphenyl) benzotriazole process synthesis method

Method used

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  • Preparing method of ultraviolet absorber UV-329
  • Preparing method of ultraviolet absorber UV-329
  • Preparing method of ultraviolet absorber UV-329

Examples

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Effect test

Embodiment 1

[0033] The present invention prepares 2-(2'-hydroxyl-5'-tertoctylphenyl)benzotriphenylene from o-nitrochlorobenzene through ammoniation, diazotization, coupling, one-step reduction, two-step reduction reaction and post-treatment process azole products.

[0034] Step 1, the preparation of 2-nitroaniline: put 1mol of 2-nitrochlorobenzene and 20mol of 20% ammonia water into the pipeline type ammoniation reactor and perform the ammoniation reaction at 150~220°C and 12~20MPa for 30~ After 50 minutes, the residual ammonia in the system was sprayed to circulate and absorb the low-concentration ammonia water produced, and after adding part of the liquid ammonia, it continued to be used for the ammonification reaction. neutralize and recover ammonia in water), and obtain 2-nitroaniline product through cooling and crystallization, with a yield of ≥98.6% and a purity of ≥99.6%.

[0035] Step 2. Preparation of 2-nitrodiazophenyl hydrochloride: Add 1mol of 2-nitroaniline, 3-4mol of 31% hy...

Embodiment 2

[0040] The present invention prepares 2-(2'-hydroxyl-5'-tertoctylphenyl)benzotriphenylene from o-nitrochlorobenzene through ammoniation, diazotization, coupling, one-step reduction, two-step reduction reaction and post-treatment process azole products.

[0041] Step 1. Preparation of 2-nitroaniline: put 1mol of 2-nitrochlorobenzene and 22mol of 10% ammonia water into the pipeline ammoniation reactor, and perform ammoniation reaction at 150~220°C and 12~20MPa for 30~ After 50 minutes, the residual ammonia in the system was sprayed to circulate and absorb the low-concentration ammonia water produced, and after adding part of the liquid ammonia, it continued to be used for the ammonification reaction. neutralize and recover ammonia in water), and obtain 2-nitroaniline product through cooling and crystallization, with a yield of ≥98.3% and a purity of ≥99.2%.

[0042] Step 2. Preparation of 2-nitrodiazophenyl hydrochloride: Add 1 mol of 2-nitroaniline, 3 mol of 5% hydrochloric ac...

Embodiment 3

[0047] The present invention prepares 2-(2'-hydroxyl-5'-tertoctylphenyl)benzotriphenylene from o-nitrochlorobenzene through ammoniation, diazotization, coupling, one-step reduction, two-step reduction reaction and post-treatment process azole products.

[0048] Step 1. Preparation of 2-nitroaniline: put 1mol of 2-nitrochlorobenzene and 12mol of 25% ammonia water into a pipeline ammoniation reactor and perform ammoniation reaction at 150-220°C and 12-20MPa for 30- After 50 minutes, the residual ammonia in the system was sprayed to circulate and absorb the low-concentration ammonia water produced, and after adding part of the liquid ammonia, it continued to be used for the ammonification reaction. neutralize and recover ammonia in water), and obtain 2-nitroaniline product through cooling and crystallization, with a yield of ≥98.2% and a purity of ≥99.5%.

[0049] Step 2, preparation of 2-nitrodiazophenyl hydrochloride: add 1mol of 2-nitroaniline, 4mol of 35% hydrochloric acid a...

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Abstract

The invention provides a preparing method of an ultraviolet absorber UV-329. The preparing method comprises the following steps of conducting ammoniation, diazotization, coupling, first-step reduction, second-step reduction reaction and post-treatment on ortho-nitrochlorobenzene to prepare a 2-(2'-hydroxy-5'-octylphenyl)benzotriazole product. According to the preparing method, ortho-nitrochlorobenzene is ammonified by adopting ammonium hydroxide with the concentration of 10-25%, then is subjected to diazotization with nitrite to produce diazonium salt, no diazotization needs to occur under a strong acid medium, by-product ammonium hydroxide of existing products of a company is comprehensively utilized, low emission of three wastes is achieved, and the required cost is low; a two-step reduction method is adopted in a reduction ring closing process of intermediate azo products, the situation is avoided that a strong reduction agent directly reduces azo double bonds into amine, impurity production is reduced, and not only is the purity of the products increased but also the product yield is increased.

Description

technical field [0001] The invention relates to the technical field of substance synthesis, in particular to a preparation method of an ultraviolet absorber UV-329. Background technique [0002] Ultraviolet absorber 2-(2'-hydroxy-5'-tertoctylphenyl)benzotriazole (also known as UV-329), is a high-efficiency anti-aging additive with excellent performance, soluble in benzene, styrene , dichloromethane and cyclohexane, slightly soluble in alcohols, insoluble in water; can effectively absorb ultraviolet light at 270-380 nanometers; non-flammable, non-explosive, non-toxic, safe and harmless to use; widely used in PE, PVC, PP, PS, PC, polypropylene fiber, ABS resin, epoxy resin, resin fiber and ethylene vinyl acetate, etc., and can be used in packaging materials such as plastic containers and food packaging boxes, providing them with good light stabilization effect , hardly absorbs visible light, especially suitable for colorless, transparent and light-colored products. [0003] ...

Claims

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Application Information

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IPC IPC(8): C07D249/20
CPCC07D249/20
Inventor 张雪
Owner XIANGYANG JINDACHENG FINE CHEM
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