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A kind of preparation method of ultraviolet absorber uv-328

A technology of UV-328 and absorbent, applied in the field of preparation of UV absorbent UV-328, can solve the problems of high cost, environmental pollution, low yield and the like

Active Publication Date: 2020-07-07
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-3', 5'-di-t-pentylphenyl) benzotriazole process synthesis method

Method used

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  • A kind of preparation method of ultraviolet absorber uv-328
  • A kind of preparation method of ultraviolet absorber uv-328
  • A kind of preparation method of ultraviolet absorber uv-328

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Embodiment 1

[0032] The invention prepares 2-(2'-hydroxyl-3',5'-di-t-pentylphenyl from o-nitrochlorobenzene through ammoniation, diazotization, coupling, one-step reduction, two-step reduction reaction and post-treatment process ) Benzotriazole products.

[0033] 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%.

[0034] Step 2. Preparation of 2-nitrodiazophenyl hydrochloride: Add 1mol of 2-nitroaniline, 3.2mol of 31% hydrochloric ...

Embodiment 2

[0039] The invention prepares 2-(2'-hydroxyl-3',5'-di-t-pentylphenyl from o-nitrochlorobenzene through ammoniation, diazotization, coupling, one-step reduction, two-step reduction reaction and post-treatment process ) Benzotriazole products.

[0040] 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%.

[0041] Step 2. Preparation of 2-nitrodiazophenyl hydrochloride: Add 1 mol of 2-nitroaniline, 3 mol of 5% hydrochloric acid and 500 ...

Embodiment 3

[0046] The invention prepares 2-(2'-hydroxyl-3',5'-di-t-pentylphenyl from o-nitrochlorobenzene through ammoniation, diazotization, coupling, one-step reduction, two-step reduction reaction and post-treatment process ) Benzotriazole products.

[0047] 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%.

[0048] Step 2, preparation of 2-nitrodiazophenyl hydrochloride: add 1mol of 2-nitroaniline, 4mol of 35% hydrochloric acid and 500ml of...

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Abstract

A preparation method of an ultraviolet absorber UV-328 is provided. The method includes o-nitrochlorobenzene ammoniation, diazotization, coupling, a first reduction step, a second reduction reaction and after-treatment to prepare a 2-(2'-hydroxyl-3',5'-di-tert-amyl phenyl) benzotriazole product. Ammonia water having a concentration of 10-25% is adopted for o-nitrochlorobenzene ammoniation, then diazotization is performed with nitrite to generate a diazonium salt, the diazotization does not need a strong acidic medium, and the ammonia water which is a byproduct of products of the company is comprehensively utilized, thus achieving low emission of three wastes and a low cost. Reduction for ring closing of an intermediate azo product adopts a two-step reduction process, avoiding a situation that a strong reductant directly reduces azo double bonds into amine, reducing impurity generation, increasing product purity and increasing the product yield.

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-328. Background technique [0002] 2-(2'-Hydroxy-3',5'-Di-t-pentylphenyl) benzotriazole is an excellent light stabilizer variety with the advantages of stable performance, low toxicity and strong ultraviolet absorption capacity , so it is used as a UV absorber, and has a trade name of UV-328. It can effectively absorb ultraviolet light. As an important ultraviolet absorber, it has been used in coatings based on polyethylene, polypropylene, polystyrene, polyvinyl chloride, polyester, epoxy resin, ABS resin and cellulose resin. Among them, it also has excellent light stabilizing effect in various coatings. [0003] When synthesizing 2-(2'-hydroxyl-3',5'-dipentylphenyl)benzotriazole, the following steps are usually adopted: Step 1, o-nitroaniline and nitrous acid (under strong acid medium) The diazonium salt is genera...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D249/20
CPCC07D249/20
Inventor 张雪
Owner XIANGYANG JINDACHENG FINE CHEM