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A kind of synthetic method of benzotriazole compound

A technology of benzotriazoles and a synthetic method, applied in the field of synthesizing benzotriazoles, can solve the problems such as failure to avoid the use of lye, increase production cost, difficulty in post-processing, and achieve simplified post-processing process, Easy to recycle, low cost effect

Active Publication Date: 2018-02-09
TIANJIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But as with all the aforementioned methods, the use of lye has not been avoided
The use of a large amount of lye not only increases the production cost, but also brings great difficulties to the post-treatment of the reaction
If it is not handled properly, the discharge of a large amount of lye will cause serious environmental pollution, especially the pollution of water bodies

Method used

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  • A kind of synthetic method of benzotriazole compound
  • A kind of synthetic method of benzotriazole compound
  • A kind of synthetic method of benzotriazole compound

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Preparation of hydrogenation-solid base bifunctional catalyst (equal volume impregnation method):

[0030] The aqueous solution of platinum chloride and magnesium nitrate hexahydrate and the mixed carrier were impregnated in equal volumes for 12 hours to obtain a catalyst precursor (i.e. the carrier loaded with platinum chloride and magnesium nitrate hexahydrate). The mixed carrier was composed of Hβ molecular sieve and active oxidation Aluminum (the mass ratio of Hβ molecular sieve to activated alumina is 1:1), dried at 100°C for 24h, then calcined at 500°C for 4h; washed repeatedly with deionized water until the washing liquid no longer contained chloride ions, and then Dry at 100°C for 24 hours to obtain an oxidative hydrogenation-solid base dual-function catalyst; reduce at 350°C for 1 hour under 3MPa hydrogen pressure to obtain a hydrogenation-solid base dual-function catalyst. According to ICP-AES analysis, the mass content of hydrogenation active metal element pl...

Embodiment 2

[0033] A kind of synthetic method of benzotriazole compound (II-1), comprises the steps: the hydrogenation-solid base bifunctional catalyst that 40mL (15.23g) embodiment 1 prepares is packed in single tubular fixed-bed reactor , the inner diameter of the reactor is 14mm, and the pipe length is 650mm; the compound (purity is 98.43%) shown in the formula (I-1) is dissolved in 1,4-dioxane to obtain the compound shown in the formula (I-1) The mass concentration of the compound is 25% solution, the volume space velocity is 300h -1 The single-tubular fixed-bed reactor is continuously fed into the single-tubular fixed-bed reactor under certain conditions, and hydrogen is fed in, and heated so that the hydrogen pressure in the single-tubular fixed-bed reactor is 0.1MPa and the temperature is 150°C; the reaction liquid continues to flow from the single-tubular fixed-bed The lower end of the reactor flows out, and the reaction solution flowing out is cooled to room temperature, gas-liqu...

Embodiment 3

[0038] Preparation of hydrogenation-solid alkali bifunctional catalyst (secondary impregnation method):

[0039] The nickel nitrate aqueous solution, the potassium nitrate aqueous solution and the mixed carrier were impregnated by the second impregnation method, each time for 12 hours, a total of 2 times, to obtain the catalyst precursor (i.e. the carrier loaded with nickel nitrate and potassium nitrate), and the mixed carrier was made of HZSM- Composed of 5 molecular sieves and activated alumina, (the mass ratio of HZSM-5 molecular sieves to activated alumina is 9:1) dried at 130°C for 12 hours, then roasted at 500°C for 4 hours, washed repeatedly with deionized water into the washing liquid It no longer contains nitrate ions, and then dried at 130°C for 12 hours to obtain an oxidized hydrogenation-solid base dual-function catalyst; at 360°C and 0.1MPa hydrogen pressure for 5 hours, a hydrogenation-solid base dual-function catalyst was obtained. According to ICP-AES analysis,...

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Abstract

The invention discloses a synthetic method of a benzotriazoles compound. The synthetic method comprises the following steps: loading a bifunctional catalyst of hydrogenation-solid alkali into a fixed bed reactor; continuously leading a solution of a compound represented by the formula (I) into the fixed bed reactor, leading hydrogen, and performing heating; enabling the reaction liquid to continuously flow out from a lower end of the fixed bed reactor; cooling the effluent reaction liquid to the room temperature; performing gas-liquid separation, liquid filtration, and filtrate condensation to remove the solvent; and performing purification to obtain the benzotriazoles compound represented by the formula (II). The bifunctional catalyst of hydrogenation-solid alkali is adopted for catalytic hydrogenation to synthesize the benzotriazoles compound. The bifunctional catalyst has catalytic performance of solid alkali during catalytic hydrogenation, so that insufficient addition of alkali liquor is effectively avoided in the prior art. The bifunctional catalyst is high in catalytic activity and is convenient to recycle and reuse. Post-treatment of synthesizing the benzotriazoles compound is simplified, and the problem of environmental pollution resulting from post-treatment of the alkali liquor is effectively avoided. The synthetic method is efficient, and is low in cost and easy and simple to operate.

Description

technical field [0001] The invention relates to a method for synthesizing green and high-efficiency benzotriazole compounds. Background technique [0002] Benzotriazole compounds are an important class of light stabilizers, which are widely used in food packaging, polyolefins, photosensitive materials, polyester resins, coatings, especially automotive coatings and other synthetic materials. It has the advantages of good stability, small relative molecular weight, low toxicity, good compatibility with polymers, strong absorption of ultraviolet rays, and low volatility. [0003] At present, benzotriazole compounds are mainly obtained by reductive cyclization reaction of azo compounds containing nitro groups. Common cyclization methods mainly include zinc powder reduction method, hydrazine hydrate reduction method, alkali sulfide reduction method, catalytic hydrogenation method, hydrazine hydrate-zinc powder reduction method, glucose-zinc powder reduction method, sodium sulfid...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D249/20
CPCC07D249/20
Inventor 陈立功王博威司磊磊李阳闫喜龙
Owner TIANJIN UNIV
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