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A kind of preparation method of ultraviolet absorber

An absorbent and ultraviolet technology, applied in the field of polymers, can solve the problems of low atom utilization, complicated operation, and environmental pollution, and achieve the effect of avoiding low atom utilization, high conversion rate, and high selectivity

Active Publication Date: 2021-09-03
GUANGDONG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] In view of this, the present invention provides a preparation method of an ultraviolet absorber, which solves the technical problems in the prior art of polluting the environment, complicated operation, low utilization rate of atoms and high cost

Method used

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Experimental program
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Effect test

Embodiment 1

[0033] Take 10g 16g of xylene, 3.4g of water, 3.4g of diethanolamine (DEA) and 0.5g of ruthenium phosphide (Ru-P) were loaded into a 100mL reactor, and hydrogen was passed through, and reacted at 1.0MPa and 60°C until the hydrogen pressure remained constant. After the reaction, the temperature was lowered to obtain a brown-black reaction solution. Filter the reaction solution, remove the catalyst, extract the organic phase, add absolute ethanol and ice water at a volume ratio of 1:1 overnight, and filter to obtain 2.5 g of light yellow crystals, namely the ultraviolet absorber.

[0034] figure 1 For the nuclear magnetic pattern of the azo intermediate that embodiment 1 makes, by figure 1 It can be seen that the single peak at δ=2.455ppm is -CH 3 The peak of three hydrogens on the top; the single peak at δ=12.25ppm is the peak of active hydrogen on -OH; the multi-peak at δ=6.99-8.15ppm is the peak of seven hydrogens on two benzene rings, which is consistent with the azo int...

Embodiment 2

[0037] Take 10g 16g of xylene, 3.4g of water, 3.4g of DEA additives and 1.0g of Ru-P were loaded into a 100mL reactor, hydrogen was passed through, and the reaction was carried out at 1.0MPa and 60°C until the hydrogen pressure remained constant. After the reaction, the temperature was lowered to obtain a brown-black reaction solution. Filter the reaction solution, remove the catalyst, separate the water layer, add absolute ethanol at a volume ratio of 1:1, and put it in ice water overnight, and filter to obtain 2.7g of light yellow crystals, that is, the ultraviolet absorber. The test results are shown in Table 1.

Embodiment 3

[0039] Take 10g 16g of xylene, 3.4g of water, 3.4g of DEA additives and 0.5g of Ru-P were loaded into a 100mL reactor, hydrogen was passed through until the hydrogen pressure remained constant, and the reaction was carried out at 1.5MPa and 60°C. After the reaction, the temperature was lowered to obtain a brown-black reaction solution. Filter the reaction liquid, remove the catalyst, extract to obtain the organic phase, add absolute ethanol at a volume ratio of 1:1, and spend the night in ice water, and filter to obtain 2.7 g of light yellow crystals, which are ultraviolet absorbers. The test results are shown in Table 1.

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Abstract

The invention belongs to the field of macromolecules, and in particular relates to a preparation method of an ultraviolet absorber. The preparation method of a kind of ultraviolet absorber provided by the present invention uses ruthenium phosphide as a catalyst, formula I and described ruthenium phosphide are reacted by catalytic hydrogenation to prepare ultraviolet absorber, and the structural formula of described ultraviolet absorber is formula II; Wherein, R=H or Cl; R 1 =(CH 3 ) 3 or H, R 2 =CH 3 , (CH 3 ) 3 or t‑C 8 h 17 . The preparation method of an ultraviolet absorber provided by the invention solves the technical problems of environmental pollution, complicated operation, low atom utilization rate and high cost in the prior art.

Description

technical field [0001] The invention belongs to the field of macromolecules, and in particular relates to a preparation method of an ultraviolet absorber. Background technique [0002] Ultraviolet absorber is a kind of light stabilizer, which can absorb ultraviolet rays in sunlight when added to polymer materials, protect polymer materials from ultraviolet radiation, and prevent photoaging of materials. In addition, it can also be treated on the surface of textiles to prepare textiles with UV protection function to avoid the damage of ultraviolet rays to human skin. [0003] At present, the methods for preparing ultraviolet absorbers at home and abroad mainly include chemical reduction method, hydrogen conversion reduction method, electrochemical reduction method and catalytic hydrogenation reduction method. The chemical reduction method has the most mature technology, but its waste residue and wastewater pollution are relatively serious, the utilization rate of atoms is lo...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D249/20
CPCC07D249/20
Inventor 赵杏方岩雄张维刚蔡晓兰
Owner GUANGDONG UNIV OF TECH
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