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Preparation method of ultraviolet light absorber UV-PS

A UV-PS, ultraviolet technology, applied in the direction of organic chemistry, etc., can solve the problem of low yield of benzotriazole ultraviolet absorbers, achieve high yield, reduce environmental pollution, and increase yield

Inactive Publication Date: 2016-08-24
启东金美化学有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] Yet, adopt the method in the reference document, the yield of the benzotriazole ultraviolet absorber that prepares is not high

Method used

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  • Preparation method of ultraviolet light absorber UV-PS
  • Preparation method of ultraviolet light absorber UV-PS

Examples

Experimental program
Comparison scheme
Effect test

example 1

[0034] Step S1, add 13.8g (0.1mol) of o-nitroaniline and 36.5g of 30% hydrochloric acid (0.3mol) into a 250ml three-necked flask with stirring, heat up to complete dissolution, add 40g of water, and cool down to below 0°C. Add 7.25g (0.105mol) sodium nitrite aqueous solution dropwise, keep warm for 2h after dripping, add 1g urea, eliminate excess sodium nitrite, filter to obtain diazonium salt solution;

[0035] Step S2. In a 500ml three-neck flask, add 50ml of toluene, add 2g of additives, add 15g (0.1mol) of p-tert-butylphenol, heat up to completely dissolve, then cool down to 15°C, dropwise add the aforementioned diazonium salt solution, and use Alkali controls the pH at 8, and keeps warm for 3 hours after dripping.

[0036] Step S3, heating up to evaporate toluene, and filtering to obtain 28.4 g (0.095 mol) of azo compound, with a yield of 95%;

[0037] Step S4, add 28.4g (0.095mol) of the above-mentioned azo compound, 10g (0.25mol) sodium hydroxide, 100ml water and 50ml ...

Embodiment 2

[0042] Step S1, add 13.8g (0.1mol) of o-nitroaniline and 36.5g of 30% hydrochloric acid (0.3mol) into a 250ml three-necked flask with stirring, heat up to complete dissolution, add 40g of water, and cool down to below 0°C. Add 10.4g (0.15mol) sodium nitrite aqueous solution dropwise, keep warm for 2h after dropping, add 1g urea, eliminate excess sodium nitrite, filter to obtain diazonium salt solution;

[0043]Step S2. In a 500ml three-neck flask, add 50ml of toluene, add 2g of additives, add 15g (0.1mol) of p-tert-butylphenol, heat up to completely dissolve, then cool down to 15-20°C, and dropwise add the aforementioned diazonium salt solution , use alkali to control the pH at 8-9, and keep it warm for 3 hours after dripping.

[0044] Step S3, heating up to distill toluene, and filtering to obtain 30.5 g (0.102 mol) of azo compound, with a yield of 95.1%;

[0045] Step S4, adding 30.5g (0.102mol) of the above azo compound, 10g (0.25mol) sodium hydroxide, 100ml water and 50ml...

Embodiment 3

[0050] Step S1, add 13.8g (0.1mol) of o-nitroaniline and 36.5g of 30% hydrochloric acid (0.3mol) into a 250ml three-necked flask with stirring, heat up to complete dissolution, add 40g of water, and cool down to below 0°C. Add 7.25g (0.105mol) sodium nitrite aqueous solution dropwise, keep warm for 2h after dripping, add 1g urea, eliminate excess sodium nitrite, filter to obtain diazonium salt solution;

[0051] Step S2. In a 500ml three-neck flask, add 50ml of toluene, add 2g of additives, add 15g (0.1mol) of p-tert-butylphenol, heat up to completely dissolve, then cool down to 15-20°C, and dropwise add the aforementioned diazonium salt solution , use alkali to control the pH at 8.5, and keep it warm for 3 hours after dripping.

[0052] Step S3, heating up to evaporate toluene, and filtering to obtain 28.4 g (0.095 mol) of azo compound, with a yield of 95%;

[0053] Step S4, add 28.4g (0.095mol) of the above-mentioned azo compound, 14g (0.25mol) potassium hydroxide, 100ml wa...

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Abstract

The invention discloses a preparation method of ultraviolet light absorber UV-PS as indicated in the formula (I). The preparation method comprises the steps of 1, mixing ortho-nitroaniline with hydrochloric acid, then adding sodium nitrite, and conducting a reaction for 1-3 hours with the temperature preserved; adding urea for a reaction, so that a diazonium salt solution is obtained; 2, mixing and dissolving first solvent, an auxiliary agent and tert-butylphenol, lowering the temperature, adding the diazonium salt solution, adding alkali, and preserving the temperature for 1-3 hours; 3, conducting purification for the first time on a mixed solution obtained in step 2, so that azo matter as indicated in the formula (II) is obtained; 4, mixing the azo matter, alkali and second solvent for a reaction, raising the temperature to 60-70 DEG C, adding glucose, conducting backflow for 2-4 hours, and adding acid; 5, conducting purification for the second time on a mixed solution obtained in step 4, so that an intermediate as indicated in the formula (III) is obtained; 6, mixing the intermediate, third solvent and an auxiliary agent for a reaction, raising the temperature to 80-85 DEG C, adding zinc powder, conducting a reaction for 2.5-3 hours, and adding adsorbent; 7, conducting purification for the third time on a mixed solution obtained in step 6, so that the ultraviolet light absorber UV-PS as indicated in the formula (I) is obtained. According to the preparation method of the ultraviolet light absorber UV-PS, a fractional-step method is adopted, reactant in each step can fully react, the yield of products of all steps is guaranteed, and the yield of a final product is remarkably raised.

Description

technical field [0001] The invention relates to the field of ultraviolet absorber synthesis, more specifically, it relates to a preparation method of ultraviolet absorber UV-PS. Background technique [0002] The ultraviolet absorber can effectively absorb ultraviolet light with a wavelength of 280-400nm in sunlight and fluorescent light sources, avoid its redox effect, and keep the ultraviolet absorber itself unchanged. It is a light stabilizer. Generally, UV absorbers are used in fields such as plastics, building finishes, automobile spray paints, post-printing and dyeing treatments, sunscreen cosmetics, and printing inks. Moreover, the ultraviolet absorber has the advantages of good thermal stability, immersion resistance, stable chemical properties, good miscibility and insoluble in water. [0003] Among them, the benzotriazole ultraviolet absorber can selectively absorb sunlight ultraviolet rays with a wavelength of 300-385nm to prevent damage to polymers, and it has hi...

Claims

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Application Information

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IPC IPC(8): C07D249/20C07D487/04
CPCC07D249/20C07D487/04
Inventor 周志强潘行平
Owner 启东金美化学有限公司
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