Preparation method of ultraviolet absorbent UV-9

A technology of UV-9 and absorber, which is applied in the field of preparation of ultraviolet absorber UV-9, can solve the problems of high cost, uneven color, unfavorable for the next step, etc., and achieve the goal of reducing product cost and improving product yield Effect

Inactive Publication Date: 2019-02-15
XIANGYANG JINDACHENG FINE CHEM
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The purpose of the present invention is to overcome the defect in the prior art, provide a kind of preparation method of ultraviolet absorber UV-9, adopt water and methanol to mix and be mixed with low The concentrated methanol aqueous solution is used as a solvent, which solves the disadvantages of poor color and high viscosity of the UV-0 crude product obtained by using pure water as a solvent, which is not conducive to the next step, and solves the problem of low yield and low cost of UV-0 obtained by using methanol as a solvent. high disadvantage
In the process of synthesizing UV-9 from UV-0 and dimethyl sulfate (step 2), toluene is used as a solvent, sodium carbonate is used as an acid-binding agent, and PEG-400 is used as a catalyst, which solves the problem of uneven color of UV-9 products. Increased product yield and reduced product cost

Method used

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  • Preparation method of ultraviolet absorbent UV-9
  • Preparation method of ultraviolet absorbent UV-9
  • Preparation method of ultraviolet absorbent UV-9

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] 1. Synthesis of the first step:

[0026]

[0027] When synthesizing UV-9, first add 550kg of water and 100kg of methanol into the UV-0 reactor, start stirring and add 240kg of resorcinol, raise the temperature to 55°C, keep it warm for 40min, and then add 460kg of trichlorotoluene dropwise to the UV-9 -0 reaction kettle, the dropwise addition time is about 6 hours, then control the temperature at 55-60°C, keep the temperature for 5-6 hours, and take samples to check whether the reaction has reached the end point. After the reaction, the mother liquor was dried by centrifugation, and washed with water until neutral to obtain 470 kg of 2,4-dihydroxybenzophenone, namely UV-0 crude product.

[0028] 2. Synthesis of the second step:

[0029]

[0030] Then add 100kg of toluene, 470kg of UV-0 crude product obtained above, and 200kg of acid-binding agent sodium carbonate into the UV-9 reaction kettle, heat up and reflux to separate water until no water drops appear, cool...

Embodiment 2

[0032] 1. Synthesis of the first step:

[0033]

[0034] When synthesizing UV-9, first add 500kg of water and 100kg of methanol into the UV-0 reactor, start stirring and add 165kg of resorcinol, raise the temperature to 55°C, keep it warm for 40min, and then add 391kg of trichlorotoluene dropwise to the UV-9 -0 reaction kettle, the dropwise addition time is about 6 hours, then control the temperature at 55-60°C, keep the temperature for 5-6 hours, and take samples to check whether the reaction has reached the end point. After the reaction, the mother liquor was dried by centrifugation, and washed with water until neutral to obtain 321 kg of 2,4-dihydroxybenzophenone, namely UV-0 crude product.

[0035] 2. Synthesis of the second step:

[0036]

[0037] Then add 100kg of toluene, 321kg of UV-0 crude product obtained above, and 200kg of acid-binding agent sodium carbonate into the UV-9 reaction kettle, heat up and reflux to separate water until no water drops appear, cool...

Embodiment 3

[0039] 1. Synthesis of the first step:

[0040]

[0041]When synthesizing UV-9, first add 600kg of water and 150kg of methanol into the UV-0 reactor, start stirring and add 275kg of resorcinol, heat up to 55°C, keep warm for 40min, and then add 586kg of trichlorotoluene dropwise to the UV-9 -0 reaction kettle, the dropwise addition time is about 6 hours, then control the temperature at 55-60°C, keep the temperature for 5-6 hours, and take samples to check whether the reaction has reached the end point. After the reaction, the mother liquor was dried by centrifugation, and washed with water until neutral to obtain 535 kg of 2,4-dihydroxybenzophenone, namely UV-0 crude product.

[0042] 2. Synthesis of the second step:

[0043]

[0044] Then add 100kg of toluene, 535kg of UV-0 crude product obtained above, and 200kg of acid-binding agent sodium carbonate into the UV-9 reaction kettle, heat up and reflux to separate water until no water drops appear, cool down to 40°C, add...

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PUM

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Abstract

The invention provides a preparation method of an ultraviolet absorbent UV-9. The preparation method comprises following steps: step 1, water and methanol are added to a reaction kettle firstly, stirring is started, resorcinol is added, heating is performed, then benzotrichloride is dropwise added to the reaction kettle until the reaction is completed, mother liquor is subjected to centrifugal spin-drying, washing is performed until pH is neutral, and a UV-0 crude product is obtained; step 2, the UV-0 crude product, toluene and an acid-binding agent sodium carbonate are added to another reaction kettle, heating reflux is performed until no water drops appear, after cooling is performed, a catalyst PEG-400 is added, dimethyl sulfate is dropwise added, a mixture is heated after addition andsubjected to thermal insulation reaction until the components are reacted completely, water is added for washing, a product is left to stand for layering, organic phase is distilled under reduced pressure to remove an organic solvent methylbenzene, and a UV-9 crude product is obtained; step 3, the organic solvent is added to the UV-9 crude product for recrystallization, and a UV-9 finished productis obtained after centrifugation and drying. The problem of non-uniform color of the UV-9 product is solved, the product yield is increased, and the product cost is reduced.

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-9. Background technique [0002] 2-Hydroxy-4-methoxybenzophenone can be activated by ultraviolet light to form a quinone structure, and then restore it by emitting fluorescence, and the net result is absorption of ultraviolet light. Due to this characteristic of molecular structure, it is used as an ultraviolet absorber and has a trade name of UV-9. It can effectively absorb ultraviolet light from 190 to 400nm, and has the advantages of high absorption rate, non-toxicity, no teratogenic effect, and good light and thermal stability. As an important UV absorber, it has been used on polyvinyl chloride, polyacrylate, polyolefin and other materials and added to coatings based on polyacrylate, epoxy resin, polyurethane, etc. to improve its anti-aging performance. It is also used to prepare sunscreen cosmetics such as sun...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C49/84C07C45/64C07C49/83C07C45/00
CPCC07C45/008C07C45/64C07C49/83C07C49/84
Inventor 王清才张雪
Owner XIANGYANG JINDACHENG FINE CHEM
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