Preparation method of 2-hydroxybenzophenone derivative base silane

A technology of hydroxybenzophenone and derivatives, applied in chemical instruments and methods, compounds of group 4/14 elements of the periodic table, organic chemistry, etc., can solve low absorption efficiency and limited content of benzophenone groups and other issues to achieve the effect of low product price, sufficient market supply and good color

Inactive Publication Date: 2016-01-27
SHAANXI RES DESIGN INST OF PETROLEUM CHEM IND
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  • Summary
  • Abstract
  • Description
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  • Application Information

AI Technical Summary

Problems solved by technology

However, the content of benzophenone groups in polymer compounds is limited, and the UV absorption efficiency is low

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Add 46Kg of toluene, 21.4Kg of 2,4-hydroxybenzophenone, 24.8Kg of 3-(2,3-epoxypropoxy)propyltrimethoxysilane in sequence in the reactor equipped with a condensation reflux device, 150r / Stir for 1 min to completely dissolve 2,4-hydroxybenzophenone, then increase the system temperature to 85-90°C, add 92.4g of sodium hydroxide powder, and keep the temperature for 5 hours. Then, lower the reaction temperature to below 50°C, add 50Kg of deionized water below 40°C, stir at 300r / min for 20 minutes, let stand for 30min, release the lower aqueous phase, and repeat the above water washing process 3 times. Then, transfer the upper layer into the still, under the condition of stirring at 200r / min, slowly reduce the pressure to a gauge pressure of 0.01MPa, gradually increase the temperature to 75°C, distill off the solvent toluene until no solvent is distilled, and discharge the material to obtain a thin Yellow viscous liquid, the corresponding peak of the epoxy group is confirmed...

Embodiment 2

[0021] Add 40Kg of benzene, 24.4Kg of 2,4'-dihydroxy-4-methoxybenzophenone, and 3-(2,3-epoxypropoxy)propylmethyl to the reactor equipped with a condensation reflux device. Dimethoxysilane 23.2Kg, stirred at 200r / min to completely dissolve 2,4'-dihydroxy-4-methoxybenzophenone, then raise the temperature of the system to 75-80°C, and add potassium hydroxide Powder 50g, insulation reaction 6h. Then, reduce the reaction temperature to below 40°C, add 40Kg of deionized water below 40°C, stir at 300r / min for 20 minutes, let stand for 30min, release the lower aqueous phase, and repeat the above water washing process 3 times. Then, transfer the upper layer into the still, under the condition of stirring at 200r / min, slowly reduce the pressure to a gauge pressure of 0.01MPa, gradually increase the temperature to 80°C, distill the solvent benzene until no solvent is distilled, and discharge the material to obtain a light Yellow viscous liquid, confirmed by H NMR spectrum that the corre...

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PUM

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Abstract

The invention relates to a preparation method of 2-hydroxybenzophenone derivative base silane. The method includes the following steps that a 2-hydroxybenzophenone derivative, epoxy silane and an appropriate quantity of solvent are added into a reaction kettle and stirred, the temperature is raised to 70-100 DEG C after the reactants are completely dissolved, an appropriate quantity of base catalyst is put into the reaction kettle, a heat preservation reaction is conducted for 3-8 h, then the reaction temperature is lowered to be below 50 DEG C, deionized water is added to perform washing several times, the solvent is separated out through reduced pressure distillation, and light yellow to amber thick liquid, namely, the 2-hydroxybenzophenone derivative base silane is obtained. The adopted raw materials are sufficient in the market, the product cost is low, and the obtained 2-hydroxybenzophenone derivative base silane has a good absorption effect on 280-400 nm ultraviolet light and can be reacted with the surfaces of metal, glass, wood, ceramic, silicate, plastic and other materials to form a film with ultraviolet light absorption and light curing functions.

Description

technical field [0001] The invention relates to the field of new organosilicon materials, in particular to a method for preparing a silane containing 2-hydroxybenzophenone groups and having functions of ultraviolet absorption and photocuring. Background technique [0002] A moderate amount of ultraviolet radiation can make people healthy, but excessive ultraviolet radiation is enough to cause disorders or loss of human body functions, such as eye damage, skin tanning, burns, and even skin cancer, or cause immune system disorders. In addition, ultraviolet radiation is also the main cause of photoaging. Long-term sunlight exposure accelerates the aging of cultural relics and historical monuments such as ancient buildings, stone carvings, wood carvings, calligraphy and paintings, and polymers. Anti-ultraviolet finishing of clothes, or coating a layer of materials with ultraviolet absorption function on the surface of ancient buildings and other cultural relics and polymer mater...

Claims

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Application Information

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IPC IPC(8): C07F7/18
Inventor 王前进史李刚张存社习娟黄方方
Owner SHAANXI RES DESIGN INST OF PETROLEUM CHEM IND
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