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Preparation method of 2-hydroxy benzophenone derivative-based silane

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

Inactive Publication Date: 2016-07-06
SHAANXI RES DESIGN INST OF PETROLEUM CHEM IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • 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

[0027] 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

[0029] 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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Abstract

The invention relates to a preparation method of 2-hydroxybenzophenone derivative silane, which comprises the following steps: adding 2-hydroxybenzophenone derivative, epoxy silane and an appropriate amount of solvent into a reaction kettle, stirring, After the reactants are completely dissolved, raise the temperature to 70-100°C, put in an appropriate amount of alkali catalyst, then keep the temperature for 3-8 hours, then lower the reaction temperature to below 50°C, add deionized water to wash several times, and distill off the solvent under reduced pressure. A light yellow to amber viscous liquid, namely 2-hydroxybenzophenone derivative silane, was obtained. The market of the raw material adopted in the present invention is sufficient, and the product cost is low, and the obtained 2-hydroxybenzophenone derivative silane has good absorption to the ultraviolet rays of 280nm to 400nm, and can be combined with metal, glass, wood, ceramics under mild conditions , silicate, plastic and other materials to react on the surface to form a film with UV 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
CPCC07F7/1804C07F7/1892
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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