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Method for preparing homosalate

A technology of raw film powdered ester and methyl salicylate, applied in the field of daily chemical industry, can solve the problem of not giving the product HMS stereo information and the like

Active Publication Date: 2015-11-25
ANHUI SHENGNUOBEI CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Furthermore, the literature does not give stereo information about the obtained product HMS

Method used

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  • Method for preparing homosalate
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preparation example Construction

[0073] According to the method for preparing the original membrane loose ester provided by the invention, it has the following beneficial effects:

[0074] (1) After the isophorone hydrogenation reduction reaction is finished, the stereoselectivity of the product isophorol is cis:trans≤1:1, and the method of epimerization can be used to obtain the cis isomer Isophorol with a ratio of trans isomer greater than 85:15, which provides guarantee for the subsequent preparation of high-quality promembrane loose ester;

[0075] (2) Using the method of epimerization, any ratio of cis:trans>1:1 isophorol can be obtained, and the epimerization reaction does not need to use other catalysts, only after the reaction is completed It can be completed by properly adjusting the temperature and hydrogen pressure in the reactor, and the operation is simple and the effect is remarkable;

[0076] (3) The isophor alcohol prepared according to the method provided by the present invention has a purit...

Embodiment 1

[0083] (1) Add 2000kg isophorone and 14.0kg Ru / C (based on the total weight of Ru / C, containing Ru5.1wt% and water content 45.4%) in the hydrogenation reactor, close the hydrogenation reactor, and replace with nitrogen The air in the reactor was replaced three times with hydrogen, and the nitrogen in the reactor was replaced three times. The hydrogen pressure in the reactor was set at 0.8MPa, the stirring was started, and the temperature was raised to 80°C to start hydrogenation. Until no hydrogen was absorbed, samples were taken for GC analysis. The cis form is 33.27%, the trans form is 66.52%, the total content is 99.79%, cis form:trans form=0.5.

[0084] (2) Epimerization: Raise the hydrogen pressure in the reactor to 1.4MPa, raise the temperature in the reactor to 140°C, and take a sample after stirring for 5 hours. The cis form is 89.89%, the trans form is 9.84%, and the total content is 99.73% %, cis:trans=9.14.

[0085] (3) The temperature of the material in the reacto...

Embodiment 2

[0089] (1) in hydrogenation reactor, add 2000kg isophorone, embodiment 1 reclaims Ru / C catalyst 10.6Kg and 2.0Kg fresh Ru / C catalyst (based on Ru / C gross weight, wherein containing Ru5.1%, Moisture content 45.4%), close the hydrogenation kettle, replace the air in the kettle with nitrogen three times, and then replace the nitrogen in the kettle with hydrogen three times, set the hydrogen pressure in the kettle at 1.2MPa, start stirring, heat up to 110°C to start hydrogenation, Until the hydrogen is no longer absorbed, samples are taken for GC analysis, the cis form is 10.10%, the trans form is 89.68%, the total content is 99.78%, cis form:trans form=0.11.

[0090] (2) Epimerization: Raise the hydrogen pressure in the reactor to 1.6MPa, raise the temperature in the reactor to 150°C, and take a sample after stirring for 7 hours. The cis form is 90.35%, the trans form is 9.35%, and the total content is 99.70% %, cis:trans=9.66.

[0091] (3) Cool the material in the kettle to 70°...

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Abstract

The invention provides a method for preparing homosalate. The method comprises the steps that isophorone serves as raw materials, a hydrogenation reaction is performed under the action of a catalyst, then an epimerization reaction is performed, and 3,3,5-Trimethylcyclohexanol is prepared; a transesterification reaction is performed on the prepared 3,3,5-Trimethylcyclohexanol and methyl salicylate, and finally the homosalate is prepared. The method is easy and convenient to operate, green and environmentally friendly, and the prepared homosalate is high in quality, wherein the cis form content is larger than or equal to 85.0 percent, the trans form content is smaller than or equal to 15 percent, the total content is larger than or equal to 99.0 percent, the single impurity content (GC) is smaller than or equal to 0.1 percent, and the total impurity content (GC) is smaller than or equal to 0.5 percent.

Description

technical field [0001] The invention belongs to the technical field of daily chemical industry, and relates to a preparation method of an organic intermediate, in particular to a preparation method of sunscreen agent original film loose ester. Background technique [0002] Sunscreen agent HMS, the chemical name is 3,3,5-trimethylcyclohexyl salicylate, the CAS number is 118-56-9, the English name is Homosalate, and its structural formula is shown in the following formula I : [0003] [0004] HMS is a colorless transparent viscous liquid with a boiling point of 161-165°C / 12mmHg, a relative molecular mass of 262.34, and a relative density of 1.049-1.053g / mL (20°C). [0005] HMS is a kind of ultraviolet UVB sunscreen agent, which belongs to chemical sunscreen agent. It can absorb UVB295~315nm band. It has good compatibility with resin and is not colored. It is widely used in soft and rigid PVC and other plastics and nitrocellulose. As a light stabilizer in coatings such as...

Claims

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Application Information

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IPC IPC(8): C07C69/84C07C67/03C07C35/08C07C29/17
CPCC07C29/175C07C67/03C07C69/84C07C35/08
Inventor 刘启发王荣
Owner ANHUI SHENGNUOBEI CHEM TECH
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