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Method for directly synthesizing phenyl salicylate from carbon dioxide and phenol

A technology of phenyl salicylate and carbon dioxide, applied in chemical instruments and methods, preparation of organic compounds, preparation of carboxylic acid esters, etc., can solve the problems of difficult recycling, long reaction time, environmental pollution, etc., and achieve low cost, Raw materials are easily available and the effect of reducing environmental pollution

Active Publication Date: 2017-08-25
CHINA PETROLEUM & CHEM CORP
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Problems solved by technology

[0003] The current synthetic method still has the shortcomings of long reaction time, low yield, and a large amount of waste acid and waste gas generated during the esterification process, difficult recycling, serious environmental pollution, etc.

Method used

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  • Method for directly synthesizing phenyl salicylate from carbon dioxide and phenol

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Experimental program
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Effect test

Embodiment 1

[0017] Add 50mmol phenol, 50mLCCl in 250mL reactor 4 , 150mmol methanol, 20mol% ZnFe 2 o 4 , pass 2.0MPa carbon dioxide into the reaction kettle to replace the air in the kettle three times, raise the temperature to 100°C, pass carbon dioxide into the kettle until the pressure in the kettle rises to 9.0MPa, continue stirring for 10.0h, stop stirring, and cool the reaction mixture To room temperature, qualitative analysis was carried out with gas chromatography-mass spectrometry, quantitative analysis was carried out with gas chromatography, and the yield of phenyl salicylate was 1.7%.

Embodiment 2

[0019] Add 50mmol phenol, 50mLCCl in 250mL reactor 4 , 25 mmol K 2 CO 3 , 40mol% ZnFe 2 o 4 , pass 2.0MPa carbon dioxide into the reaction kettle to replace the air in the kettle three times, raise the temperature to 125°C, feed carbon dioxide into the kettle until the pressure in the kettle rises to 12.0MPa, continue to stir the reaction for 6.0h, stop stirring, and cool the reaction mixture to At room temperature, qualitative analysis was carried out with gas chromatography-mass spectrometry, and quantitative analysis was carried out with gas chromatography. The yield of phenyl salicylate was 6.2%.

Embodiment 3

[0021] Add 50mmol phenol, 50mLCCl in 250mL reactor 4 , 20mol% ZnFe 2 o 4 , 16.7 mmol Et 3 N, pass 2.0MPa carbon dioxide into the reaction kettle to replace the air in the kettle three times, raise the temperature to 125°C, pass carbon dioxide into the kettle until the pressure in the kettle rises to 12.0MPa, continue to stir the reaction for 2.0h, stop stirring, and cool the reaction mixture To room temperature, qualitative analysis was carried out with gas chromatography-mass spectrometry, and quantitative analysis was carried out with gas chromatography. The yield of phenyl salicylate was 13.0%.

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Abstract

The invention relates to a method for synthesizing phenyl salicylate, in particular to a method for directly synthesizing phenyl salicylate from carbon dioxide and phenol. The method uses carbon dioxide and phenol as reactants, and reacts to generate phenyl salicylate under the action of a magnetic nano ferrite catalyst and an auxiliary agent. The synthesis method provided by the invention can directly use carbon dioxide and phenol as raw materials to synthesize phenyl salicylate, the process route is simple, the raw materials are easy to get, and the cost is low; carbon dioxide is used as a reactant to realize its chemical utilization and reduce environmental pollution, which has important advantages economic and social significance.

Description

technical field [0001] The invention relates to a method for synthesizing phenyl salicylate, in particular to a method for directly synthesizing phenyl salicylate from carbon dioxide and phenol. Background technique [0002] Phenyl salicylate, also known as Salol, is a commonly used ultraviolet absorber. It is often used for sun protection of plastic products, and can also be used as preservatives, antibacterial disinfectants, pharmaceuticals and organic synthesis. The synthetic method of phenyl salicylate is less at present, and reported synthetic method has phosphorus oxychloride as acyl chloride reagent, and salicylic acid and phenol are raw material synthetic method (Wang Jiyuan, Sun Xuejun, Li Pengtao, Ma Yunlei, Wang Mingqing, Kong Desheng, You Jin Mao, Journal of Qufu Normal University, 2009,35,82-84), sodium bisulfate, sodium bisulfate-sulfuric acid as catalysts to catalyze salicylic acid and phenol (Li Wenqi, Xiong Shuangxi, Science Technology and Engineering, 2012,...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C69/84C07C67/00
Inventor 达建文张荣召李留忠鲍春伟
Owner CHINA PETROLEUM & CHEM CORP
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