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Method for continuously synthesizing isooctyl salicylate in micro-channels

A technology of isooctyl salicylate and microchannels is applied in the preparation of carboxylate, chemical instruments and methods, preparation of organic compounds, etc. The effect of reaction efficiency, fast mass transfer, and easy availability of raw materials

Inactive Publication Date: 2020-01-07
JIANGSU ZIQI CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Similar to the usual concentrated sulfuric acid catalyzed esterification process, this process also has problems such as serious corrosion of production equipment and large environmental pollution, and generally the produced products have a darker color
Although many other catalysts for synthesizing isooctyl salicylate have been found, mainly including JPC-1 solid acid, solid superacid TiO 2 / SO 4 2- and sodium methoxide, etc., although they all have a higher conversion rate of salicylic acid, there are still disadvantages such as high cost, cumbersome production process, and complicated post-treatment.

Method used

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  • Method for continuously synthesizing isooctyl salicylate in micro-channels
  • Method for continuously synthesizing isooctyl salicylate in micro-channels

Examples

Experimental program
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Effect test

Embodiment 1

[0023] Weigh 138g (1mol) salicylic acid and dissolve it in an appropriate amount of xylene; get 390g (3mol) isooctanol (2-ethylhexanol) and dissolve it in an equal amount of xylene, and add 10g p-toluenesulfonic acid as a catalyst, After fully dissolving, the two solutions were simultaneously pumped into the microchannel with a high-pressure constant-flow pump, maintaining a constant flow rate, and continuously reacting at a temperature of 150 °C. , saturated sodium carbonate solution, washed with distilled water at 65°C, then dried with anhydrous sodium sulfate, and suction filtered to obtain a mixed solution. Then use a vacuum pump to distill under reduced pressure, steam out isooctyl alcohol and the solvent for recycling, and finally collect the fraction at 123 ° C to obtain isooctyl salicylate, a colorless or light yellow transparent oily liquid, the yield can reach 96%, and the gas phase purity is 99%.

Embodiment 2

[0025] Take 138g (1mol) salicylic acid and dissolve it in an appropriate amount of xylene; take 390g (3mol) isooctanol (2-ethylhexanol) and dissolve it in an equal amount of xylene, and add 15g p-toluenesulfonic acid as a catalyst, After fully dissolving, the two solutions were simultaneously pumped into the microchannel with a high-pressure constant-flow pump, maintaining a constant flow rate, and continuously reacting at a temperature of 150 °C. , saturated sodium carbonate solution, washed with distilled water at 65°C, then dried with anhydrous sodium sulfate, and suction filtered to obtain a mixed solution. Then use a vacuum pump to depressurize distillation, steam out isooctanol and the solvent for recycling, and finally collect the fraction at 123 ° C to obtain isooctyl salicylate, a colorless or light yellow transparent oily liquid, the yield can reach 94%, and the gas phase purity is 99%.

Embodiment 3

[0027] Weigh 138g (1mol) salicylic acid and dissolve it in an appropriate amount of xylene, take 390g (3mol) isooctanol (2-ethylhexanol) and dissolve it in an equal amount of xylene, and add 10g p-toluenesulfonic acid as a catalyst, After fully dissolving, the two solutions were simultaneously pumped into the microchannel with a high-pressure constant-flow pump, maintaining a constant flow rate, and reacting continuously at a temperature of 160 °C. , saturated sodium carbonate solution, washed with distilled water at 65°C, then dried with anhydrous sodium sulfate, and suction filtered to obtain a mixed solution. Then use a vacuum pump to distill under reduced pressure, steam out isooctyl alcohol and the solvent for recycling, and finally collect the fraction at 123 ° C to obtain isooctyl salicylate, a colorless or light yellow transparent oily liquid, the yield can reach 91%, and the gas phase purity is 99 %.

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Abstract

The invention discloses a method for continuously synthesizing isooctyl salicylate in micro-channels. According to the method, salicylic acid and isooctyl alcohol are taken as raw materials, p-toluenesulfonic acid is taken as a catalyst, isooctyl salicylate is synthesized in micro-channels, and a triangular inner cross toe type micro-reactor is adopted. The width and the depth of the adopted micro-channels are small, and range from dozens of microns to hundreds of microns, so that the diffusion distance between reactants is greatly shortened, the mass transfer speed is high, and the reactantscan be fully mixed and reacted in a short time in the flowing process. According to the invention, micro-reaction technology is introduced into synthesis of isooctyl salicylate, so that continuous preparation of isooctyl salicylate is realized. By introducing the micro-reaction technology, the reaction operation is simple, the selectivity and yield of products are high, and the method has a wide industrial development prospect.

Description

technical field [0001] The invention relates to a method for continuously synthesizing isooctyl salicylate in a microchannel, and belongs to the technical field of microfluidics and organic synthesis. Background technique [0002] Isooctyl salicylate, also known as -2-ethylhexyl salicylate, is an important chemical product with a slightly aromatic odor. It is widely used in daily chemical, pharmaceutical and other industries. It is also used as an organic solvent and Organic synthesis intermediate is a product with broad prospects and great development value. At present, the industrial synthesis of isooctyl salicylate mainly uses salicylic acid and isooctanol as raw materials, and is directly catalyzed by concentrated sulfuric acid as a catalyst. Similar to the usual concentrated sulfuric acid catalyzed esterification process, this process also has problems such as serious corrosion to production equipment and large environmental pollution, and generally the products produc...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C67/08C07C69/84
CPCC07C67/08C07C69/84
Inventor 李斌栋许洪训
Owner JIANGSU ZIQI CHEM TECH
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