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Synthetic method of methyl salicylate

A technology for the synthesis of methyl salicylate, which is applied in the preparation of carboxylic acid esters, chemical instruments and methods, and the preparation of carboxylic acid salts. Corrosion, waste water" is less, the effect of process environmental protection

Pending Publication Date: 2021-02-09
江苏宏邦化工科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The main disadvantages of this method are as follows: 1. strong acid corrodes the equipment seriously; 2. the waste acid is difficult to treat, the amount of waste water is large, and the environment is seriously polluted; 3. due to the strong oxidation of concentrated sulfuric acid, many side reactions are caused, which affects the yield

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Put caustic soda 45g (1.1mol), water 90g, phenol 94g (1mol) into the autoclave successively, heat up, stir and react at 80°C-90°C for 2-3 hours, remove 45g of water under negative pressure (reuse), cool down To 50°C, add 500g of toluene, heat up, and use toluene to carry out the water (reuse the water taken out) to obtain a suspension of sodium phenate in toluene.

[0025] Continuously feed gasified carbon dioxide gas into the toluene suspension of sodium phenate to carry out carboxylation reaction. During the reaction, control the temperature of the kettle at 140°C to 150°C and the pressure at 0.6Mpa to 0.8Mpa. When the pressure of the kettle does not drop anymore, stop Pass through carbon dioxide, keep the pressure for 1 hour, finish the reaction, lower the temperature, and replace with nitrogen to obtain a suspension of sodium salicylate in toluene.

[0026] Add 3g of benzyltriethylammonium chloride to the above toluene suspension of sodium salicylate, stir to raise ...

Embodiment 2

[0029] Put caustic soda 49g (1.2mol), water 147g, phenol 94g (1mol) into the autoclave successively, heat up, stir and react at 80°C-90°C for 2-3 hours, remove 73g of water under negative pressure (reuse), cool down To 50°C, add 550g of toluene, heat up, and use toluene to carry out the water (reuse the water taken out) to obtain a suspension of sodium phenate in toluene.

[0030] Continuously feed gasified carbon dioxide gas into the toluene suspension of sodium phenate to carry out carboxylation reaction. During the reaction, control the temperature of the kettle at 140°C to 150°C and the pressure at 0.6Mpa to 0.8Mpa. When the pressure of the kettle does not drop anymore, stop Pass through carbon dioxide, keep the pressure for 1 hour, finish the reaction, lower the temperature, and replace with nitrogen to obtain a suspension of sodium salicylate in toluene.

[0031] Add 4g of benzyltriethylammonium bromide to the above toluene suspension of sodium salicylate, stir to raise ...

Embodiment 3

[0034] Put caustic soda 53g (1.1mol), water 210g, phenol 94g (1mol) into the autoclave successively, heat up, stir and react at 80℃~90℃ for 2~3 hours, remove 105g water under negative pressure (reuse), cool down To 50°C, add 600g of toluene, heat up, and use toluene to carry out the water (reuse the water taken out) to obtain a suspension of sodium phenate in toluene.

[0035] Continuously feed vaporized carbon dioxide gas into the toluene suspension of sodium phenate to carry out carboxylation reaction. During the reaction, control the temperature of the kettle at 140°C to 150°C and the pressure at 0.6Mpa to 0.8Mpa. When the pressure of the kettle does not drop anymore, stop Pass through carbon dioxide, keep the pressure for 1 hour, finish the reaction, lower the temperature, and replace with nitrogen to obtain a suspension of sodium salicylate in toluene.

[0036] Add 5g of tetrabutylammonium chloride to the above-mentioned toluene suspension of sodium salicylate, stir and r...

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Abstract

The invention discloses a synthesis method of methyl salicylate. The method comprises the following steps: preparing sodium phenolate by using caustic soda flakes and phenol as raw materials, carryingout carboxylation reaction on the obtained sodium phenolate and carbon dioxide gas to obtain sodium salicylate, reacting the obtained sodium salicylate with chloromethane gas under the action of a phase transfer catalyst to obtain a crude methyl salicylate product containing a toluene solvent, neutralizing and washing the crude methyl salicylate product, recovering the toluene solvent at normal pressure, and carrying out vacuum distillation to obtain a finished methyl salicylate product. According to the method, a strong acid catalyst is not used, so that the wastewater amount is greatly reduced, and the corrosion to equipment and the pollution to the environment are reduced. According to the method, equipment is not seriously corroded, the wastewater amount is small, and the process is more environmentally friendly.

Description

technical field [0001] The invention belongs to the technical field of organic synthesis, in particular to a method for synthesizing methyl salicylate. Background technique [0002] Methyl salicylate, the chemical name is methyl o-hydroxybenzoate, also known as wintergreen oil, methyl salicylate. Appearance is colorless oily liquid with sweet, wintergreen characteristic aroma and taste. Molecular formula is C 8 h 8 o 3 , the molecular weight is 152.15, the melting point is -8°C, and the boiling point at normal pressure is 222°C. It is soluble in organic solvents such as alcohol and ether, and almost insoluble in water. Methyl salicylate occurs naturally in wintergreen, birch, tuberose, carnation, tomato, cherry, strawberry. As a fragrance, methyl salicylate is widely used in daily flavors such as acacia, tuberose, ylang-ylang, sucrose, and gardenia, especially in toothpaste and oral cleansers, and also used in strawberries, grapes, In food flavors such as vanilla; as m...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C67/10C07C69/84
CPCC07C67/10C07C37/66C07C51/15C07C69/84C07C39/235C07C65/10
Inventor 陈文抗杨丽谢雨
Owner 江苏宏邦化工科技有限公司
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