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Efficient preparation method of methyl salicylate

A high-efficiency technology for methyl salicylate, applied in the field of high-efficiency preparation of methyl salicylate, can solve problems such as affecting processing efficiency and product quality, poor recycling, and low product purity, so as to improve processing efficiency and product quality. The effect of quality, short production cycle time, and shortened reaction time

Inactive Publication Date: 2016-05-25
ZHENJIANG GAOPENG PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Methyl salicylate in the prior art adopts the method of collecting the branches and leaves of the Rhododendronaceae plant Pleurotus chinensis, extracting the available wintergreen oil by steam distillation, or separating the water from the natural essential oil by means of fractionation. The method of methyl cylate has long processing time, low product purity and high cost, and is generally not used in industrialized production; if a chemical preparation method is used, it is esterified and refined with salicylic acid and methanol under the action of a sulfuric acid catalyst, and synthesized Catalytic effect, product separation, and purification are technical difficulties in this field, which affect processing efficiency and product quality. At the same time, there are also problems such as poor recycling and certain pollution.

Method used

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Examples

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Effect test

Embodiment 1

[0026] A kind of efficient preparation method of methyl salicylate, its preparation method is as follows:

[0027] (1) Pretreatment

[0028] ①Put diatomite in aqueous acetic acid solution, the volume ratio of diatomite to aqueous acetic acid solution is 1:1.2, the pH of the aqueous acetic acid solution is 3, soak for 5 hours, then pour the aqueous acetic acid solution, and diatom The soil is washed to a pH of 6.5 to make modified diatomite;

[0029] ② Stir and mix the modified diatomite, hydroxypropyl cellulose, carboxymethyl cellulose and water to obtain the total material, the modified diatomite, hydroxypropyl cellulose, carboxymethyl cellulose and water The mass ratio is 10:3:1:4, and then put into the extruder to make strips, dry the strips for 30 minutes, and control the drying temperature at 60°C; then put the strips into the granulator to make granules Particles with a diameter of 3mm were put into a muffle furnace and baked at 600°C for 2 hours to obtain diatomaceous...

Embodiment 2

[0041] A kind of efficient preparation method of methyl salicylate, its preparation method is as follows:

[0042] (1) Pretreatment

[0043] ① put diatomite into aqueous acetic acid solution, the volume ratio of diatomite to aqueous acetic acid solution is 1:1.3, the pH of the aqueous acetic acid solution is 3.6, soak for 5.2 hours, then pour the aqueous acetic acid solution, and diatom The soil is washed to a pH of 6.8 to make modified diatomite;

[0044] ② Stir and mix the modified diatomite, hydroxypropyl cellulose, carboxymethyl cellulose and water to obtain the total material, the modified diatomite, hydroxypropyl cellulose, carboxymethyl cellulose and water The mass ratio is 10:3:1:4, and then put into the extruder to make strips, dry the strips for 45min, and control the drying temperature at 73°C; then put the strips into the granulator to make granules Particles with a diameter of 3mm were put into a muffle furnace and baked at 400°C for 3 hours to obtain diatomite-...

Embodiment 3

[0056] A kind of efficient preparation method of methyl salicylate, its preparation method is as follows:

[0057] (1) Pretreatment

[0058] ① put diatomite into aqueous acetic acid solution, the volume ratio of diatomite to aqueous acetic acid solution is 1:1.4, the pH of the aqueous acetic acid solution is 3.5, soak for 5.1 hours, then pour the aqueous acetic acid solution, and diatom The soil is washed to a pH of 6.5 to make modified diatomite;

[0059] ② Stir and mix the modified diatomite, hydroxypropyl cellulose, carboxymethyl cellulose and water to obtain the total material, the modified diatomite, hydroxypropyl cellulose, carboxymethyl cellulose and water The mass ratio is 10:3:1:4, and then put into the extruder to make strips, dry the strips for 42min, and control the drying temperature at 76°C; then put the strips into the granulator to make granules Particles with a diameter of 5mm were put into a muffle furnace and baked at 500°C for 2.7 hours to obtain diatomit...

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Abstract

The invention relates to an efficient preparation method of methyl salicylate, comprising the following steps: (1) pretreatment: I, preparing modified kieselguhr; II, preparing kieselguhr load particles; III, taking the kieselguhr load particles, adding dicyclohexylcarbodiimide, 4-dimethylamino pyridine and ethyl alcohol, and preparing a solid composite catalyst; (2) synthesis reaction: adding salicylic acid and methyl alcohol into a reaction kettle, and putting in the solid composite catalyst to prepare reaction liquid; (3) product extraction and purification: recovering the solid composite catalyst, skimming to take an oil layer, washing by using a sodium carbonate solution, adding the oil layer into water for washing, collecting a fraction, and adding activated carbon for heating and decoloring, thus obtaining a fine product of the methyl salicylate. By adopting the efficient preparation method, the production efficiency and product quality of the methyl salicylate can be improved, meanwhile the recovery rate is increased, pollution is reduced, and production risk degree and production cost are lowered.

Description

technical field [0001] The invention relates to a high-efficiency preparation method of methyl salicylate, which belongs to the technical field of chemical production. Background technique [0002] Methyl salicylate is a colorless to pale yellow transparent liquid with a fragrance like wintergreen oil and can be used as a solvent and intermediate, such as the reaction of methyl salicylate with ammonia to produce salicylamide, which is used as an antipyretic and painkiller B Salicylamide itself is also an antipyretic and analgesic, which can be used in the manufacture of insecticides, fungicides, spices, paints, cosmetic inks, and fiber dyeing aids. [0003] Methyl salicylate in the prior art adopts the method of collecting the branches and leaves of the Rhododendronaceae Phytophthora japonica, extracting with steam distillation to obtain the wintergreen oil and then rectifying, or separating the water from the natural essential oil by means of fractionation The method of me...

Claims

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Application Information

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IPC IPC(8): C07C67/08C07C69/84B01J31/02
CPCB01J31/0241B01J31/0244B01J31/0254C07C67/08C07C69/84
Inventor 王成栋王成慧
Owner ZHENJIANG GAOPENG PHARMA
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