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Composite solid catalyst for preparing methyl salicylate and preparation method thereof

A solid catalyst, methyl salicylate technology, applied in chemical instruments and methods, organic compound/hydride/coordination complex catalysts, physical/chemical process catalysts, etc., can solve problems affecting processing efficiency and product quality, catalysts The problems of poor catalytic effect and poor recycling rate can reduce the difficulty of sewage treatment, reduce the cost of sewage treatment, and facilitate recycling and utilization.

Inactive Publication Date: 2016-04-20
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 the chemical preparation method is used, it is formed by esterification and refining of salicylic acid and methanol under the action of a sulfuric acid catalyst, while The catalysts in the prior art have poor catalytic effect, increase the difficulty of the process for purification and separation, affect the processing efficiency and product quality, and also have problems such as poor recycling and certain pollution.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] A kind of preparation method of composite solid catalyst for preparing methyl salicylate, its preparation method is as follows:

[0033] (1) Preparation of modified composite soil particles

[0034] 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;

[0035] ②Put attapulgite in the hydrochloric acid aqueous solution, the volume ratio of the diatomite and the acetic acid aqueous solution is 1:1.4, the pH of the hydrochloric acid aqueous solution is 2, soak for 4.5 hours, then pour the hydrochloric acid aqueous solution, and water diatomite Wash until the pH is 7.0 to make modified attapulgite;

[0036] ③ Stir and mix 28 parts of modified diatomite, 15 parts of modified attapulgite, 9 parts of hydroxypropyl cellulose, 3 p...

Embodiment 2

[0040] A kind of preparation method of composite solid catalyst for preparing methyl salicylate, its preparation method is as follows:

[0041] (1) Preparation of modified composite soil particles

[0042] 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;

[0043] ② put attapulgite in hydrochloric acid aqueous solution, the volume ratio of described diatomite and acetic acid aqueous solution is 1:1.3, the pH of described hydrochloric acid aqueous solution is 2, soak for 4 hours, then pour out hydrochloric acid aqueous solution, water diatomite Wash until the pH is 6.9 to make modified attapulgite;

[0044] ③ Stir and mix 31 parts of modified diatomite, 17 parts of modified attapulgite, 7 parts of hydroxypropyl cellulos...

Embodiment 3

[0048] A kind of preparation method of composite solid catalyst for preparing methyl salicylate, its preparation method is as follows:

[0049] (1) Preparation of modified composite soil particles

[0050] 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;

[0051] ② put attapulgite in aqueous hydrochloric acid solution, the volume ratio of diatomite to aqueous acetic acid solution is 1:1.2, the pH of the aqueous hydrochloric acid solution is 3, soak for 5 hours, then pour the aqueous hydrochloric acid solution, diatomaceous earth with water Wash until the pH is 7.0 to make modified attapulgite;

[0052] ③ Stir and mix 25 parts of modified diatomite, 13 parts of modified attapulgite, 5 parts of hydroxypropyl cellulose, ...

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PUM

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Abstract

The invention relates to a composite solid catalyst for preparing methyl salicylate and a preparation method thereof. In the composite solid catalyst, the mass ratio of modified composite soil particles to dicyclohexylcarbodiimide to 4-dimethylaminopyridine is 20:9:8, wherein the modified composite soil particles are prepared from the following components in parts by mass: 20-35 parts of modified diatomite, 10-20 parts of modified attapulgite clay, 3-12 parts of hydroxy propyl cellulose, 1-4 parts of carboxymethylcellulose and 8-16 parts of water. The preparation method has the advantages of high catalyzing rate, convenience in recycling and utilization, contribution to reduction of the process difficulty, and increase of the production efficiency.

Description

technical field [0001] The invention relates to a composite solid catalyst for preparing methyl salicylate and a preparation method thereof, belonging 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 f...

Claims

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Application Information

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IPC IPC(8): B01J31/06B01J35/02C07C67/08C07C69/84
CPCC07C67/08B01J31/06B01J2231/49B01J35/50C07C69/84
Inventor 王成栋王成慧
Owner ZHENJIANG GAOPENG PHARMA
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