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Chemosynthesis preparation method for methyl catechol

A technology of guaiacol and chemical synthesis, applied in ether preparation, organic chemistry, ester reaction to prepare ether, etc., can solve the problems of product quality decline, increased chance of veratrole, product loss, etc., and reduce the chance of generating tar , good controllability and selectivity, and the effect of offsetting the cost of separation

Inactive Publication Date: 2014-10-15
东营益盟盛药业有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] The traditional process uses 30% sodium hydroxide as the reaction raw material, which is an esterification reaction involving water. The reaction mechanism is mainly due to the free movement, collision and contact of ions in the solution. Because the raw material catechol is not ionized in water at low temperature The higher the temperature, the faster the molecular movement and the more intense the reaction, but due to the irregular molecular movement, the reaction is relatively passive, the conversion of catechol is relatively slow, and the process of forming guaiacol and veratrole is controllable Poor, correspondingly poor selectivity, the probability of generating the by-product veratrole is greatly increased, due to the slow conversion of raw materials, resulting in a longer reaction time, the guaiacol and veratrole generated at higher temperatures can be absorbed by the air Oxidative deterioration produces tar, which can be suspended in aqueous solution, and can be miscible with organic guaiacol, etc., resulting in difficulty in delamination between the organic phase and the water phase. The corresponding organic phase has more tar, and the water phase has more guaiacol. Too much, resulting in product loss, product quality decline, and too much tar in the generated water phase, the Glauber's salt generated after multi-effect distillation has no recovery value
Recycling will increase the production cost, and if it is not recycled, the amount of waste water will be large and the environment will be seriously polluted

Method used

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  • Chemosynthesis preparation method for methyl catechol

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Embodiment 1

[0033] Embodiment 1, the present invention is mainly made of the raw material of following preferred parts by weight:

[0034] A) Catechol Industrial grade >99.5% 500kg;

[0035] B) Dimethyl sulfate Industrial grade >99.5% 480 kg;

[0036] C) Sodium carbonate Industrial grade ≥99% 460kg;

[0037] D) Toluene Industrial grade 99.9% 105 kg;

[0038] E) Sodium hydroxide Industrial grade 99% 110 kg.

[0039] F) sulfuric acid industrial grade 60% 60kg

[0040] The chemical synthesis process of guaiacol of the present invention comprises the following production steps:

[0041] (1) Reaction process

[0042]Add 85kg of toluene and 460kg of sodium carbonate solution to the reaction kettle at room temperature, add 500kg of catechol while stirring, turn on steam heating after feeding, control the temperature at about 95°C for 0.5h, and simultaneously add 480kg of dimethyl sulfate The ester is poured into the head tank for later use. After the end of t...

Embodiment 2

[0049] Embodiment 2: A kind of chemical synthesis formula of guaiacol mainly contains the following raw materials to make:

[0050] A) Catechol Industrial grade >99.5% 450kg;

[0051] B) Dimethyl sulfate Industrial grade >99.5% 450 kg;

[0052] C) Sodium carbonate industrial grade ≥99% 420kg;

[0053] D) Toluene Industrial grade 99.9% 95 kg;

[0054] E) Sodium hydroxide Industrial grade 99% 100 kg.

[0055] F) sulfuric acid industrial grade 60% 50kg

[0056] The chemical synthesis process of guaiacol of the present invention comprises the following production steps:

[0057] (1) Reaction process

[0058] Add 75kg of toluene and 420kg of sodium carbonate solution to the reaction kettle at room temperature, add 450kg of catechol while stirring, turn on steam heating after feeding, control the temperature at about 95°C for 0.5h, and simultaneously add 450kg of dimethyl sulfate The ester is poured into the head tank for later use. After the end...

Embodiment 3

[0065] Embodiment 3: A kind of chemical synthesis formula of guaiacol mainly contains the following raw materials to make:

[0066] A) Catechol Industrial grade >99.5% 550kg;

[0067] B) Dimethyl sulfate Industrial grade >99.5% 500 kg;

[0068] C) Sodium carbonate Industrial grade ≥99% 480kg;

[0069] D) Toluene Industrial grade 99.9% 115 kg;

[0070] E) Sodium hydroxide Industrial grade 99% 120 kg.

[0071] F) sulfuric acid industrial grade 60% 100kg

[0072] The chemical synthesis process of guaiacol of the present invention comprises the following production steps:

[0073] (1) Reaction process

[0074] Add 95kg of toluene and 480kg of sodium carbonate solution to the reaction kettle at room temperature, add 550kg of catechol while stirring, turn on steam heating after feeding, control the temperature at about 95°C for 0.5h, and simultaneously add 500kg of dimethyl sulfate The ester is poured into the head tank for later use. After the e...

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Abstract

The invention relates to a chemosynthesis preparation method for methyl catechol. The preparation technology comprises the following steps: adding 95-115 parts of methyl benzene and 420-480 parts of soda in a reaction still at the room temperature; adding 450-550 parts of pyrocatechol while stirring; starting steam heating after batch charging is fulfilled; dripping 450-550 parts of methyl sulfate at the same time; then adding 100-120 parts of sodium hydroxide to conduct alkali washing; generating by-product crude methanol solution by generated tail gas; stopping stirring after insulation is fulfilled; still standing for 20 minutes to conduct delamination; putting water layer into a geosyncline; conducting extraction, exsolution and distillation on an organic phase to obtain the product. The chemosynthesis preparation method has the benefits that hydrous free radical reaction is replaced by anhydrous free radical reaction; benzenediol is adopted as a starting material; various raw materials are added to synthesize the product; the technology has the excellent characteristics of advanced technology, safety, reliability, low cost, cleanness, low pollution and the like; serious environmental pollution of an original technology is avoided.

Description

technical field [0001] The invention relates to a production process of guaiacol, in particular to a chemical synthesis preparation method of guaiacol. Background technique [0002] Guaiacol has a special sweet and slightly phenolic smell, and is an important intermediate in medicine and spices. Guaiac [0003] Wood phenol can synthesize a variety of anti-inflammatory and antibacterial drugs, and can also be directly used as a spice, or it can be synthesized into a variety of food [0004] Pharmaceutical and daily fragrances, such as artificial musk and vanillin, which are widely used in food, tobacco, wine and fragrance industries, etc., in recent years, more and more [0005] Quencus has made great breakthroughs in the research and application of high-end series products in the fragrance industry, and the application market has won a lot of attention. [0006] In short, guaiacol, as a pharmaceutical raw material with excellent performance and wide application, will ...

Claims

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Application Information

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IPC IPC(8): C07C43/23C07C41/16
CPCC07C41/16C07C43/23
Inventor 王光辉
Owner 东营益盟盛药业有限公司
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