CN105669444A - Preparation method of green environment-friendly methyl salicylate - Google Patents
Preparation method of green environment-friendly methyl salicylate Download PDFInfo
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- CN105669444A CN105669444A CN201511013000.6A CN201511013000A CN105669444A CN 105669444 A CN105669444 A CN 105669444A CN 201511013000 A CN201511013000 A CN 201511013000A CN 105669444 A CN105669444 A CN 105669444A
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/08—Preparation of carboxylic acid esters by reacting carboxylic acids or symmetrical anhydrides with the hydroxy or O-metal group of organic compounds
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Abstract
The invention provides a preparation method of green environment-friendly methyl salicylate. The preparation method includes the steps of weighing raw materials, preheating the raw materials, performing primary stirring and secondary stirring, and heating the raw materials. The preparation method is convenient to carry out and is simple in operations. Firstly, salicylic acid is reacted with methanol with addition of a catalyst for catalyzing the reaction; secondly, the reaction products are washed with sodium carbonate; and finally, a finish product is obtained through high-temperature heating. The preparation method is green and environment-friendly, is economical and reliable, is energy-saving and low-cost, is improved in reaction extent and is reduced in reaction time, has convenience on recycling utilization, reduces treatment difficulty of wastewater, reduces wastewater treatment cost, improves total safety, is short in production period and satisfies user demands.
Description
Technical field
The present invention relates to methyl salicylate technical field, the preparation method particularly relating to a kind of environmental type methyl salicylate.
Background technology
Methyl salicylate has another name called wintergreen oil, birch oil, and colourless have the special odor of medicinal herbs to weak yellow liquid, and taste is sweet and peppery, fusing point-8.6 DEG C, boiling point 218～224 DEG C, local external use's rubefacient. There is local irritant effect, can promoting local blood circulation, external or local are embrocated and can be produced the irritant reaction such as cutaneous vasodilation, the colour of skin be rubescent, and reflexive ground affects the skin of corresponding site, muscle, nerve and joint, play detumescence, antiinflammatory and analgesic activity, also have antipruritic effect. For spraining, dampening, lumbago, myalgia, neuralgia, antipruritic. But existing methyl salicylate produces, and there is long processing time, product purity is low, simultaneously relatively costly, reclaims profit recycling degree poor, affects natural environment, can not meet the demand of user.
Summary of the invention
The preparation method that it is an object of the invention to provide a kind of environmental type methyl salicylate, solves existing methyl salicylate and produces, there is long processing time, product purity is low, simultaneously relatively costly, reclaims profit recycling degree poor, affect natural environment, the problem that can not meet the demand of user.
The purpose of the present invention can be achieved through the following technical solutions;
A kind of preparation method of environmental type methyl salicylate, its preparation method is as follows:
(1) raw material is weighed: weigh following component by weight and include salicylic acid 30-50 part, water 300-500 part, methanol 60-80 part, catalyst 5-15 part, sodium carbonate 15-25 part, concentrated sulphuric acid 50-70 part and zeolite 1-3 part;
(2) preheating: first think that adding water in bottle is heated, until after water temperature rises to 55 DEG C-65 DEG C, being sequentially added into salicylic acid and methanol stirring 20-30min, obtaining mixed liquor A;
(3) first time stirring: after the temperature in mixed liquor A rises to 80 DEG C-100 DEG C, after adding concentrated sulphuric acid stirring 45-65min, adds catalyst stirring 10-20min, obtains mixture B;
(4) second time stirring: after the temperature of mixture B rises to 105 DEG C-115 DEG C, after adding sodium carbonate stirring 55-75min, obtains mixed liquor C;
(5) heating: after adding zeolite in mixed liquor C, at 210 DEG C-220 DEG C, at the uniform velocity stir 30-45min, finished product can be obtained.
The preparation method of above-mentioned a kind of environmental type methyl salicylate, wherein, described catalyst is that toluenesulfonic acid mixes together with water, and the ratio of described toluenesulfonic acid and water is 1:5, is added to the water by toluenesulfonic acid under room temperature again and stirs 15-25min.
The beneficial effect of this programme:
The preparation method of a kind of environmental type methyl salicylate provided by the invention, including weighing raw material, preheating, first time stirring, second time stirring and heating five steps, configuration is convenient, simple to operate, first react with salicylic acid and methanol, add catalyst and carry out catalysis, wash utilizing sodium carbonate, finished product is obtained finally by high-temperature heating, environmental protection, economical reliable, save the energy, less costly, more original preparation method extent of reaction improves, response time shortens, simultaneously facilitate recycling, reduce sewage disposal difficulty, reduce cost of sewage disposal, improve the safety of entirety, production cycle is shorter, more can meet the demand of user.
Detailed description of the invention
Embodiment 1: the preparation method of a kind of environmental type methyl salicylate, its preparation method is as follows:
(1) raw material is weighed: weigh following component by weight and include salicylic acid 30 parts, 300 parts of water, methanol 60 parts, catalyst 5 parts, sodium carbonate 15 parts, concentrated sulphuric acid 50 parts and 1 part of zeolite;
(2) preheating: first think that adding water in bottle is heated, until after water temperature rises to 55 DEG C, being sequentially added into salicylic acid and methanol stirring 20min, obtaining mixed liquor A;
(3) first time stirring: after the temperature in mixed liquor A rises to 80 DEG C, after adding concentrated sulphuric acid stirring 45min, adds catalyst stirring 10min, obtains mixture B;
(4) second time stirring: after the temperature of mixture B rises to 105 DEG C, after adding sodium carbonate stirring 55min, obtains mixed liquor C;
(5) heating: after adding zeolite in mixed liquor C, at 210 DEG C, at the uniform velocity stir 30min, finished product can be obtained.
The preparation method of above-mentioned a kind of environmental type methyl salicylate, wherein, described catalyst is that toluenesulfonic acid mixes together with water, and the ratio of described toluenesulfonic acid and water is 1:5, is added to the water by toluenesulfonic acid under room temperature again and stirs 15min.
Embodiment 2: the preparation method of a kind of environmental type methyl salicylate, its preparation method is as follows:
(1) raw material is weighed: weigh following component by weight and include salicylic acid 40 parts, 400 parts of water, methanol 70 parts, catalyst 10 parts, sodium carbonate 20 parts, concentrated sulphuric acid 60 parts and 2 parts of zeolite;
(2) preheating: first think that adding water in bottle is heated, until after water temperature rises to 60 DEG C, being sequentially added into salicylic acid and methanol stirring 25min, obtaining mixed liquor A;
(3) first time stirring: after the temperature in mixed liquor A rises to 90 DEG C, after adding concentrated sulphuric acid stirring 55min, adds catalyst stirring 15min, obtains mixture B;
(4) second time stirring: after the temperature of mixture B rises to 110 DEG C, after adding sodium carbonate stirring 65min, obtains mixed liquor C;
(5) heating: after adding zeolite in mixed liquor C, at 215 DEG C, at the uniform velocity stir 40min, finished product can be obtained.
The preparation method of above-mentioned a kind of environmental type methyl salicylate, wherein, described catalyst is that toluenesulfonic acid mixes together with water, and the ratio of described toluenesulfonic acid and water is 1:5, is added to the water by toluenesulfonic acid under room temperature again and stirs 20min.
Embodiment 3: the preparation method of a kind of environmental type methyl salicylate, its preparation method is as follows:
(1) raw material is weighed: weigh following component by weight and include salicylic acid 50 parts, 500 parts of water, methanol 80 parts, catalyst 15 parts, sodium carbonate 25 parts, concentrated sulphuric acid 70 parts and 3 parts of zeolite;
(2) preheating: first think that adding water in bottle is heated, until after water temperature rises to 65 DEG C, being sequentially added into salicylic acid and methanol stirring 30min, obtaining mixed liquor A;
(3) first time stirring: after the temperature in mixed liquor A rises to 100 DEG C, after adding concentrated sulphuric acid stirring 65min, adds catalyst stirring 20min, obtains mixture B;
(4) second time stirring: after the temperature of mixture B rises to 115 DEG C, after adding sodium carbonate stirring 75min, obtains mixed liquor C;
(5) heating: after adding zeolite in mixed liquor C, at 220 DEG C, at the uniform velocity stir 45min, finished product can be obtained.
The preparation method of above-mentioned a kind of environmental type methyl salicylate, wherein, described catalyst is that toluenesulfonic acid mixes together with water, and the ratio of described toluenesulfonic acid and water is 1:5, is added to the water by toluenesulfonic acid under room temperature again and stirs 25min.
The preparation method of a kind of environmental type methyl salicylate provided by the invention, including weighing raw material, preheating, first time stirring, second time stirring and heating five steps, configuration is convenient, simple to operate, first react with salicylic acid and methanol, add catalyst and carry out catalysis, wash utilizing sodium carbonate, finished product is obtained finally by high-temperature heating, environmental protection, economical reliable, save the energy, less costly, more original preparation method extent of reaction improves, response time shortens, simultaneously facilitate recycling, reduce sewage disposal difficulty, reduce cost of sewage disposal, improve the safety of entirety, production cycle is shorter, more can meet the demand of user.
The above; being only the present invention preferably detailed description of the invention, but protection scope of the present invention is not limited thereto, any those familiar with the art is in the technical scope that the invention discloses; the change that can readily occur in or replacement, all should be encompassed in protection scope of the present invention. Therefore, protection scope of the present invention should be as the criterion with the protection domain of claims.
Claims (2)
1. a preparation method for environmental type methyl salicylate, is characterized by, its preparation method is as follows:
(1) raw material is weighed: weigh following component by weight and include salicylic acid 30-50 part, water 300-500 part, methanol 60-80 part, catalyst 5-15 part, sodium carbonate 15-25 part, concentrated sulphuric acid 50-70 part and zeolite 1-3 part;
(2) preheating: first think that adding water in bottle is heated, until after water temperature rises to 55 DEG C-65 DEG C, being sequentially added into salicylic acid and methanol stirring 20-30min, obtaining mixed liquor A;
(3) first time stirring: after the temperature in mixed liquor A rises to 80 DEG C-100 DEG C, after adding concentrated sulphuric acid stirring 45-65min, adds catalyst stirring 10-20min, obtains mixture B;
(4) second time stirring: after the temperature of mixture B rises to 105 DEG C-115 DEG C, after adding sodium carbonate stirring 55-75min, obtains mixed liquor C;
(5) heating: after adding zeolite in mixed liquor C, at 210 DEG C-220 DEG C, at the uniform velocity stir 30-45min, finished product can be obtained.
2. the preparation method of a kind of environmental type methyl salicylate as claimed in claim 1, it is characterized by, described catalyst is that toluenesulfonic acid mixes together with water, and the ratio of described toluenesulfonic acid and water is 1:5, is added to the water by toluenesulfonic acid under room temperature again and stirs 15-25min.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201511013000.6A CN105669444A (en) | 2015-12-31 | 2015-12-31 | Preparation method of green environment-friendly methyl salicylate |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201511013000.6A CN105669444A (en) | 2015-12-31 | 2015-12-31 | Preparation method of green environment-friendly methyl salicylate |
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| CN105669444A true CN105669444A (en) | 2016-06-15 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116023259A (en) * | 2023-01-09 | 2023-04-28 | 江苏普源化工有限公司 | High-purity low-cost high-efficiency wintergreen oil production process |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102267911A (en) * | 2011-08-08 | 2011-12-07 | 天津市化学试剂研究所 | Synthesis method of methyl salicylate |
-
2015
- 2015-12-31 CN CN201511013000.6A patent/CN105669444A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102267911A (en) * | 2011-08-08 | 2011-12-07 | 天津市化学试剂研究所 | Synthesis method of methyl salicylate |
Non-Patent Citations (3)
| Title |
|---|
| 俞善信等: "对甲苯磺酸催化合成水杨酸甲酯", 《化学试剂》 * |
| 林洁等: "不同催化剂下合成水杨酸甲酯", 《广东化工》 * |
| 王雪等: "水杨酸甲酯生产工艺的研究进展", 《化工时刊》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116023259A (en) * | 2023-01-09 | 2023-04-28 | 江苏普源化工有限公司 | High-purity low-cost high-efficiency wintergreen oil production process |
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