CN102690196A - Preparation and purification method of 3,4,5-trimethoxybenzoic acid - Google Patents
Preparation and purification method of 3,4,5-trimethoxybenzoic acid Download PDFInfo
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- CN102690196A CN102690196A CN2011100945229A CN201110094522A CN102690196A CN 102690196 A CN102690196 A CN 102690196A CN 2011100945229 A CN2011100945229 A CN 2011100945229A CN 201110094522 A CN201110094522 A CN 201110094522A CN 102690196 A CN102690196 A CN 102690196A
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- trimethoxybenzoic acid
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Abstract
The invention provides a preparation and purification method of 3,4,5-trimethoxybenzoic acid, which comprises the following steps: completely dissolving gallic acid in water in a reaction vessel, adding liquid alkali and dimethyl sulfate to carry out methylation reaction, hydrolyzing, regulating the pH value by acidification, and dewatering to obtain coarse crystals; decolorizing with activated carbon, dewatering, and carrying out vacuum drying to obtain the fine 3,4,5-trimethoxybenzoic acid product; and adding the measured fine 3,4,5-trimethoxybenzoic acid product and 45 wt% sodium carbonate solution into a reaction kettle in a ratio of 1:4.5, reacting at 90 DEG C for 4 hours, cooling to 40 DEG C, adding sulfuric acid to regulate the pH value to 1-2, dewatering, mixing the fine 3,4,5-trimethoxybenzoic acid crystals, activated carbon and water in a ratio of 10:2:100, keeping the temperature at 85 DEG C for 30 minutes, filtering, regulating the pH value to 2 with sulfuric acid, dewatering, and finally, carrying out vacuum drying to obtain the high-purity finished 3,4,5-trimethoxybenzoic acid product.
Description
Technical field
The present invention relates to a kind of preparation and method of purification of organic cpds, particularly a kind of 3,4, the preparation of 5-trimethoxybenzoic acid and method of purification.
Background technology
At present, the preparation of prior art trimethoxybenzoic acid is after water all dissolves in reaction vessel with Chinese gallotanninic acid, to add liquid caustic soda and methyl-sulfate and carry out methylation reaction, after hydrolysis, regulates pH value and carries out acidifying; Make 3,4 after the dehydration, 5-trimethoxybenzoic acid coarse crystal; After activated carbon decolorizing, dehydration, vacuum-drying, get 3,4,5-trimethoxybenzoic acid elaboration; Main content reaches 99.5%, and total impurities is controlled at 0.5%, and its foreign matter content is very high.
Summary of the invention
In order to improve 3,4, the content of 5-trimethoxybenzoic acid reduces its impurity, and it is a kind of 3,4 that the present invention proposes, the preparation of 5-trimethoxybenzoic acid and method of purification.
Technical scheme of the present invention is: a kind of 3,4, and the preparation of 5-trimethoxybenzoic acid and method of purification; It is characterized in that: after at first water all dissolves in reaction vessel with gallic acid, add liquid caustic soda and methyl-sulfate and carry out methylation reaction, after hydrolysis, regulate pH value and carry out acidifying; Make 3,4 after the dehydration, 5-trimethoxybenzoic acid coarse crystal; After activated carbon decolorizing, dehydration, vacuum-drying, get 3,4,5-trimethoxybenzoic acid elaboration; Then, with measure 3,4; 5-trimethoxybenzoic acid elaboration and mass percent concentration are that 45% sodium carbonate solution is put in the reaction kettle in the ratio of 1:4.5, and reaction is 4 hours under 90 ℃ of temperature, cools to 40 ℃; Add sulfuric acid, transferring pH value is 1-2, dewater 3; The smart crystal of 4,5-trimethoxybenzoic acid; Then 3,4, the smart crystal of 5-trimethoxybenzoic acid, gac, water are with the mixed of 10:2:100; Insulation 30 minutes under 85 ℃ of temperature, filtration, using sulfuric acid to transfer pH value is 2, dehydration; After vacuum-drying gets 3,4,5-trimethoxybenzoic acid finished product.
Beneficial effect: preparation and method of purification that the present invention adopts, make 3,4,5-trimethoxybenzoic acid master content reaches more than 99.90%, and total impurities is controlled at below 0.10%.
Embodiment
Specify through embodiment below, a kind of 3,4, the preparation of 5-trimethoxybenzoic acid and method of purification: will measure 150 kilogram 3; 4,5-trimethoxybenzoic acid elaboration and mass percent concentration are that 45% sodium carbonate solution joins in 1000 liters of closed reaction kettle for 675 kilograms, open steam and heat up; Reaction is 4 hours under 90 ℃ of temperature, cools to 40 ℃, and adding sulfuric acid accent pH value is 2; Dewater 3,4, the smart crystal of 5-trimethoxybenzoic acid; 3,4, the smart crystal of 5-trimethoxybenzoic acid, gac, water be with the mixed of 10:2:100, insulation 30 minutes under 85 ℃ of temperature, filters, and transferring pH value with sulfuric acid is 2, and dehydration gets finished product through vacuum-drying then; Said mass percent concentration is that 45% sodium carbonate solution is: yellow soda ash is dissolved in the aqueous solution of preparing in the water.The present invention through gallic acid is carried out methylation reaction, hydrolysis, acidifying, dehydration obtain 3,4,5-trimethoxybenzoic acid coarse crystal; After activated carbon decolorizing, dehydration, vacuum-drying, get 3,4; 5-trimethoxybenzoic acid elaboration, purification processing then: add mass percent concentration and be 45% sodium carbonate solution and trimethoxybenzoic acid elaboration and react, with in the sulfuric acid and after; Make finished product through dehydration, drying, its purity rises to more than 99.90%, has improved 3 greatly; The purity of 4,5-trimethoxybenzoic acid.
Claims (1)
1. one kind 3,4, the preparation of 5-trimethoxybenzoic acid and method of purification; It is characterized in that: after at first water all dissolves in reaction vessel with gallic acid, add liquid caustic soda and methyl-sulfate and carry out methylation reaction, after hydrolysis, regulate pH value and carry out acidifying; Make 3,4 after the dehydration, 5-trimethoxybenzoic acid coarse crystal; After activated carbon decolorizing, dehydration, vacuum-drying, get 3,4,5-trimethoxybenzoic acid elaboration; Then, with measure 3,4; 5-trimethoxybenzoic acid elaboration and mass percent concentration are that 45% sodium carbonate solution is put in the reaction kettle in the ratio of 1:4.5, and reaction is 4 hours under 90 ℃ of temperature, cools to 40 ℃; Add sulfuric acid, transferring pH value is 1-2, dewater 3; The smart crystal of 4,5-trimethoxybenzoic acid; Then 3,4, the smart crystal of 5-trimethoxybenzoic acid, gac, water are with the mixed of 10:2:100; Insulation 30 minutes under 85 ℃ of temperature, filtration, using sulfuric acid to transfer pH value is 2, dehydration; After vacuum-drying gets 3,4,5-trimethoxybenzoic acid finished product.
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| Application Number | Priority Date | Filing Date | Title |
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| CN2011100945229A CN102690196A (en) | 2011-04-15 | 2011-04-15 | Preparation and purification method of 3,4,5-trimethoxybenzoic acid |
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| CN2011100945229A CN102690196A (en) | 2011-04-15 | 2011-04-15 | Preparation and purification method of 3,4,5-trimethoxybenzoic acid |
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| CN102690196A true CN102690196A (en) | 2012-09-26 |
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| CN2011100945229A Pending CN102690196A (en) | 2011-04-15 | 2011-04-15 | Preparation and purification method of 3,4,5-trimethoxybenzoic acid |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105017000A (en) * | 2015-06-17 | 2015-11-04 | 遵义鑫湘生物科技有限公司 | Trimethoxybenzoic acid preparation method |
| CN106977397A (en) * | 2017-04-11 | 2017-07-25 | 五峰赤诚生物科技股份有限公司 | A kind of synthetic method of 3,4,5 trimethoxybenzoic acid |
| CN107337599A (en) * | 2017-07-28 | 2017-11-10 | 竹山县天新医药化工有限责任公司 | A kind of preparation method of 3,4,5 tri-methoxybenzoates |
| US10900657B2 (en) | 2017-08-01 | 2021-01-26 | Technical Consumer Products, Inc. | Edge-lit light fixture having capabilities for a secondary service |
| CN113801009A (en) * | 2021-09-26 | 2021-12-17 | 武汉工程大学 | Method for catalyzing gallic acid methylation by using ionic liquid |
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| CN1480446A (en) * | 2002-09-05 | 2004-03-10 | 张家界贸源化工有限公司 | Technique for producing gallic acid by direct acid hydrolysis of gallnut |
| CN1706792A (en) * | 2005-05-09 | 2005-12-14 | 竹山县天新医药化工有限责任公司 | Purifying process of 3,4,5-trimethoxyl benzoic acid |
| CN101260038A (en) * | 2008-04-12 | 2008-09-10 | 竹山县天新医药化工有限责任公司 | Method for purifying 3,4,5-trimethoxylbenzoic acid |
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2011
- 2011-04-15 CN CN2011100945229A patent/CN102690196A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1480446A (en) * | 2002-09-05 | 2004-03-10 | 张家界贸源化工有限公司 | Technique for producing gallic acid by direct acid hydrolysis of gallnut |
| CN1706792A (en) * | 2005-05-09 | 2005-12-14 | 竹山县天新医药化工有限责任公司 | Purifying process of 3,4,5-trimethoxyl benzoic acid |
| CN101260038A (en) * | 2008-04-12 | 2008-09-10 | 竹山县天新医药化工有限责任公司 | Method for purifying 3,4,5-trimethoxylbenzoic acid |
Non-Patent Citations (1)
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105017000A (en) * | 2015-06-17 | 2015-11-04 | 遵义鑫湘生物科技有限公司 | Trimethoxybenzoic acid preparation method |
| CN106977397A (en) * | 2017-04-11 | 2017-07-25 | 五峰赤诚生物科技股份有限公司 | A kind of synthetic method of 3,4,5 trimethoxybenzoic acid |
| CN106977397B (en) * | 2017-04-11 | 2020-06-05 | 五峰赤诚生物科技股份有限公司 | Synthetic method of 3,4, 5-trimethoxybenzoic acid |
| CN107337599A (en) * | 2017-07-28 | 2017-11-10 | 竹山县天新医药化工有限责任公司 | A kind of preparation method of 3,4,5 tri-methoxybenzoates |
| US10900657B2 (en) | 2017-08-01 | 2021-01-26 | Technical Consumer Products, Inc. | Edge-lit light fixture having capabilities for a secondary service |
| CN113801009A (en) * | 2021-09-26 | 2021-12-17 | 武汉工程大学 | Method for catalyzing gallic acid methylation by using ionic liquid |
| CN113801009B (en) * | 2021-09-26 | 2022-12-20 | 武汉工程大学 | Method for catalyzing gallic acid methylation by using ionic liquid |
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Application publication date: 20120926 |