CN107141215A - A kind of salicylic acid preparation method of environmental protection in high yield - Google Patents
A kind of salicylic acid preparation method of environmental protection in high yield Download PDFInfo
- Publication number
- CN107141215A CN107141215A CN201710328978.4A CN201710328978A CN107141215A CN 107141215 A CN107141215 A CN 107141215A CN 201710328978 A CN201710328978 A CN 201710328978A CN 107141215 A CN107141215 A CN 107141215A
- Authority
- CN
- China
- Prior art keywords
- sodium
- salicylic acid
- solution
- environmental protection
- high yield
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/02—Preparation of carboxylic acids or their salts, halides or anhydrides from salts of carboxylic acids
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C37/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom of a six-membered aromatic ring
- C07C37/64—Preparation of O-metal compounds with O-metal group bound to a carbon atom belonging to a six-membered aromatic ring
- C07C37/66—Preparation of O-metal compounds with O-metal group bound to a carbon atom belonging to a six-membered aromatic ring by conversion of hydroxy groups to O-metal groups
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/15—Preparation of carboxylic acids or their salts, halides or anhydrides by reaction of organic compounds with carbon dioxide, e.g. Kolbe-Schmitt synthesis
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/41—Preparation of salts of carboxylic acids
- C07C51/412—Preparation of salts of carboxylic acids by conversion of the acids, their salts, esters or anhydrides with the same carboxylic acid part
Abstract
A kind of salicylic acid preparation method of environmental protection of the present invention in high yield, its preparation method comprises the following steps：1st, prepared by sodium phenate powder；2nd, prepared by sodium salicylate solution；3rd, finished product salicylic acid is made；The present invention, more conventional salicylic acid preparation technology is compared, water requirement is less, greatly reduce water resource waste, sodium phenate is dried quick, sodium phenate resinification and coloring can be prevented effectively from, salicylic product yield is substantially increased, meanwhile, the carboxylation reaction time is short, while reducing energy consumption, anti- due purity is higher, salicylic product yield is improved again, in summary, a kind of environmental protection salicylic acid preparation method in high yield of the present invention, it possess environmental protection, water saving, energy-conservation, efficiently, in high yield the characteristics of.
Description
Technical field
The present invention relates to a kind of salicylic preparation method, the salicylic acid system of particularly a kind of environmental protection in high yield
Preparation Method.
Background technology
Salicylic acid, chemical name septichen, also known as salicylic acid, are present in the willow bark, Gaultheria leaf, sweet tea of nature
In birch and other many plants.Salicylic acid has clearing heat and detoxicating and sterilization effect, primarily now as the original of medical industry
Material, for preparing the medicines such as aspirin, sodium salicylate, salicylamide, ethoxybenzamide, phenyl salicylate, Niclosamide.Be medicine,
The important source material of the fine chemicals such as dyestuff, rubber industry, resin, spices, agricultural chemicals.It is widely used in antipyretic-antalgic, direct dyes, kills
The manufacturing of the products such as worm agent, deodorant tune and ultra-violet absorber.
In very widely used today salicylic acid preparation technology, the water requirement existed more is high, the shortcoming of carboxylation reaction time length,
Cause product yield low, energy consumption is also greatly improved therewith, the characteristics of not possessing environment protection energy-saving efficient.
The content of the invention
In view of the above-mentioned problems, the salicylic acid preparation method the invention discloses a kind of environmental protection in high yield.
To solve above technical problem, the technical scheme that the present invention is provided is:
The salicylic acid preparation method of a kind of environmental protection in high yield, it is characterised in that its preparation method comprises the following steps：
（1）It is prepared by sodium phenate powder：Under nitrogen protection, phenol is dissolved in dimethylbenzene, the xylene solution of phenol is made,
The xylene solution of phenol is pumped into reactor, is stirred and is slowly heated, and treats that temperature rises to 42 ~ 60 DEG C, by 50% hydroxide
Sodium hot solution is heated in reactor, carries out salinization reaction, is treated that temperature reaches 80 DEG C, is maintained 30 ~ 45 minutes, treats salinization reaction knot
Beam, obtains phenol sodium solution, and subsequent continuous heating carries out heating drop to 130 ~ 135 DEG C, and progressively to being depressured in reactor
Press dry dry, finally obtain sodium phenate powder；
（2）It is prepared by sodium salicylate solution：Maintain step（1）The temperature of middle sodium phenate powder is at 100 DEG C, while leading into reactor
The CO2 for entering 0.5~0.6Mpa carries out carboxylation, to avoid after sodium phenate powder resin and coloring, band CO2 are passed through 5 minutes, is pumped into
Distilled water, promotes carboxylation reaction, and be heated to 160~170 DEG C, maintenance 3 ~ 4 hours；Question response is completed, and is concentrated in vacuo, obtained
To sodium salicylate solution；
（3）Finished product salicylic acid is made：By step（2）In obtained sodium salicylate solution be put into decolouring groove, by add zinc powder and
Activated carbon, is decolourized, and is waited to decolourize to complete, after press filtration, is obtained clear liquid, obtained clear liquid is pumped into sulfuric acid tank, and add dilute
Sulfuric acid carries out acid out, treats that acid out is completed, and after reaction solution centrifugal drying, obtains salicylic acid, receives after Flexible Container, obtain finished product bigcatkin willow
Acid.
A kind of salicylic acid preparation method of above-mentioned environmental protection in high yield, wherein, step（1）In, the phenol and two
The mass ratio of toluene is 1：3.9.
A kind of salicylic acid preparation method of above-mentioned environmental protection in high yield, wherein, step（1）In, 50% hydrogen-oxygen
The temperature for changing sodium hot solution is 30 ~ 40 DEG C, the mass ratio of the xylene solution of 50% sodium hydroxide hot solution and phenol for 51 ~
52：48~49.
A kind of salicylic acid preparation method of above-mentioned environmental protection in high yield, wherein, step（2）In, the distilled water with
The mass ratio of sodium phenate powder is 200 ~ 230：1.
A kind of salicylic acid preparation method of above-mentioned environmental protection in high yield, wherein, step（2）In, obtained salicylic acid
The solid-liquid ratio of sodium solution is 30%.
A kind of salicylic acid preparation method of above-mentioned environmental protection in high yield, wherein, step（3）In, the dilute sulfuric acid
Concentration is 35%~55%.
Beneficial effects of the present invention are：
A kind of salicylic acid preparation method of environmental protection of the present invention in high yield, its preparation method comprises the following steps：1st, phenol
It is prepared by sodium powder material；2nd, prepared by sodium salicylate solution；3rd, finished product salicylic acid is made；The present invention, more conventional salicylic acid preparation technology
Compare, water requirement is less, greatly reduce water resource waste, sodium phenate dry it is quick, can be prevented effectively from sodium phenate resinification and
Coloring, substantially increases salicylic product yield, meanwhile, the carboxylation reaction time is short, while reducing energy consumption, anti-due
Purity is higher, and salicylic product yield is improved again, in summary, a kind of bigcatkin willow of environmental protection of the invention in high yield
Sour preparation method, it possess environmental protection, water saving, energy-conservation, efficiently, in high yield the characteristics of.
Embodiment
Embodiment one
The salicylic acid preparation method of a kind of environmental protection in high yield, it is characterised in that its preparation method comprises the following steps：
（1）It is prepared by sodium phenate powder：Under nitrogen protection, phenol is dissolved in dimethylbenzene, the xylene solution of phenol is made,
The xylene solution of phenol is pumped into reactor, is stirred and is slowly heated, and treats that temperature rises to 50 DEG C, by 50% sodium hydroxide heat
Solution is heated in reactor, carries out salinization reaction, is treated that temperature reaches 80 DEG C, is maintained 40 minutes, is treated that salinization reaction terminates, is obtained
Phenol sodium solution, subsequent continuous heating carries out heating decompression drying, finally to 130 DEG C, and progressively to being depressured in reactor
Obtain sodium phenate powder；
（2）It is prepared by sodium salicylate solution：Maintain step（1）The temperature of middle sodium phenate powder is at 100 DEG C, while leading into reactor
The CO2 for entering 0.5~0.6Mpa carries out carboxylation, to avoid after sodium phenate powder resin and coloring, band CO2 are passed through 5 minutes, is pumped into
Distilled water, promotes carboxylation reaction, and be heated to 160 DEG C, maintenance 3.2 hours；Question response is completed, and is concentrated in vacuo, obtains water
Poplar acid sodium solution；
（3）Finished product salicylic acid is made：By step（2）In obtained sodium salicylate solution be put into decolouring groove, by add zinc powder and
Activated carbon, is decolourized, and is waited to decolourize to complete, after press filtration, is obtained clear liquid, obtained clear liquid is pumped into sulfuric acid tank, and add dilute
Sulfuric acid carries out acid out, treats that acid out is completed, and after reaction solution centrifugal drying, obtains salicylic acid, receives after Flexible Container, obtain finished product bigcatkin willow
Acid.
Wherein, step（1）In, the mass ratio of the phenol and dimethylbenzene is 1：3.9, the 50% sodium hydroxide hot solution
Temperature be 35 DEG C, the mass ratio of the xylene solution of 50% sodium hydroxide hot solution and phenol is 51：49, step（2）In, institute
The mass ratio for stating distilled water and sodium phenate powder is 200：1, step（2）In, the solid-liquid ratio of obtained sodium salicylate solution is
30%, step（1）In, the concentration of the dilute sulfuric acid is 45%.
Embodiment two
The salicylic acid preparation method of a kind of environmental protection in high yield, it is characterised in that its preparation method comprises the following steps：
（1）It is prepared by sodium phenate powder：Under nitrogen protection, phenol is dissolved in dimethylbenzene, the xylene solution of phenol is made,
The xylene solution of phenol is pumped into reactor, is stirred and is slowly heated, and treats that temperature rises to 55 DEG C, by 50% sodium hydroxide heat
Solution is heated in reactor, carries out salinization reaction, is treated that temperature reaches 80 DEG C, is maintained 45 minutes, is treated that salinization reaction terminates, is obtained
Phenol sodium solution, subsequent continuous heating carries out heating decompression drying, finally to 135 DEG C, and progressively to being depressured in reactor
Obtain sodium phenate powder；
（2）It is prepared by sodium salicylate solution：Maintain step（1）The temperature of middle sodium phenate powder is at 100 DEG C, while leading into reactor
The CO2 for entering 0.5~0.6Mpa carries out carboxylation, to avoid after sodium phenate powder resin and coloring, band CO2 are passed through 5 minutes, is pumped into
Distilled water, promotes carboxylation reaction, and be heated to 170 DEG C, maintenance 4 hours；Question response is completed, and is concentrated in vacuo, obtains bigcatkin willow
Acid sodium solution；
（3）Finished product salicylic acid is made：By step（2）In obtained sodium salicylate solution be put into decolouring groove, by add zinc powder and
Activated carbon, is decolourized, and is waited to decolourize to complete, after press filtration, is obtained clear liquid, obtained clear liquid is pumped into sulfuric acid tank, and add dilute
Sulfuric acid carries out acid out, treats that acid out is completed, and after reaction solution centrifugal drying, obtains salicylic acid, receives after Flexible Container, obtain finished product bigcatkin willow
Acid.
Wherein, step（1）In, the mass ratio of the phenol and dimethylbenzene is 1：3.9, the 50% sodium hydroxide hot solution
Temperature be 40 DEG C, the mass ratio of the xylene solution of 50% sodium hydroxide hot solution and phenol is 52：48, step（2）In, institute
The mass ratio for stating distilled water and sodium phenate powder is 220：1, step（2）In, the solid-liquid ratio of obtained sodium salicylate solution is
30%, step（3）In, the concentration of the dilute sulfuric acid is 55%.
The foregoing is only a preferred embodiment of the present invention, but protection scope of the present invention be not limited thereto,
Any one skilled in the art the invention discloses technical scope in, the change or replacement that can be readily occurred in,
It should all cover within the scope of the present invention.Therefore, protection scope of the present invention should be with the protection domain of claims
It is defined.
Claims (6)
1. the salicylic acid preparation method of a kind of environmental protection in high yield, it is characterised in that its preparation method comprises the following steps：
（1）It is prepared by sodium phenate powder：Under nitrogen protection, phenol is dissolved in dimethylbenzene, the xylene solution of phenol is made,
The xylene solution of phenol is pumped into reactor, is stirred and is slowly heated, and treats that temperature rises to 42 ~ 60 DEG C, by 50% hydroxide
Sodium hot solution is heated in reactor, carries out salinization reaction, is treated that temperature reaches 80 DEG C, is maintained 30 ~ 45 minutes, treats salinization reaction knot
Beam, obtains phenol sodium solution, and subsequent continuous heating carries out heating drop to 130 ~ 135 DEG C, and progressively to being depressured in reactor
Press dry dry, finally obtain sodium phenate powder；
（2）It is prepared by sodium salicylate solution：Maintain step（1）The temperature of middle sodium phenate powder is at 100 DEG C, while leading into reactor
The CO2 for entering 0.5~0.6Mpa carries out carboxylation, to avoid after sodium phenate powder resin and coloring, band CO2 are passed through 5 minutes, is pumped into
Distilled water, promotes carboxylation reaction, and be heated to 160~170 DEG C, maintenance 3 ~ 4 hours；Question response is completed, and is concentrated in vacuo, obtained
To sodium salicylate solution；
（3）Finished product salicylic acid is made：By step（2）In obtained sodium salicylate solution be put into decolouring groove, by add zinc powder and
Activated carbon, is decolourized, and is waited to decolourize to complete, after press filtration, is obtained clear liquid, obtained clear liquid is pumped into sulfuric acid tank, and add dilute
Sulfuric acid carries out acid out, treats that acid out is completed, and after reaction solution centrifugal drying, obtains salicylic acid, receives after Flexible Container, obtain finished product bigcatkin willow
Acid.
2. a kind of salicylic acid preparation method of environmental protection in high yield as claimed in claim 1, it is characterised in that step（1）
In, the mass ratio of the phenol and dimethylbenzene is 1：3.9.
3. the salicylic acid preparation method of a kind of environmental protection in high yield as claimed in claim 1, it is characterised in that described 50%
The temperature of sodium hydroxide hot solution is 30 ~ 40 DEG C, and the mass ratio of the xylene solution of 50% sodium hydroxide hot solution and phenol is
51~52：48~49.
4. a kind of salicylic acid preparation method of environmental protection in high yield as claimed in claim 1, it is characterised in that the distillation
The mass ratio of water and sodium phenate powder is 200 ~ 230：1.
5. a kind of salicylic acid preparation method of environmental protection in high yield as claimed in claim 1, it is characterised in that obtained water
The solid-liquid ratio of poplar acid sodium solution is 30%.
6. a kind of salicylic acid preparation method of environmental protection in high yield as claimed in claim 1, it is characterised in that dilute sulphur
The concentration of acid is 35%~55%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710328978.4A CN107141215A (en) | 2017-05-11 | 2017-05-11 | A kind of salicylic acid preparation method of environmental protection in high yield |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710328978.4A CN107141215A (en) | 2017-05-11 | 2017-05-11 | A kind of salicylic acid preparation method of environmental protection in high yield |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN107141215A true CN107141215A (en) | 2017-09-08 |
Family
ID=59778269
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710328978.4A Pending CN107141215A (en) | 2017-05-11 | 2017-05-11 | A kind of salicylic acid preparation method of environmental protection in high yield |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN107141215A (en) |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109180491A (en) * | 2018-10-29 | 2019-01-11 | 淮安万邦香料工业有限公司 | A kind of synthetic method of pineapple ether |
| CN110642707A (en) * | 2019-10-22 | 2020-01-03 | 成都市科隆化学品有限公司 | Purification production method of low-cost environment-friendly sodium salicylate |
| CN112341335A (en) * | 2020-11-24 | 2021-02-09 | 江苏宏邦化工科技有限公司 | Synthesis method of methyl salicylate |
| CN114345285A (en) * | 2022-01-12 | 2022-04-15 | 青岛科技大学 | Continuous production process of sodium salicylate solution |
| CN114874092A (en) * | 2022-06-13 | 2022-08-09 | 扬州大学 | Method for preparing sodium salicylate through sodium phenolate carboxylation reaction |
| CN115650842A (en) * | 2022-10-25 | 2023-01-31 | 江苏普源化工有限公司 | Production process of circulating dehydration high-purity salicylic acid |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4171453A (en) * | 1978-02-22 | 1979-10-16 | The Dow Chemical Company | Carbonation of alkali metal phenates |
| EP0478197A1 (en) * | 1990-09-17 | 1992-04-01 | MITSUI TOATSU CHEMICALS, Inc. | Control process of isomer ratio of aromatic hydroxycarboxylic acid |
| EP0548906A2 (en) * | 1991-12-27 | 1993-06-30 | Sanko Kaihatsu Kagaku Kenkyusho | Method for preparing nuclear-substituted salicylic acids and metal salts thereof |
| CN1733684A (en) * | 2005-08-02 | 2006-02-15 | 山东轻工业学院 | Novel supercritical phase salicylic acid synthesis process |
| CN101143817A (en) * | 2007-10-09 | 2008-03-19 | 山东新华隆信化工有限公司 | Method for producing salicylic acid by refining salicylic acid solution |
| CN101613270A (en) * | 2009-07-30 | 2009-12-30 | 浙江大学 | A kind of salicylic preparation method |
-
2017
- 2017-05-11 CN CN201710328978.4A patent/CN107141215A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4171453A (en) * | 1978-02-22 | 1979-10-16 | The Dow Chemical Company | Carbonation of alkali metal phenates |
| EP0478197A1 (en) * | 1990-09-17 | 1992-04-01 | MITSUI TOATSU CHEMICALS, Inc. | Control process of isomer ratio of aromatic hydroxycarboxylic acid |
| EP0548906A2 (en) * | 1991-12-27 | 1993-06-30 | Sanko Kaihatsu Kagaku Kenkyusho | Method for preparing nuclear-substituted salicylic acids and metal salts thereof |
| CN1733684A (en) * | 2005-08-02 | 2006-02-15 | 山东轻工业学院 | Novel supercritical phase salicylic acid synthesis process |
| CN101143817A (en) * | 2007-10-09 | 2008-03-19 | 山东新华隆信化工有限公司 | Method for producing salicylic acid by refining salicylic acid solution |
| CN101613270A (en) * | 2009-07-30 | 2009-12-30 | 浙江大学 | A kind of salicylic preparation method |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109180491A (en) * | 2018-10-29 | 2019-01-11 | 淮安万邦香料工业有限公司 | A kind of synthetic method of pineapple ether |
| CN110642707A (en) * | 2019-10-22 | 2020-01-03 | 成都市科隆化学品有限公司 | Purification production method of low-cost environment-friendly sodium salicylate |
| CN110642707B (en) * | 2019-10-22 | 2022-04-19 | 成都市科隆化学品有限公司 | Purification production method of low-cost environment-friendly sodium salicylate |
| CN112341335A (en) * | 2020-11-24 | 2021-02-09 | 江苏宏邦化工科技有限公司 | Synthesis method of methyl salicylate |
| CN114345285A (en) * | 2022-01-12 | 2022-04-15 | 青岛科技大学 | Continuous production process of sodium salicylate solution |
| CN114345285B (en) * | 2022-01-12 | 2023-09-08 | 青岛科技大学 | Continuous production process of sodium salicylate solution |
| CN114874092A (en) * | 2022-06-13 | 2022-08-09 | 扬州大学 | Method for preparing sodium salicylate through sodium phenolate carboxylation reaction |
| CN115650842A (en) * | 2022-10-25 | 2023-01-31 | 江苏普源化工有限公司 | Production process of circulating dehydration high-purity salicylic acid |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN107141215A (en) | A kind of salicylic acid preparation method of environmental protection in high yield | |
| CN105924623B (en) | A kind of eugenol epoxy resin and the preparation method and application thereof | |
| Wang et al. | Linear polyester synthesized from furfural-based monomer by photoreaction in sunlight | |
| CN102101847B (en) | Method for preparing N-methyl-N'-(2-chloroethyl)piperazine | |
| WO2018152870A1 (en) | Method for preparing levoglucosenone by catalytic pyrolysis of biomass | |
| Luo et al. | Hydrothermal conversion of water lettuce biomass at 473 or 523 K | |
| CN104693032A (en) | Process for manufacturing high-purity alpha-ethyl linolenate | |
| Huang et al. | Solid protonic acids and luminescent carbon dots derived from waste expanded polystyrene | |
| CN110483268A (en) | A kind of method that heteropoly acid catalysis microcrystalline cellulose prepares levulic acid | |
| CN107892640B (en) | Preparation method for preparing camphene by alpha-pinene isomerization | |
| CN107827728A (en) | Based on the processing method for reclaiming chloroacetic monoxone heavy constituent | |
| CN102267911A (en) | Synthesis method of methyl salicylate | |
| CN105218366B (en) | Preparation method of glyceryl triacetate | |
| CN101885669A (en) | Preparation method of 4-vinyl guaiacol | |
| CN103374046A (en) | Method for preparing D-glucosamine hydrochloride | |
| WO2023245919A1 (en) | Method for improving ultra-violet light transmittance of ethylene glycol | |
| CN108546248B (en) | Preparation method of 1, 2-dihydro-3, 6-pyridazine dione | |
| CN104087562A (en) | Extraction method of superoxide dismutase | |
| CN106986762A (en) | A kind of technique for preparing DL mandelic acids | |
| CN111004137B (en) | Synthesis method of racemic phenylglycine | |
| CN106146284B (en) | A method of gallic acid and pyrogallic acid are prepared with tannin biomass | |
| CN106010280A (en) | Production method of hydrogenated rosin | |
| CN105418556A (en) | Furfural preparation method using corn stalk as raw material | |
| CN108752271A (en) | A kind of synthetic method of oxyquinoline | |
| CN106946665A (en) | The method that phenols chemicals and acids chemicals are extracted from pyrolkigneous liquid |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20170908 |