CN119241352A - A method for refining and purifying industrial salicylic acid - Google Patents
A method for refining and purifying industrial salicylic acid Download PDFInfo
- Publication number
- CN119241352A CN119241352A CN202411443387.8A CN202411443387A CN119241352A CN 119241352 A CN119241352 A CN 119241352A CN 202411443387 A CN202411443387 A CN 202411443387A CN 119241352 A CN119241352 A CN 119241352A
- Authority
- CN
- China
- Prior art keywords
- salicylic acid
- industrial
- refining
- purifying
- reducing agent
- 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
- YGSDEFSMJLZEOE-UHFFFAOYSA-N salicylic acid Chemical compound OC(=O)C1=CC=CC=C1O YGSDEFSMJLZEOE-UHFFFAOYSA-N 0.000 title claims abstract description 97
- 229960004889 salicylic acid Drugs 0.000 title claims abstract description 48
- FJKROLUGYXJWQN-UHFFFAOYSA-N papa-hydroxy-benzoic acid Natural products OC(=O)C1=CC=C(O)C=C1 FJKROLUGYXJWQN-UHFFFAOYSA-N 0.000 title claims abstract description 47
- 238000000034 method Methods 0.000 title claims abstract description 21
- 238000007670 refining Methods 0.000 title claims abstract description 14
- 238000003756 stirring Methods 0.000 claims abstract description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 9
- 238000001816 cooling Methods 0.000 claims abstract description 7
- JVBXVOWTABLYPX-UHFFFAOYSA-L sodium dithionite Chemical group [Na+].[Na+].[O-]S(=O)S([O-])=O JVBXVOWTABLYPX-UHFFFAOYSA-L 0.000 claims description 6
- 238000001035 drying Methods 0.000 abstract description 8
- 238000001914 filtration Methods 0.000 abstract description 7
- 238000010438 heat treatment Methods 0.000 abstract description 6
- 239000000126 substance Substances 0.000 abstract description 4
- 230000000694 effects Effects 0.000 abstract description 2
- 239000012535 impurity Substances 0.000 abstract description 2
- 238000009776 industrial production Methods 0.000 abstract description 2
- 150000003839 salts Chemical class 0.000 abstract description 2
- 238000002156 mixing Methods 0.000 description 5
- ABBQHOQBGMUPJH-UHFFFAOYSA-M Sodium salicylate Chemical compound [Na+].OC1=CC=CC=C1C([O-])=O ABBQHOQBGMUPJH-UHFFFAOYSA-M 0.000 description 3
- 229960004025 sodium salicylate Drugs 0.000 description 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 2
- 238000003916 acid precipitation Methods 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- AZQWKYJCGOJGHM-UHFFFAOYSA-N 1,4-benzoquinone Chemical compound O=C1C=CC(=O)C=C1 AZQWKYJCGOJGHM-UHFFFAOYSA-N 0.000 description 1
- LODHFNUFVRVKTH-ZHACJKMWSA-N 2-hydroxy-n'-[(e)-3-phenylprop-2-enoyl]benzohydrazide Chemical compound OC1=CC=CC=C1C(=O)NNC(=O)\C=C\C1=CC=CC=C1 LODHFNUFVRVKTH-ZHACJKMWSA-N 0.000 description 1
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 229910017053 inorganic salt Inorganic materials 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000006722 reduction reaction Methods 0.000 description 1
- NESLWCLHZZISNB-UHFFFAOYSA-M sodium phenolate Chemical compound [Na+].[O-]C1=CC=CC=C1 NESLWCLHZZISNB-UHFFFAOYSA-M 0.000 description 1
- 229910052938 sodium sulfate Inorganic materials 0.000 description 1
- 235000011152 sodium sulphate Nutrition 0.000 description 1
- 238000000859 sublimation Methods 0.000 description 1
- 230000008022 sublimation Effects 0.000 description 1
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a method for refining and purifying industrial salicylic acid, which comprises the following steps of S1, adding industrial salicylic acid into pure water, stirring and heating to 55-85 ℃, S2, adding a reducing agent, stirring for 20-40min at a constant temperature, S3, cooling to 35-45 ℃, filtering, centrifuging and drying to obtain refined salicylic acid. The refining and purifying method provided by the invention removes impurities such as water-soluble inorganic salts, colored substances and the like in the industrial salicylic acid by using pure water and a reducing agent, so that the product is refined and purified, and the method has the characteristics of remarkable effect, simple process, strong practicability and the like, and is suitable for industrial production.
Description
Technical Field
The invention relates to the technical field of salicylic acid preparation, in particular to a method for refining and purifying industrial salicylic acid.
Background
The salicylic acid alias o-hydroxybenzoic acid and the 2-hydroxybenzoic acid are raw materials with wide application in the industries of medicine, chemical industry and the like. Salicylic acid can be classified into technical grade salicylic acid, sublimation grade salicylic acid and pharmaceutical grade salicylic acid according to grades. The industrial grade salicylic acid is also called industrial salicylic acid, and is prepared by using phenol and liquid alkali as raw materials to react to generate sodium phenolate, drying, reacting with carbon dioxide to generate sodium salicylate, adding water to dissolve the sodium salicylate to obtain a sodium salicylate solution, and then carrying out acid precipitation, centrifugation and drying. The industrial salicylic acid prepared by the process at present has the common conditions of low purity, deep appearance color and high ash content.
Disclosure of Invention
In order to solve the technical problems, the invention provides a method for refining and purifying industrial salicylic acid, which comprises the following specific steps:
s1, adding industrial salicylic acid into pure water, stirring and heating to 55-85 ℃;
S2, adding a reducing agent, and stirring for 20-40min at a constant temperature;
S3, cooling to 35-45 ℃, filtering, centrifuging and drying to obtain refined salicylic acid.
Preferably, in the step S1, the mass ratio of the industrial salicylic acid to the pure water is 1:1-5.
Preferably, in the step S2, the addition ratio of the reducing agent is 0.05-0.2% of that of the industrial salicylic acid.
Preferably, in S2, the reducing agent is sodium dithionite.
According to the industrial salicylic acid refining and purifying method, the reducing agent is added to perform a reduction reaction with colored substances (mainly benzoquinone generated by phenol oxidation) in the industrial salicylic acid so as to achieve the purpose of reducing chromaticity, and the water-soluble inorganic salt (mainly sodium sulfate generated by an acid precipitation working section) in the industrial salicylic acid is removed by mixing and stirring with pure water and filtering so as to achieve the purpose of reducing ash content. The method removes impurities such as colored substances and water-soluble inorganic salts in the industrial salicylic acid, thereby refining and purifying the product.
The industrial salicylic acid refining and purifying method can obviously improve the purity of the product and obviously reduce the chromaticity and ash content of the product. The method has the characteristics of remarkable effect, simple process, strong practicability and the like, and is suitable for industrial production.
Drawings
FIG. 1 is a process flow diagram of the industrial salicylic acid refining and purifying method of the invention.
Examples
The invention will be further described with reference to examples, comparative examples and figures, which do not limit the practice of the invention.
Example 1
Mixing and stirring light pink salicylic acid with the purity of 99.1% and the ash content of 0.25% with pure water according to the mass ratio of 1:2, heating to 55 ℃, adding sodium dithionite with the mass of 0.2% of salicylic acid, keeping the temperature and stirring for 40min, cooling to 35 ℃, filtering, centrifuging and drying to obtain white-like salicylic acid with the purity of 99.6% and the ash content of 0.04%.
Example 2
Mixing and stirring light pink salicylic acid with the purity of 99.1% and the ash content of 0.25% with pure water according to the mass ratio of 1:5, heating to 85 ℃, adding sodium dithionite with the mass of 0.1% of salicylic acid, keeping the temperature and stirring for 30min, cooling to 40 ℃, filtering, centrifuging and drying to obtain white-like salicylic acid with the purity of 99.7% and the ash content of 0.02%.
Example 3
Mixing and stirring light pink salicylic acid with the purity of 99.1% and the ash content of 0.25% with pure water according to the mass ratio of 1:1, heating to 70 ℃, adding sodium dithionite with the mass of 0.05% of salicylic acid, keeping the temperature and stirring for 20min, cooling to 45 ℃, filtering, centrifuging and drying to obtain white-like salicylic acid with the purity of 99.5% and the ash content of 0.05%.
Comparative example
Mixing and stirring the light pink salicylic acid with the purity of 99.1% and the ash content of 0.25% with pure water according to the mass ratio of 2:1, heating to 45 ℃, adding sodium dithionite with the mass of 0.02% of salicylic acid, keeping the temperature and stirring for 10min, cooling to 35 ℃, filtering, centrifuging and drying to obtain the light pink salicylic acid with the purity of 99.2% and the ash content of 0.18%.
Claims (4)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202411443387.8A CN119241352A (en) | 2024-10-16 | 2024-10-16 | A method for refining and purifying industrial salicylic acid |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202411443387.8A CN119241352A (en) | 2024-10-16 | 2024-10-16 | A method for refining and purifying industrial salicylic acid |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN119241352A true CN119241352A (en) | 2025-01-03 |
Family
ID=94031213
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202411443387.8A Pending CN119241352A (en) | 2024-10-16 | 2024-10-16 | A method for refining and purifying industrial salicylic acid |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN119241352A (en) |
-
2024
- 2024-10-16 CN CN202411443387.8A patent/CN119241352A/en active Pending
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101792187B (en) | Method for producing feed grade ferrous sulfate monohydrate from titanium pigment waste acid condensed slag | |
| CN100469771C (en) | Refining method of rubber vulcanization accelerator MBT | |
| CN104774165B (en) | A kind of green industrialized preparation method of rubber peptizer DBD | |
| CN119241352A (en) | A method for refining and purifying industrial salicylic acid | |
| CN114538471B (en) | Comprehensive utilization method of sodium sulfate-sodium chloride mixed salt | |
| CA1076774A (en) | Process of producing sulfuric acid from waste acid and iron sulfate | |
| CN112010792B (en) | Production method of high-purity diphenyl sulfone | |
| CN113336640B (en) | Method for reducing content of 1, 4-naphthalenedicarboxylic acid impurities | |
| CN108977672B (en) | Method for preparing iron molybdate by taking molybdenum-removing slag as raw material | |
| CN114317999B (en) | Method for preparing rhodium trichloride hydrate by doping and dissolving crude rhodium | |
| CN1321060C (en) | Preparation method for zinc borate | |
| WO2024027016A1 (en) | Stable glacial acetic acid-sodium acetate compound and use thereof | |
| CN115650243A (en) | Method for separating and recovering fluorine and silicon in fluorine-containing silicon slag in one step | |
| CN104384169B (en) | The separation and recovery method of pyrite cinder | |
| CN106744725B (en) | The method that selenium is leached from cadmium selenide waste material | |
| CN115010599B (en) | Method for separating and refining salicylic acid from sodium salicylate acidified material | |
| CN111302396A (en) | Preparation method of vanadium pentoxide | |
| CN104961153A (en) | Production method of superfine nano sodium stannate | |
| CN110790288A (en) | Electronic alkali production system and electronic alkali production method | |
| CN109607613A (en) | A method for cleaning and producing high-purity vanadium pentoxide with deionized water | |
| CN102181633A (en) | Molybdenum concentrate constant pressure oxidation leaching technology of byproduct concentrated sulfuric acid | |
| CN119504418A (en) | Extraction and refining method of long carbon chain dibasic acid produced by biological fermentation method | |
| CN119100428A (en) | A method for preparing pharmaceutical aluminum chloride hexahydrate with uniform quality | |
| US2167238A (en) | Process for the manufacture of very pure aluminum compounds | |
| CN116478034A (en) | Purification method of 1,3, 5-trimesic acid |
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 |