CN109734574A - The refinement method of benzoic acid - Google Patents
The refinement method of benzoic acid Download PDFInfo
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- CN109734574A CN109734574A CN201910154130.3A CN201910154130A CN109734574A CN 109734574 A CN109734574 A CN 109734574A CN 201910154130 A CN201910154130 A CN 201910154130A CN 109734574 A CN109734574 A CN 109734574A
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- China
- Prior art keywords
- benzoic acid
- reaction
- acid solution
- crude benzol
- formic acid
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Abstract
The invention discloses a kind of refinement methods of benzoic acid comprising following steps: step 1, adding raw materials, and toluene, solvent, catalyst are added in the reaction vessel, is stirred；Step 2, heating reaction carry out oxidation reaction, and the reaction time is 11~12 hours, and reaction temperature is 120~130 DEG C, obtained crude benzol formic acid solution；Step 3, it is cooling, room temperature is cooled to by crude benzol formic acid that step 2 obtains is molten；Step 4, filtering, the crude benzol formic acid solution that step 3 obtains is filtered, and removes catalyst and impurity.The present invention is using distillation and filtering etc., without the use of the other materials other than system components, to guarantee that new impurity will not be introduced, improves the purity of benzoic acid.
Description
Technical field
The present invention relates to a kind of benzoic acid, more particularly to a kind of refinement method of benzoic acid.
Background technique
Benzoic acid is also known as benzoic acid, is that a hydrogen on phenyl ring is replaced the compound formed by carboxyl (- COOH).Room temperature
For flakey or acicular crystal with benzene or the smell of formaldehyde.Its steam has very strong irritation, and cough is easily caused after sucking
It coughs.It is slightly soluble in water, is soluble in the organic solvents such as ethyl alcohol, ether.The purity of existing benzoic acid is inadequate, influences its normal use.
Summary of the invention
Technical problem to be solved by the invention is to provide a kind of refinement methods of benzoic acid, improve the pure of benzoic acid
Degree, guarantees its normal use.
The present invention is to solve above-mentioned technical problem by following technical proposals: a kind of refinement method of benzoic acid,
It is characterized in that comprising following steps:
Toluene, solvent, catalyst are added in the reaction vessel, is stirred for step 1, adding raw materials；
Step 2, heating reaction carry out oxidation reaction, and the reaction time is 11~12 hours, and reaction temperature is 120~130 DEG C, obtain
The crude benzol formic acid solution arrived；
Step 3, it is cooling, room temperature is cooled to by crude benzol formic acid that step 2 obtains is molten；
Step 4, filtering, the crude benzol formic acid solution that step 3 obtains is filtered, and removes catalyst and impurity；
Filtered crude benzol formic acid solution is distilled, obtains the higher benzoic acid solution of density by step 5, distillation；
Step 6, crystallization, benzoic acid solution are crystallized in crystallization kettle, and Benzoic Acid Crystal is precipitated；
Step 7, dry, the Benzoic Acid Crystal that step 6 is obtained is dried；
Step 8, packaging are packed after dry.
Preferably, the solvent is one or more of in methylene chloride, DMF, THF, benzene, acetonitrile, methanol or nitromethane.
Preferably, the catalyst is benzophenone or metalloporphyrin or cobalt naphthenate.
Preferably, the reaction vessel can be reaction flask or reaction kettle.
Preferably, there are two mouths for the reaction vessel tool.
The positive effect of the present invention is that: the present invention is using distillation and filtering etc., without the use of other than system components
Other materials, thus guarantee will not introduce new impurity, improve the purity of benzoic acid, guarantee its normal use, structure is simple,
It is easy to use.
Specific embodiment
Present pre-ferred embodiments are given below, in order to explain the technical scheme of the invention in detail.
The refinement method of benzoic acid of the present invention the following steps are included:
Toluene, solvent, catalyst are added in the reaction vessel, is stirred for step 1, adding raw materials；
Step 2, heating reaction carry out oxidation reaction, and the reaction time is 11~12 hours, and reaction temperature is 120~130 DEG C, obtain
The crude benzol formic acid solution arrived；
Step 3, it is cooling, room temperature is cooled to by crude benzol formic acid that step 2 obtains is molten；
Step 4, filtering, the crude benzol formic acid solution that step 3 obtains is filtered, and removes catalyst and impurity；
Filtered crude benzol formic acid solution is distilled, obtains the higher benzoic acid solution of density by step 5, distillation；
Step 6, crystallization, benzoic acid solution are crystallized in crystallization kettle, and Benzoic Acid Crystal is precipitated；
Step 7, dry, the Benzoic Acid Crystal that step 6 is obtained is dried；
Step 8, packaging are packed after dry.
Solvent is one or more in methylene chloride, DMF, THF, benzene, acetonitrile, methanol or nitromethane, uses model in this way
It encloses wide.
Catalyst is that benzophenone or metalloporphyrin or cobalt naphthenate, such use scope are wide.
Reaction vessel can be reaction flask or reaction kettle, easy to use in this way, at low cost.
There are two mouths for reaction vessel tool, can be separately added into toluene, solvent, catalyst etc., easy to use.
In conclusion the present invention uses distillation and filtering etc., without the use of the other materials other than system components, to protect
Card will not introduce new impurity, improve the purity of benzoic acid, guarantee its normal use, structure is simple, easy to use.
Particular embodiments described above, the technical issues of to solution of the invention, technical scheme and beneficial effects carry out
It is further described, it should be understood that the above is only a specific embodiment of the present invention, is not limited to
The present invention, all within the spirits and principles of the present invention, any modification, equivalent substitution, improvement and etc. done should be included in this
Within the protection scope of invention.
Claims (5)
1. a kind of refinement method of benzoic acid, which is characterized in that itself the following steps are included:
Toluene, solvent, catalyst are added in the reaction vessel, is stirred for step 1, adding raw materials；
Step 2, heating reaction carry out oxidation reaction, and the reaction time is 11~12 hours, and reaction temperature is 120~130 DEG C, obtain
The crude benzol formic acid solution arrived；
Step 3, it is cooling, room temperature is cooled to by crude benzol formic acid that step 2 obtains is molten；
Step 4, filtering, the crude benzol formic acid solution that step 3 obtains is filtered, and removes catalyst and impurity；
Filtered crude benzol formic acid solution is distilled, obtains the higher benzoic acid solution of density by step 5, distillation；
Step 6, crystallization, benzoic acid solution are crystallized in crystallization kettle, and Benzoic Acid Crystal is precipitated；
Step 7, dry, the Benzoic Acid Crystal that step 6 is obtained is dried；
Step 8, packaging are packed after dry.
2. the refinement method of benzoic acid as described in claim 1, which is characterized in that the solvent be methylene chloride, DMF,
It is one or more of in THF, benzene, acetonitrile, methanol or nitromethane.
3. the refinement method of benzoic acid as described in claim 1, which is characterized in that the catalyst is benzophenone or metal
Porphyrin or cobalt naphthenate.
4. the refinement method of benzoic acid as described in claim 1, which is characterized in that the reaction vessel can be reaction flask or
Reaction kettle.
5. the refinement method of benzoic acid as described in claim 1, which is characterized in that there are two mouths for the reaction vessel tool.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910154130.3A CN109734574A (en) | 2019-03-01 | 2019-03-01 | The refinement method of benzoic acid |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910154130.3A CN109734574A (en) | 2019-03-01 | 2019-03-01 | The refinement method of benzoic acid |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN109734574A true CN109734574A (en) | 2019-05-10 |
Family
ID=66369004
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201910154130.3A Pending CN109734574A (en) | 2019-03-01 | 2019-03-01 | The refinement method of benzoic acid |
Country Status (1)
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| CN (1) | CN109734574A (en) |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20120058024A1 (en) * | 2007-06-27 | 2012-03-08 | H R D Corporation | System and process for production of benzoic acids and phthalic acids |
| CN103910623A (en) * | 2014-03-03 | 2014-07-09 | 复旦大学 | Preparation method for benzoic acid |
| CN106866403A (en) * | 2017-02-15 | 2017-06-20 | 中山大学惠州研究院 | A kind of preparation method of benzoic acid |
-
2019
- 2019-03-01 CN CN201910154130.3A patent/CN109734574A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20120058024A1 (en) * | 2007-06-27 | 2012-03-08 | H R D Corporation | System and process for production of benzoic acids and phthalic acids |
| CN103910623A (en) * | 2014-03-03 | 2014-07-09 | 复旦大学 | Preparation method for benzoic acid |
| CN106866403A (en) * | 2017-02-15 | 2017-06-20 | 中山大学惠州研究院 | A kind of preparation method of benzoic acid |
Non-Patent Citations (1)
| Title |
|---|
| 翁世伟等: "苯甲酸", 《化工产品实用手册（二）》 * |
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Application publication date: 20190510 |