CN107903151A - A kind of purification process of 2,2 ' dihydroxybiphenyls - Google Patents
A kind of purification process of 2,2 ' dihydroxybiphenyls Download PDFInfo
- Publication number
- CN107903151A CN107903151A CN201711172600.6A CN201711172600A CN107903151A CN 107903151 A CN107903151 A CN 107903151A CN 201711172600 A CN201711172600 A CN 201711172600A CN 107903151 A CN107903151 A CN 107903151A
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- dihydroxybiphenyl
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- 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
- C07C37/68—Purification; separation; Use of additives, e.g. for stabilisation
- C07C37/685—Processes comprising at least two steps in series
-
- 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
- C07C37/68—Purification; separation; Use of additives, e.g. for stabilisation
- C07C37/86—Purification; separation; Use of additives, e.g. for stabilisation by treatment giving rise to a chemical modification
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The present invention provides a kind of purification process of 2,2 ' dihydroxybiphenyls, and purification step is as follows：First 2,2 ' dihydroxybiphenyl of liquid is added in ionized water, is heated up, after temperature is increased to 50 DEG C 75 DEG C, acidulant sulfuric acid is added dropwise, after ten minutes, control acidifying terminal pH value is 23 for reaction；After the acid liquid of acquisition is stood 30 50 minutes, aqueous slkali is added, after being warming up to 30 DEG C 50 DEG C, is reacted 15 minutes, control lotion pH value is 10 12；When after alkalization, standing, cooling down, after reaching room temperature, 2,2' bipyridyls are added in liquid, are heated up again, to 80 DEG C 120 DEG C, after reacting 1 1.5H, that is, stopped；Liquid carries out decolorization by standing, after cooling treatment, using activated carbon.The present invention is easy to operate, and process safety is reliable, in the case of can stablizing ensureing product quality, realizes the purpose of 2,2 ' dihydroxybiphenyls purifying, the technical blank of in the market has been filled up, suitable for industrialized production.
Description
Technical field
The invention mainly relates to technical field prepared by medicine, and in particular to one kind 2, the purifying side of 2 '-dihydroxybiphenyl
Method.
Background technology
2,2 '-dihydroxybiphenyl is a kind of gray powdery solid, and 108-111 DEG C of fusing point, is dissolved in ethanol, acetic acid second
Ester, dichloromethane etc., insoluble in n-hexane, petroleum ether, benzene.2,2 '-dihydroxybiphenyl structure is present in a lot living with biology
In natural products, medicine and the prodrug and asymmetry catalysis ligand of property.There is very big application in organic synthesis field
Potentiality.
Commercially, 2, the purposes of 2 '-dihydroxybiphenyl is quite varied, since the difference of 2,2 '-dihydroxybiphenyl is made
With, 2, the purifying of 2 '-dihydroxybiphenyl is also to be particularly important, and prepares in the market in existing medicine, there are no on 2,
The technology of 2 '-dihydroxybiphenyl purifying, in order to meet the needs of in the market, it is necessary to develop one kind 2,2 '-dihydroxybiphenyl
Purification technique, to fill up the blank of in the market.
The content of the invention
Invention broadly provides one kind 2, the purification process of 2 '-dihydroxybiphenyl, to solve in above-mentioned background technology
The technical problem of proposition.
The present invention solve the technical solution that uses of above-mentioned technical problem for：One kind 2, the purification process of 2 '-dihydroxybiphenyl,
Purification step is as follows：
（1）First by liquid 2,2 '-dihydroxybiphenyl is added in ionized water, is heated up, after temperature is increased to 50 DEG C -75 DEG C,
Acidulant sulfuric acid is added dropwise, after ten minutes, control acidifying terminal pH value is in 2-3 for reaction；
（2）Step（1）After the acid liquid of middle acquisition stands 30-50 minutes, aqueous slkali is added, after being warming up to 30 DEG C -50 DEG C, instead
Answer 15 minutes, control lotion pH value is in 10-12；
（3）When after alkalization, standing, cooling down, after reaching room temperature, 2,2'- bipyridyls are added in liquid, are heated up again, extremely
80 DEG C -120 DEG C, after reacting 1-1.5H, that is, stop；
（4）By step（3）In liquid by standing, after cooling treatment, utilize activated carbon to carry out decolorization.
Preferably, described 2, the mass ratio of 2 '-dihydroxybiphenyl and the acidulant sulfuric acid is 8：1.
Preferably, the mass ratio of 2 after the acidifying, 2 '-dihydroxybiphenyl and the aqueous slkali is 6：1.
Preferably, described 2, the mass ratio of 2 '-dihydroxybiphenyl and the activated carbon is 80:1.
Preferably, the aqueous slkali is sodium hydroxide and the mixture of potassium hydroxide.
Compared with prior art, beneficial effects of the present invention are：The present invention is easy to operate, and process safety is reliable, Neng Gou
In the case of ensureing that product quality is stablized, 2 are realized, the purpose of 2 '-dihydroxybiphenyl purifying, it is technical to have filled up in the market
Blank, suitable for industrialized production.
Detailed explanation is carried out to the present invention below with reference to specific embodiment.
Embodiment
Embodiment,
（1）First by liquid 2,2 '-dihydroxybiphenyl is added in ionized water, is heated up, after temperature is increased to 50 DEG C -75 DEG C,
Acidulant sulfuric acid is added dropwise, after ten minutes, control acidifying terminal pH value is in 2-3 for reaction；
（2）Step（1）After the acid liquid of middle acquisition stands 30-50 minutes, sodium hydroxide and potassium hydroxide mixture are added, is risen
After warm to 30 DEG C -50 DEG C, react 15 minutes, control lotion pH value is in 10-12；
（3）When after alkalization, standing, cooling down, after reaching room temperature, 2,2'- bipyridyls are added in liquid, are heated up again, extremely
80 DEG C -120 DEG C, after reacting 1-1.5H, that is, stop；
（4）By step（3）In liquid by standing, after cooling treatment, utilize activated carbon to carry out decolorization.
Embodiment described above only expresses certain embodiment of the present invention, its description is more specific and detailed, but simultaneously
Therefore the limitation to the scope of the claims of the present invention cannot be interpreted as.It should be pointed out that for those of ordinary skill in the art
For, without departing from the inventive concept of the premise, various modifications and improvements can be made, these belong to the guarantor of the present invention
Protect scope.Therefore, the protection domain of patent of the present invention should be determined by the appended claims.
Claims (5)
1. one kind 2, the purification process of 2 '-dihydroxybiphenyl, it is characterised in that purification step is as follows：
（1）First by liquid 2,2 '-dihydroxybiphenyl is added in ionized water, is heated up, after temperature is increased to 50 DEG C -75 DEG C,
Acidulant sulfuric acid is added dropwise, after ten minutes, control acidifying terminal pH value is in 2-3 for reaction；
（2）Step（1）After the acid liquid of middle acquisition stands 30-50 minutes, aqueous slkali is added, after being warming up to 30 DEG C -50 DEG C, instead
Answer 15 minutes, control lotion pH value is in 10-12；
（3）When after alkalization, standing, cooling down, after reaching room temperature, 2,2'- bipyridyls are added in liquid, are heated up again, extremely
80 DEG C -120 DEG C, after reacting 1-1.5H, that is, stop；
（4）By step（3）In liquid by standing, after cooling treatment, utilize activated carbon to carry out decolorization.
2. according to claim 1 a kind of 2, the purification process of 2 '-dihydroxybiphenyl, it is characterised in that described 2,2 '-two
The mass ratio of xenol and the acidulant sulfuric acid is 8：1.
3. according to claim 1 a kind of 2, the purification process of 2 '-dihydroxybiphenyl, it is characterised in that after the acidifying
The mass ratio of 2,2 '-dihydroxybiphenyl and the aqueous slkali be 6：1.
4. according to claim 1 a kind of 2, the purification process of 2 '-dihydroxybiphenyl, it is characterised in that described 2,2 '-two
The mass ratio of xenol and the activated carbon is 80:1.
5. according to claim 1 a kind of 2, the purification process of 2 '-dihydroxybiphenyl, it is characterised in that the aqueous slkali
For sodium hydroxide and the mixture of potassium hydroxide.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711172600.6A CN107903151A (en) | 2017-11-22 | 2017-11-22 | A kind of purification process of 2,2 ' dihydroxybiphenyls |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711172600.6A CN107903151A (en) | 2017-11-22 | 2017-11-22 | A kind of purification process of 2,2 ' dihydroxybiphenyls |
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| Publication Number | Publication Date |
|---|---|
| CN107903151A true CN107903151A (en) | 2018-04-13 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201711172600.6A Pending CN107903151A (en) | 2017-11-22 | 2017-11-22 | A kind of purification process of 2,2 ' dihydroxybiphenyls |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20050075519A1 (en) * | 2003-10-07 | 2005-04-07 | General Electric Company | Process for the recovery of dihydroxybiaryl compounds |
| CN101817713A (en) * | 2010-04-30 | 2010-09-01 | 北京欧凯纳斯科技有限公司 | Preparation method of 2, 2'-biphenyl diphenol and derivatives thereof |
| CN104710284A (en) * | 2015-03-09 | 2015-06-17 | 南京理工大学 | Method for preparing 2,2'-dihydroxy diphenyl |
| CN105111049A (en) * | 2015-09-24 | 2015-12-02 | 中国中化股份有限公司 | Preparation method of 2, 2'-dihydroxybiphenyl |
-
2017
- 2017-11-22 CN CN201711172600.6A patent/CN107903151A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20050075519A1 (en) * | 2003-10-07 | 2005-04-07 | General Electric Company | Process for the recovery of dihydroxybiaryl compounds |
| CN1890199A (en) * | 2003-10-07 | 2007-01-03 | 通用电气公司 | Process for the recovery of dihydroxybiaryl compounds |
| CN101817713A (en) * | 2010-04-30 | 2010-09-01 | 北京欧凯纳斯科技有限公司 | Preparation method of 2, 2'-biphenyl diphenol and derivatives thereof |
| CN104710284A (en) * | 2015-03-09 | 2015-06-17 | 南京理工大学 | Method for preparing 2,2'-dihydroxy diphenyl |
| CN105111049A (en) * | 2015-09-24 | 2015-12-02 | 中国中化股份有限公司 | Preparation method of 2, 2'-dihydroxybiphenyl |
Non-Patent Citations (1)
| Title |
|---|
| 耿龙: "从LCP废弃物中回收高纯度4，4’-联苯二酚及4，4’-联苯二酚的合成研究", 《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》 * |
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| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20180413 |