CN102219651A - Preparation method of 2,6-dihydroxy naphthalene - Google Patents
Preparation method of 2,6-dihydroxy naphthalene Download PDFInfo
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- CN102219651A CN102219651A CN2011101033085A CN201110103308A CN102219651A CN 102219651 A CN102219651 A CN 102219651A CN 2011101033085 A CN2011101033085 A CN 2011101033085A CN 201110103308 A CN201110103308 A CN 201110103308A CN 102219651 A CN102219651 A CN 102219651A
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Abstract
The invention discloses a preparation method of 2,6-dihydroxy naphthalene, which comprises the steps of: adding 98% of KOH and NaOH to a reaction kettle, heating, adding 2,6-naphthalenedisulfonic acid disodium salt and phenol, heating up to 345 to 355 DEG C and then performing reaction, cooling materials to 260 to 270 DEG C upon the completion of the reaction, adding water to dissolve the materials, then regulating an alkali fusion diluting material to a range from 1.17g/cm<3> to 1.19g/cm<3> with water, neutralizing with an sulfuric acid aqueous solution to the condition that the pH is 2 to 3, cooling, filtering and drying by pumping to obtain the crude 2,6-dihydroxy naphthalene. According to the method, a small quantity of phenol is added as an antioxidant during high temperature alkali fusion of 2,6-naphthalenedisulfonic acid disodium salt and mixed alkali, thus the generated 2,6-naphthalenediphenol sodium (potassium) is prevented from oxidation, the selectivity of the 2,6-naphthalenedisulfonic acid disodium salt is improved and the product purity is high.
Description
Technical field
The present invention relates to a kind of 2, the preparation method of 6-dihydroxy naphthlene.
Background technology
2, the 6-dihydroxy naphthlene is a kind of important medicine intermediate.Because 2, generate in 6-naphthalene disulfonate and the mixed base high temperature alkali fuse process 2,6-naphthalenediol sodium (potassium) very easily oxidation becomes tar, directly influences 2, the selectivity of 6-dihydroxy naphthlene.
Summary of the invention
The object of the present invention is to provide a kind of product purity high 2, the preparation method of 6-dihydroxy naphthlene.
Technical solution of the present invention is:
A kind of 2, the preparation method of 6-dihydroxy naphthlene is characterized in that: in reactor, add 90%KOH, 98%NaOH, heating, add 2,6-naphthalene disulfonate and phenol are warmed up to reaction between 345～355 ℃, reaction finishes, material is cooled to 260 ~ 270 ℃, the material that is dissolved in water, and water is adjusted to 1.17 ~ 1.19g/cm with alkali fusion dilution material again
3Between, being neutralized to pH value with aqueous sulfuric acid is 2 ~ 3, cooling is filtered, and drains, and gets 2,6-dihydroxy naphthlene crude product.
The present invention is 2, adds a spot of phenol in 6-naphthalene disulfonate and the mixed base high temperature alkali fuse process as antioxidant, prevent to generate 2,6-naphthalenediol sodium (potassium) oxidation improves 2, the selectivity of 6-naphthalene disulfonate, product purity height.
The invention will be further described below in conjunction with embodiment.
Embodiment
In the 2000L stainless steel cauldron, add 90%KOH523g, 98%NaOH523g is heated to 260 ℃, add 2,6-naphthalene disulfonate 332g(content is 75%, and purity is 94%) and phenol 52g, be warmed up between 345～355 ℃ and react 3h, reaction finishes, material is cooled to 260 ~ 270 ℃, adds 4000ml water dissolution material, and water is adjusted to 1.17 ~ 1.19g/cm with alkali fusion dilution material again
3Between, with content be 38% aqueous sulfuric acid to be neutralized to pH value be 2 ~ 3, be cooled to 25 ℃, filter, drain, get 2,6-dihydroxy naphthlene crude product 253g(organic content is 62%, 2,6-dihydroxy naphthlene purity is 88.32%, is elaboration more than 98% by the refining purity that becomes.）。
By comparing, under other conditions situation identical with embodiment, 2, do not add antioxidant phenol in 6-naphthalene disulfonate and the mixed base high temperature alkali fuse process, get 2,6-dihydroxy naphthlene crude product 206g(organic content is 64.3%, and purity is 72.28%, is about 92% elaboration by the refining purity that can only become.）。
Claims (1)
1. one kind 2, the preparation method of 6-dihydroxy naphthlene is characterized in that: in reactor, add 90%KOH, 98%NaOH, heating, add 2,6-naphthalene disulfonate and phenol are warmed up to reaction between 345～355 ℃, reaction finishes, material is cooled to 260 ~ 270 ℃, the material that is dissolved in water, and water is adjusted to 1.17 ~ 1.19g/cm with alkali fusion dilution material again
3Between, being neutralized to pH value with aqueous sulfuric acid is 2 ~ 3, cooling is filtered, and drains, and gets 2,6-dihydroxy naphthlene crude product.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011101033085A CN102219651A (en) | 2011-04-25 | 2011-04-25 | Preparation method of 2,6-dihydroxy naphthalene |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011101033085A CN102219651A (en) | 2011-04-25 | 2011-04-25 | Preparation method of 2,6-dihydroxy naphthalene |
Publications (1)
| Publication Number | Publication Date |
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| CN102219651A true CN102219651A (en) | 2011-10-19 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN2011101033085A Pending CN102219651A (en) | 2011-04-25 | 2011-04-25 | Preparation method of 2,6-dihydroxy naphthalene |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102442888A (en) * | 2011-11-10 | 2012-05-09 | 丹东深兰化工有限公司 | Method for producing 1,5-dihydroxy naphthalene |
| CN103467250A (en) * | 2013-09-25 | 2013-12-25 | 南通柏盛化工有限公司 | Preparation method of 1,7-dihydroxy naphthlene |
| CN104844425A (en) * | 2015-04-20 | 2015-08-19 | 南通柏盛化工有限公司 | Synthetic method of 2,6 dihydroxy naphthlene |
| CN106187835A (en) * | 2016-07-14 | 2016-12-07 | 江苏扬农化工集团有限公司 | 2,3 dihydroxy naphthlene 1,6 disulfonic acid chemical intermediate synthetic methods |
| CN106588575A (en) * | 2016-12-02 | 2017-04-26 | 沈阳化工研究院有限公司 | Preparation method of 2,6-dihydroxynaphthalene |
| CN108299162A (en) * | 2018-01-22 | 2018-07-20 | 南通柏盛化工有限公司 | A kind of preparation process of synthesis 2,6- dihydroxy naphthlenes |
| CN111018676A (en) * | 2019-12-11 | 2020-04-17 | 乌海时联环保科技有限责任公司 | Method for preventing resorcinol from discoloring |
| CN111116319A (en) * | 2019-12-17 | 2020-05-08 | 枣庄市泰瑞精细化工有限公司 | Synthesis and refining method of high-purity 1, 6-dihydroxynaphthalene |
| CN113929561A (en) * | 2020-06-29 | 2022-01-14 | 王兴路 | Alkali fusion method for preparing phenolic compound |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH03258739A (en) * | 1990-03-08 | 1991-11-19 | Kawasaki Steel Corp | Production of 2,6-naphthalenediol |
-
2011
- 2011-04-25 CN CN2011101033085A patent/CN102219651A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH03258739A (en) * | 1990-03-08 | 1991-11-19 | Kawasaki Steel Corp | Production of 2,6-naphthalenediol |
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102442888A (en) * | 2011-11-10 | 2012-05-09 | 丹东深兰化工有限公司 | Method for producing 1,5-dihydroxy naphthalene |
| CN102442888B (en) * | 2011-11-10 | 2014-03-26 | 丹东深兰化工有限公司 | Method for producing 1,5-dihydroxy naphthalene |
| CN103467250A (en) * | 2013-09-25 | 2013-12-25 | 南通柏盛化工有限公司 | Preparation method of 1,7-dihydroxy naphthlene |
| CN104844425A (en) * | 2015-04-20 | 2015-08-19 | 南通柏盛化工有限公司 | Synthetic method of 2,6 dihydroxy naphthlene |
| CN106187835A (en) * | 2016-07-14 | 2016-12-07 | 江苏扬农化工集团有限公司 | 2,3 dihydroxy naphthlene 1,6 disulfonic acid chemical intermediate synthetic methods |
| CN106588575A (en) * | 2016-12-02 | 2017-04-26 | 沈阳化工研究院有限公司 | Preparation method of 2,6-dihydroxynaphthalene |
| CN108299162A (en) * | 2018-01-22 | 2018-07-20 | 南通柏盛化工有限公司 | A kind of preparation process of synthesis 2,6- dihydroxy naphthlenes |
| CN108299162B (en) * | 2018-01-22 | 2021-01-12 | 南通柏盛化工有限公司 | Preparation process for synthesizing 2, 6-dihydroxynaphthalene |
| CN111018676A (en) * | 2019-12-11 | 2020-04-17 | 乌海时联环保科技有限责任公司 | Method for preventing resorcinol from discoloring |
| CN111116319A (en) * | 2019-12-17 | 2020-05-08 | 枣庄市泰瑞精细化工有限公司 | Synthesis and refining method of high-purity 1, 6-dihydroxynaphthalene |
| CN111116319B (en) * | 2019-12-17 | 2023-02-03 | 枣庄市泰瑞精细化工有限公司 | Synthesis and refining method of 1, 6-dihydroxynaphthalene |
| CN113929561A (en) * | 2020-06-29 | 2022-01-14 | 王兴路 | Alkali fusion method for preparing phenolic compound |
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Application publication date: 20111019 |