CN106810474A - A kind of preparation method of Xue Fo Shi sodium salts - Google Patents
A kind of preparation method of Xue Fo Shi sodium salts Download PDFInfo
- Publication number
- CN106810474A CN106810474A CN201710043521.9A CN201710043521A CN106810474A CN 106810474 A CN106810474 A CN 106810474A CN 201710043521 A CN201710043521 A CN 201710043521A CN 106810474 A CN106810474 A CN 106810474A
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- CN
- China
- Prior art keywords
- xue
- shi
- sodium salts
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- dephenolize
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C303/00—Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides
- C07C303/32—Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides of salts of sulfonic acids
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C303/00—Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides
- C07C303/02—Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides of sulfonic acids or halides thereof
- C07C303/04—Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides of sulfonic acids or halides thereof by substitution of hydrogen atoms by sulfo or halosulfonyl groups
- C07C303/06—Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides of sulfonic acids or halides thereof by substitution of hydrogen atoms by sulfo or halosulfonyl groups by reaction with sulfuric acid or sulfur trioxide
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C303/00—Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides
- C07C303/02—Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides of sulfonic acids or halides thereof
- C07C303/22—Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides of sulfonic acids or halides thereof from sulfonic acids, by reactions not involving the formation of sulfo or halosulfonyl groups; from sulfonic halides by reactions not involving the formation of halosulfonyl groups
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention provides a kind of preparation method of Xue Fo Shi sodium salts, it comprises the following steps：2 naphthols and the concentrated sulfuric acid are carried out into sulfonating reaction at 100 DEG C, sulfonated bodies is obtained；The sulfonated bodies is dissolved in the water, activated carbon is added, dephenolize is carried out at 60 DEG C, obtain dephenolize product；In being 9 alkaline solution by dephenolize product addition pH value, activated carbon is added, quaternization is carried out at 80~90 DEG C, obtain the product that alkalizes；After by the alkalization product regulation pH value to 3~6, saltoutd, obtained precipitate；The precipitate is washed, Xue Fo Shi salt is obtained.Compared with prior art, the present invention has following beneficial effect：Based on the principle that the present invention is with activated carbon as adsorbent, increase by two step purifying technique processes, and control sulfonating reaction time and temperature, high-purity and Xue's Fo Shi sodium salts in high yield can be obtained.
Description
Technical field
The present invention relates to a kind of preparation method of Xue Fo Shi sodium salts, belong to technical field of organic synthesis.
Background technology
Xue's Fo Shi sodium salts are a kind of important chemical intermediates, mainly for the manufacture of dyestuff, including acid dyes orange, acidity
Dyestuff is red, acid dyes is black, direct dyes is blue and food coloring lemon yellow.
Traditional handicraft synthesizes that its sulfonation time during Xue's Fo Shi sodium salts is long, it is necessary to substantial amounts of sulfuric acid, and product purity is low,
Outward appearance is dark-coloured in ash, and color is deeper, and R salt contents are higher.Particularly it is used for synthetic food colors lemon yellow, to Xue's Fo Shi sodium salts
Purity requirement is higher.
The content of the invention
For defect of the prior art, it is an object of the invention to provide a kind of preparation method of Xue Fo Shi sodium salts.
The present invention is achieved by the following technical solutions：
The invention provides a kind of preparation method of Xue Fo Shi sodium salts, it comprises the following steps：
Beta naphthal and the concentrated sulfuric acid are carried out into sulfonating reaction at 100 DEG C, sulfonated bodies is obtained；
The sulfonated bodies is dissolved in the water, activated carbon is added, dephenolize is carried out at 60 DEG C, obtain dephenolize product；
In being 9 alkaline solution by dephenolize product addition pH value, activated carbon is added, alkalized at 80~90 DEG C
Reaction, obtains the product that alkalizes；
After by the alkalization product regulation pH value to 3~6, saltoutd, obtained precipitate；
The precipitate is washed, Xue Fo Shi salt is obtained.
Preferably, the mass fraction of the concentrated sulfuric acid is 98%.
Preferably, the mass fraction of the alkaline solution is 30%.
Preferably, the alkaline solution is sodium hydroxide solution.
Compared with prior art, the present invention has following beneficial effect：
1st, substantial amounts of 6,6 ' two (2- naphthalene sulfonate salts) ethers (DONS), unreacted beta naphthal are contained during traditional handicraft
With the impurity such as R salt, it is impossible to meet the requirement of Vehicles Collected from Market.
2nd, based on the principle that the present invention is with activated carbon as adsorbent, increase by two step purifying technique processes, and control sulphur
Change reaction time and temperature, high-purity and Xue's Fo Shi sodium salts in high yield can be obtained.
Specific embodiment
With reference to specific embodiment, the present invention is described in detail.Following examples will be helpful to the technology of this area
Personnel further understand the present invention, but the invention is not limited in any way.It should be pointed out that to the ordinary skill of this area
For personnel, without departing from the inventive concept of the premise, various modifications and improvements can be made.These belong to the present invention
Protection domain.
Embodiment 1
The present embodiment is related to a kind of preparation method of Xue Fo Shi sodium salts, and it comprises the following steps：
(1) sulfonation process
Beta naphthal and 98% sulfuric acid are reacted 3.5 hours in 100 DEG C；
(2) dephenolize process is diluted
Above-mentioned sulfonation material is immersed in the water, 60 DEG C are heated to, until all dissolvings.It is subsequently adding activated carbon insulation 1 small
When, filter to obtain clarified mother liquor；
(3) alkalinization
Then the pH for adding sodium hydroxide solution regulation solution is 9, at 80 DEG C, adds activated carbon to be incubated 0.5 hour, mistake
Filter, if mother liquor is not clarified, filters, untill clarification again；
(4) salting-out process
Above-mentioned mother liquor dilute sulfuric acid regulation pH is 3~6, adds sodium chloride to saltout, and filters precipitate；
(5) wash
Above-mentioned precipitate is cleaned with water and filters to obtain Xue's Fo Shi sodium salts.
The yield of Xue's Fo Shi sodium salts be 98%, purity 99% and more than.
Embodiment 2
The present embodiment is related to a kind of preparation method of Xue Fo Shi sodium salts, and it comprises the following steps：
(1) sulfonation process
Beta naphthal and 98% sulfuric acid are reacted 3.5 hours in 100 DEG C；
(2) dephenolize process is diluted
Above-mentioned sulfonation material is immersed in the water, 60 DEG C are heated to, until all dissolvings.It is subsequently adding activated carbon insulation 1 small
When, filter to obtain clarified mother liquor；
(3) alkalinization
Then the pH for adding sodium hydroxide solution regulation solution is 9, at 90 DEG C, adds activated carbon to be incubated 0.5 hour, mistake
Filter, if mother liquor is not clarified, filters, untill clarification again；
(4) salting-out process
Above-mentioned mother liquor dilute sulfuric acid regulation pH is 3~6, adds sodium chloride to saltout, and filters precipitate；
(5) wash
Above-mentioned precipitate is cleaned with water and filters to obtain Xue's Fo Shi sodium salts.
The yield of Xue's Fo Shi sodium salts be 98%, purity 99% and more than.
Embodiment 3
The present embodiment is related to a kind of preparation method of Xue Fo Shi sodium salts, and it comprises the following steps：
(1) sulfonation process
Beta naphthal and 98% sulfuric acid are reacted 3.5 hours in 100 DEG C；
(2) dephenolize process is diluted
Above-mentioned sulfonation material is immersed in the water, 60 DEG C are heated to, until all dissolvings.It is subsequently adding activated carbon insulation 1 small
When, filter to obtain clarified mother liquor；
(3) alkalinization
Then the pH for adding sodium hydroxide solution regulation solution is 9, at 85 DEG C, adds activated carbon to be incubated 0.5 hour, mistake
Filter, if mother liquor is not clarified, filters, untill clarification again；
(4) salting-out process
Above-mentioned mother liquor dilute sulfuric acid regulation pH is 3~6, adds sodium chloride to saltout, and filters precipitate；
(5) wash
Above-mentioned precipitate is cleaned with water and filters to obtain Xue's Fo Shi sodium salts.
The yield of Xue's Fo Shi sodium salts be 98%, purity 99% and more than.
Specific embodiment of the invention is described above.It is to be appreciated that the invention is not limited in above-mentioned
Particular implementation, those skilled in the art can within the scope of the claims make various deformations or amendments, this not shadow
Sound substance of the invention.
Claims (4)
1. a kind of preparation method of Xue Fo Shi sodium salts, it is characterised in that comprise the following steps：
Beta naphthal and the concentrated sulfuric acid are carried out into sulfonating reaction at 100 DEG C, sulfonated bodies is obtained；
The sulfonated bodies is dissolved in the water, activated carbon is added, dephenolize is carried out at 60 DEG C, obtain dephenolize product；
In being 9 alkaline solution by dephenolize product addition pH value, activated carbon is added, carry out alkalizing at 80~90 DEG C anti-
Should, obtain the product that alkalizes；
After by the alkalization product regulation pH value to 3~6, saltoutd, obtained precipitate；
The precipitate is washed, Xue Fo Shi salt is obtained.
2. the preparation method of Xue Fo Shi sodium salts as claimed in claim 1, it is characterised in that the mass fraction of the concentrated sulfuric acid is
98%.
3. the preparation method of Xue Fo Shi sodium salts as claimed in claim 1, it is characterised in that the mass fraction of the alkaline solution
It is 30%.
4. the preparation method of Xue's Fo Shi sodium salts as described in claim 1 or 3, it is characterised in that the alkaline solution is hydrogen-oxygen
Change sodium solution.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710043521.9A CN106810474A (en) | 2017-01-19 | 2017-01-19 | A kind of preparation method of Xue Fo Shi sodium salts |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201710043521.9A CN106810474A (en) | 2017-01-19 | 2017-01-19 | A kind of preparation method of Xue Fo Shi sodium salts |
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| CN106810474A true CN106810474A (en) | 2017-06-09 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107963986A (en) * | 2017-11-30 | 2018-04-27 | 浙江龙盛化工研究有限公司 | A kind of method of co-producing high-purity Xue Fo Shi salt and G salt |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CA964280A (en) * | 1971-02-16 | 1975-03-11 | American Cyanamid Company | Recovery of pure schaeffer's salt from crude sulfonation mixtures |
| US3994963A (en) * | 1975-02-28 | 1976-11-30 | American Cyanamid Company | Schaeffer salt purification |
| CN102391161A (en) * | 2011-12-28 | 2012-03-28 | 湖北鑫慧化工有限公司 | Process for preparing amino G acid |
-
2017
- 2017-01-19 CN CN201710043521.9A patent/CN106810474A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CA964280A (en) * | 1971-02-16 | 1975-03-11 | American Cyanamid Company | Recovery of pure schaeffer's salt from crude sulfonation mixtures |
| US3994963A (en) * | 1975-02-28 | 1976-11-30 | American Cyanamid Company | Schaeffer salt purification |
| CN102391161A (en) * | 2011-12-28 | 2012-03-28 | 湖北鑫慧化工有限公司 | Process for preparing amino G acid |
Non-Patent Citations (3)
| Title |
|---|
| 李秀顺: "薛佛氏盐生产中磺化工艺的改进", 《江苏化工》 * |
| 袁金华等: "乙萘酚及其衍生物的制备", 《辽宁化工》 * |
| 陶显宏等: "高浓度薛佛氏盐生产废水的资源化处理工艺研究", 《环境科学与技术》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107963986A (en) * | 2017-11-30 | 2018-04-27 | 浙江龙盛化工研究有限公司 | A kind of method of co-producing high-purity Xue Fo Shi salt and G salt |
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Application publication date: 20170609 |