CN109651207A - A kind of T soda acid melts the solution and method of reduction Freund acid generation in reaction - Google Patents
A kind of T soda acid melts the solution and method of reduction Freund acid generation in reaction Download PDFInfo
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- CN109651207A CN109651207A CN201910019770.3A CN201910019770A CN109651207A CN 109651207 A CN109651207 A CN 109651207A CN 201910019770 A CN201910019770 A CN 201910019770A CN 109651207 A CN109651207 A CN 109651207A
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- acid
- freund
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- oxidant
- mass concentration
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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
- C07C303/42—Separation; Purification; Stabilisation; Use of additives
- C07C303/44—Separation; Purification
Abstract
It the invention discloses the solution and method that Freund acid generates is reduced in a kind of molten reaction of T soda acid, solves in tradition H acid production process, alkali fusion uses high-pressure methanol method, and the H acid acid containing Freund produced is more, needs to be cleaned in filtering with a large amount of water.The solution that the present invention uses, according to parts by weight, including following components: liquid alkaline: 10~40 parts；Methanol: 10~40 parts；Oxidant: 0.1~5 part.
Description
Technical field
The present invention relates to H acid to synthesize field, generates it particularly relates to reduce Freund acid in a kind of molten reaction of T soda acid
Solution and method.
Background technique
The H- acid dyestuff intermediate important as one, has the production history of upper a century.H- acid is dyestuff and synthesis doctor
The important source material of medicine.It can preferably be dissolved in the alkaline solutions such as sodium hydroxide, sodium carbonate and ammonia, can send out in acid and alkaline medium
Raw coupling reaction is widely applied in azo dyes synthesis.H- acid (corresponding Chinese: 1- amino-8-naphthol -3,6- disulfonic acid) is main
For producing reactive dye, acid dyes, direct dyes, azo dyestuff, pesticide and drug etc., it to be used for wool spinning, cotton spinning silk weaving
The dyeing of product, fiber product, paper and the contour shelves fabric of bast fibre spinning fabric, purposes are very extensive.H- acid is from coming out till now always
It sells well.2013, with the measure that India shuts down domestic polluted enterprises, India became import by H- acid exported country
State and China supervise the high intensity of heavy polluted industry, so that entire dye industry H- acid is insufficient, dyeing and finishing industry
Involved.Each large enterprises carry out H acid project one after another, lead to H acid excess capacity.Under keen competition, the yield of H acid is improved
It is undoubtedly the most effective method for reducing pollution, improving benefit with product quality.
In traditional H acid production process, alkali fusion uses high-pressure methanol method, the H acid produced containing Freund acid (corresponding Chinese:
1- amino naphthalenes -3,6- disulfonic acid) it is more, it needs to be cleaned in filtering with a large amount of water, it can be qualified.
Summary of the invention
The embodiment of the present invention, which is provided in a kind of molten reaction of T soda acid, reduces the solution and method that Freund acid generates, and solves to pass
In H acid production process of uniting, alkali fusion uses high-pressure methanol method, and the H acid acid containing Freund produced is more, needs in filtering with big
The problem of measuring water cleaning.
In order to realize the above target, the embodiment of the present invention uses following technical scheme:
On the one hand, the embodiment of the present invention, which is provided in a kind of molten reaction of T soda acid, reduces the solution that Freund acid generates, described molten
Liquid according to parts by weight, including following components:
Liquid alkaline: 10~40 parts；
Methanol: 10~40 parts；
Oxidant: 0.1~5 part.
As preference, the mass concentration of the liquid alkaline is 50~90%.
As preference, the mass concentration of the methanol is 80~100%.
As preference, the mass concentration of the oxidant is 10~80%.
As preference, the oxidant is in chlorate, nitrate and metal oxide with oxidizing property
A kind of or any combination.
As preference, the liquid alkaline is sodium hydroxide.
On the other hand, the embodiment of the present invention, which is provided in a kind of molten reaction of T soda acid, reduces the method that Freund acid generates, described
Method includes:
Liquid alkaline, oxidant are added in alkali-melting vessel, and are warming up to 120~180 DEG C；Methanol is added, concentration T acid is added, rises
Temperature is kept for 2~6 hours to 160~200 DEG C, obtains alkali fusion object；
According to parts by weight, the liquid alkaline: 10~40 parts；Methanol: 10~40 parts；Oxidant: 0.1~5 part；T acid is concentrated:
10~60 parts.
As preference, the mass concentration of the liquid alkaline is 50~90%, and the mass concentration of methanol is 80~100%, oxygen
The mass concentration of agent is 10~80%.
As preference, the mass concentration of the concentration T acid is 40~70%.
Compared with prior art, T acid (corresponding Chinese: 1- amino naphthalenes -3,6,9- trisulfonic acid) alkali fusion of the embodiment of the present invention
The solution and method that Freund acid generates are reduced in reaction, generation Freund acid is less, improves final product quality.Existing H acid
When industrial progress T soda acid melts reaction, more Freund acid is generated, thus the problem of influencing yield and final finished quality.This
The solution and method that Freund acid generates are reduced in the molten reaction of the T soda acid of inventive embodiments, Ferund when T soda acid can be made molten
Sour normalizing content is reduced to 1.5% or so from 7% or so.
Specific embodiment
Lower mask body introduces technical solution of the present invention.
The solution that Freund acid generates is reduced in a kind of molten reaction of T soda acid of the embodiment of the present invention, the solution is according to weight
Measure number, including following components:
Liquid alkaline: 10~40 parts；
Methanol: 10~40 parts；
Oxidant: 0.1~5 part.
Above-mentioned solution is for that can reduce the generation of Freund acid, improve the quality of final products in the molten reaction of T soda acid.
In above-described embodiment, the mass concentration of liquid alkaline is 50~90%.The mass concentration of methanol is 80~100%.Oxidation
The mass concentration of agent is 10~80%.
As preference, oxidant is one of chlorate, nitrate and metal oxide with oxidizing property
Or any combination.Oxidant can inhibit the generation of Ferund acid.
As preference, liquid alkaline is sodium hydroxide solution.Liquid alkaline is the main agents of alkali fusion reaction.
Specifically, using above-mentioned solution to the method for reducing the generation of Freund acid in the molten reaction of T soda acid, comprising:
Liquid alkaline, oxidant are added in alkali-melting vessel, and are warming up to 120~180 DEG C；Methanol is added, concentration T acid is added, rises
Temperature is kept for 2~6 hours to 160~200 DEG C, obtains alkali fusion object.Alkali fusion object is the sodium salt of H acid.Alkali fusion reaction be using liquid alkaline and
Methanol forms sodium alkoxide, then the sulfonic acid group of attack naphthalene, and nucleophilic substitution occurs, and sulfonic group becomes inferior sulfate radical, and sodium alkoxide becomes
At the phenolic hydroxyl group of methanol and naphthalene.
According to parts by weight, the liquid alkaline: 10~40 parts；Methanol: 10~40 parts；Oxidant: 0.1~5 part；T acid is concentrated:
10~60 parts.
In the above-mentioned methods, the mass concentration of the liquid alkaline is 50~90%, and the mass concentration of methanol is 80~100%,
The mass concentration of oxidant is 10~80%, and the mass concentration of concentration T acid is 40~70%.
In the method for the embodiment of the present invention, oxidant is added, so that impurity F reund acid is few in final product, filtering needs
The few advantage of filter cake wash water.Without the addition of an oxidizing agent, Ferund acid content is very high.
Less, the final product purity below by Freund acid in the final product of verification experimental verification method preparation of the invention
Higher advantage.
Example 1
A kind of method that T soda acid melts reduction Freund acid generation in reaction, comprising:
Liquid alkaline, oxidant are added in alkali-melting vessel, and are warming up to 120 DEG C；Methanol is added, concentration T acid is added, is warming up to
It 170 DEG C, is kept for 2 hours, obtains alkali fusion object.Wherein, according to parts by weight, liquid alkaline: 15 parts；Methanol: 10 parts；Oxidant: 3 parts；
It is sour that T is concentrated: 20 parts.The mass concentration of liquid alkaline is 50%, and the mass concentration of methanol is 80%, and the mass concentration of oxidant is
20%, the mass concentration of concentration T acid is 50%.
Example 2
A kind of method that T soda acid melts reduction Freund acid generation in reaction, comprising:
Liquid alkaline, oxidant are added in alkali-melting vessel, and are warming up to 180 DEG C；Methanol is added, concentration T acid is added, is warming up to
It 200 DEG C, is kept for 5 hours, obtains alkali fusion object.Wherein, according to parts by weight, liquid alkaline: 30 parts；Methanol: 20 parts；Oxidant: 0.1
Part；It is sour that T is concentrated: 10 parts.The mass concentration of liquid alkaline is 60%, and the mass concentration of methanol is 100%, and the mass concentration of oxidant is
80%, the mass concentration of concentration T acid is 70%.
Example 3
A kind of method that T soda acid melts reduction Freund acid generation in reaction, comprising:
Liquid alkaline, oxidant are added in alkali-melting vessel, and are warming up to 160 DEG C；Methanol is added, concentration T acid is added, is warming up to
It 190 DEG C, is kept for 6 hours, obtains alkali fusion object.Wherein, according to parts by weight, liquid alkaline: 40 parts；Methanol: 20 parts；Oxidant: 1 part；
It is sour that T is concentrated: 60 parts.The mass concentration of liquid alkaline is 80%, and the mass concentration of methanol is 85%, and the mass concentration of oxidant is
60%, the mass concentration of concentration T acid is 65%.
Example 4
A kind of method that T soda acid melts reduction Freund acid generation in reaction, comprising:
Liquid alkaline, oxidant are added in alkali-melting vessel, and are warming up to 150 DEG C；Methanol is added, concentration T acid is added, is warming up to
It 160 DEG C, is kept for 4 hours, obtains alkali fusion object.Wherein, according to parts by weight, liquid alkaline: 10 parts；Methanol: 40 parts；Oxidant: 5 parts；
It is sour that T is concentrated: 40 parts.The mass concentration of liquid alkaline is 90%, and the mass concentration of methanol is 90%, and the mass concentration of oxidant is
10%, the mass concentration of concentration T acid is 40%.
Example 5
A kind of method that T soda acid melts reduction Freund acid generation in reaction, comprising:
Liquid alkaline, oxidant are added in alkali-melting vessel, and are warming up to 170 DEG C；Methanol is added, concentration T acid is added, is warming up to
It 185 DEG C, is kept for 3 hours, obtains alkali fusion object.Wherein, according to parts by weight, liquid alkaline: 25 parts；Methanol: 30 parts；Oxidant: 2 parts；
It is sour that T is concentrated: 50 parts.The mass concentration of liquid alkaline is 70%, and the mass concentration of methanol is 95%, and the mass concentration of oxidant is
50%, the mass concentration of concentration T acid is 60%.
Comparative example 1
It is identical as example 1, but that oxidant is not added.
Comparative example 2
It is identical as example 2, but that oxidant is not added.
Comparative example 3
It is identical as example 3, but that oxidant is not added.
With the area normalization method method of high performance liquid chromatography detection, the alkali of above-mentioned 5 examples and the preparation of 3 comparative examples is detected
Ferund acid normalizing content in fusant, as shown in table 1.
Table 1
As can be seen from Table 1: using the method for the embodiment of the present invention, Ferund acid normalizing content is less than in alkali fusion object
1.8%.Using the method for comparative example, Ferund acid normalizing content is greater than 6.8% in alkali fusion object.Therefore, implemented using the present invention
The method of example, can effectively reduce Ferund acid content in alkali fusion object.
Claims (9)
1. reducing the solution that Freund acid generates in a kind of molten reaction of T soda acid, which is characterized in that the solution is according to parts by weight
Number, including following components:
Liquid alkaline: 10~40 parts；
Methanol: 10~40 parts；
Oxidant: 0.1~5 part.
2. reducing the solution that Freund acid generates in the molten reaction of T soda acid described in accordance with the claim 1, which is characterized in that described
The mass concentration of liquid alkaline is 50~90%.
3. reducing the solution that Freund acid generates in the molten reaction of T soda acid described in accordance with the claim 1, which is characterized in that described
The mass concentration of methanol is 80~100%.
4. reducing the solution that Freund acid generates in the molten reaction of T soda acid described in accordance with the claim 1, which is characterized in that described
The mass concentration of oxidant is 10~80%.
5. reducing the solution that Freund acid generates in the molten reaction of T soda acid described in accordance with the claim 1, which is characterized in that described
Oxidant is one of chlorate, nitrate and metal oxide with oxidizing property or any combination.
6. reducing the solution that Freund acid generates in the molten reaction of T soda acid described in accordance with the claim 1, which is characterized in that described
Liquid alkaline is sodium hydroxide.
7. reducing the method that Freund acid generates in a kind of molten reaction of T soda acid, which is characterized in that the described method includes:
Liquid alkaline, oxidant are added in alkali-melting vessel, and are warming up to 120~180 DEG C；Methanol is added, concentration T acid is added, is warming up to
It 160~200 DEG C, is kept for 2~6 hours, obtains alkali fusion object；
According to parts by weight, the liquid alkaline: 10~40 parts；Methanol: 10~40 parts；Oxidant: 0.1~5 part；It is sour that T is concentrated: 10~
60 parts.
8. reducing the method that Freund acid generates in the molten reaction of T soda acid according to claim 7, which is characterized in that described
The mass concentration of liquid alkaline is 50~90%, and the mass concentration of methanol is 80~100%, and the mass concentration of oxidant is 10~80%.
9. reducing the method that Freund acid generates in the molten reaction of T soda acid according to claim 7, which is characterized in that described
The mass concentration that T acid is concentrated is 40~70%.
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| CN201910019770.3A CN109651207A (en) | 2019-01-09 | 2019-01-09 | A kind of T soda acid melts the solution and method of reduction Freund acid generation in reaction |
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS58135849A (en) * | 1982-02-05 | 1983-08-12 | Sumitomo Chem Co Ltd | Preparation of 1-amino-8-naphthol-3,6-disulfonic acid mono-alkali metal salt |
| CN101367752A (en) * | 2008-10-15 | 2009-02-18 | 湖北楚源高新科技股份有限公司 | Novel high pressure alkali fusion production process for H acid |
| CN101381331A (en) * | 2008-10-27 | 2009-03-11 | 泰兴锦汇化工有限公司 | Method for preparing color-forming intermediate H acids |
| CN108003071A (en) * | 2017-12-04 | 2018-05-08 | 大柴旦乐青科技化学有限公司 | A kind of H acid high pressure alkali fusion technique |
| CN108191715A (en) * | 2017-11-27 | 2018-06-22 | 江苏力禾颜料有限公司 | High pressure alkali fusion preparation process |
| CN109096154A (en) * | 2018-08-16 | 2018-12-28 | 山东裕源集团有限公司 | A kind of H acid production process |
-
2019
- 2019-01-09 CN CN201910019770.3A patent/CN109651207A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS58135849A (en) * | 1982-02-05 | 1983-08-12 | Sumitomo Chem Co Ltd | Preparation of 1-amino-8-naphthol-3,6-disulfonic acid mono-alkali metal salt |
| CN101367752A (en) * | 2008-10-15 | 2009-02-18 | 湖北楚源高新科技股份有限公司 | Novel high pressure alkali fusion production process for H acid |
| CN101381331A (en) * | 2008-10-27 | 2009-03-11 | 泰兴锦汇化工有限公司 | Method for preparing color-forming intermediate H acids |
| CN108191715A (en) * | 2017-11-27 | 2018-06-22 | 江苏力禾颜料有限公司 | High pressure alkali fusion preparation process |
| CN108003071A (en) * | 2017-12-04 | 2018-05-08 | 大柴旦乐青科技化学有限公司 | A kind of H acid high pressure alkali fusion technique |
| CN109096154A (en) * | 2018-08-16 | 2018-12-28 | 山东裕源集团有限公司 | A kind of H acid production process |
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