CN101747236A - Technology for synthesizing and purifying p-toluidine-3-sulfonic acid - Google Patents
Technology for synthesizing and purifying p-toluidine-3-sulfonic acid Download PDFInfo
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- CN101747236A CN101747236A CN200810080152A CN200810080152A CN101747236A CN 101747236 A CN101747236 A CN 101747236A CN 200810080152 A CN200810080152 A CN 200810080152A CN 200810080152 A CN200810080152 A CN 200810080152A CN 101747236 A CN101747236 A CN 101747236A
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- totuidine
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Abstract
A technology for synthesizing and purifying p-toluidine-3-sulfonic acid comprises the following steps: adding p-toluidine in concentrated sulfuric acid with the same amount, stirring to react for 2-5 hours at 210-220 DEG C, cooling, curing to obtain crude 4B acid; adding the crude 4B acid in water to stir, adding alkali to neutralize at 10-50 DEG C to ensure that the PH value of the neutralized solution is 7-9 and the 4B acid is completely dissolved; in 4B acid solution, adding activated carbon at 10-50 DEG C and stirring for 30-60 minutes to absorb impurities and decolor, filtering to obtain purified aqueous solution of 4B acid, wherein the content of activated carbon is 30-50wt% of the purified 4B acid; and adding acid in the discolored 4B acid under stirring to ensure that the pH value is 1-2 and white crystals are precipitated, filtering, and washing with water to obtain high purity 4B acid. The method has the advantages of easy method, low cost and high product purity.
Description
Affiliated field
The invention belongs to a kind of synthetic technology that reaches purification para-totuidine-3-sulfonic acid.
Technical background
Para-totuidine-3-sulfonic acid (claiming 4B acid again) is important organic synthesis intermediate, is mainly used in to produce quite material such as bright red 6B and lithol rubine 7B.The method of synthetic 4B acid is more, and how technology early directly bakes and banks up with earth method production with para-totuidine and sulfuric acid under 210--220 ℃; In recent years use instead in high boiling solvent and prepare in the 75-195C sulfonation.But no matter which kind of method all to need in the aqueous solution of 100 ℃ of left and right sides comparatively high tempss, to carry out purifying with.Because 4B acid is easily being decomposed more than 100 ℃, thereby can not get high purity product, and solvent method solvent consumption cost is higher.DF-3401572 in 1985 has reported with the stream acid of being fuming and has prepared the method for high-purity 4B acid 65 ℃ of following sulfonation, because of still there is the high and high shortcoming of corrodibility of cost in a large amount of sulfuric acid of need.
Summary of the invention
It is low to the purpose of this invention is to provide a kind of cost, the highly purified synthetic technology that reaches purification para-totuidine-3-sulfonic acid.
Technology of the present invention is as follows:
(1), para-totuidine is added in the vitriol oil of man equivalent, under 210-220 ℃ temperature condition stirring reaction 2-5 hour, cooling, solidify, the 4B acid crude;
(2), the 4B acid crude of preparation is stirred in water, add alkali neutralization under the 10-50 ℃ of temperature, the pH value of neutralization back solution is 7-9, makes all dissolvings of 4B acid;
(3), in above-mentioned 4B acid solution, temperature is to add gac under the 10-50 ℃ of condition to stir and adsorbed impurity and decolouring in 30-60 minute, filter the 4B aqueous acid of purifying, the amount that adds gac is the 30-50wt% that is purified 4B acid amount;
(4), with the decolouring the 4B acid solution under agitation be acidified with acid to PH=1～2, separate out white crystals, filter, wash high-purity 4B acid.
Described acid can be all kinds of mineral acids, as: sulfuric acid or nitric acid etc. are preferably sulfuric acid.
Described alkali can be mineral alkali, as: yellow soda ash, salt of wormwood, sodium bicarbonate, saleratus, sodium hydroxide or potassium hydroxide etc. are preferably yellow soda ash.
The invention has the advantages that 4B acid synthetic method is easy, cost is low, product purity height (content is greater than 99%).
Embodiment
Embodiment 1: with being heated to 210 ℃ under 200g para-totuidine and the stirring of the 200g vitriol oil, reacted 2 hours, cooling, curing get crude product 4B acid 385g.4B acid crude with above-mentioned 100g, adding people 500ml water stirs and to add people 32g yellow soda ash neutralization (PH=8) to solid in 35 ℃ down and all dissolve, add then after the 50g gac continue to stir half an hour, filter filtrate, add the people 30g vitriol oil to PH=1 under stirring, separate out white crystals, filter, wash the high-purity 4B acid of 76g.
Embodiment 2: with being heated to 220 ℃ under 200g para-totuidine and the stirring of the 200g vitriol oil, reacted 4 hours, cooling, curing get crude product 4B acid 380g.4B acid crude with above-mentioned 100g, adding people 500ml water stirs and to add people 30g sodium hydroxide neutralization (PH=7) to solid in 50 ℃ down and all dissolve, add then after the 40g gac continue to stir half an hour, filter filtrate, add the people 30g vitriol oil to PH=2 under stirring, separate out white crystals, filter, wash the high-purity 4B acid of 80g.
Embodiment 3: with being heated to 215 ℃ under 200g para-totuidine and the stirring of the 200g vitriol oil, reacted 5 hours, cooling, curing get crude product 4B acid 390g.4B acid crude with above-mentioned 100g, adding people 500ml water stirs and to add people 30g saleratus neutralization (PH=9) to solid in 10 ℃ down and all dissolve, add then after the 40g gac continue to stir half an hour, filter filtrate, add people 30g nitric acid to PH=1 under stirring, separate out white crystals, filter, wash the high-purity 4B acid of 85g.
Claims (5)
1. a synthetic technology that reaches purification para-totuidine-3-sulfonic acid is characterized in that comprising the steps:
(1), para-totuidine is added in the vitriol oil of man equivalent, under 210-220 ℃ temperature condition stirring reaction 2-5 hour, cooling, solidify, the 4B acid crude;
(2), the 4B acid crude of preparation is stirred in water, add alkali neutralization under the 10-50 ℃ of temperature, the pH value of neutralization back solution is 7-9, makes all dissolvings of 4B acid;
(3), in above-mentioned 4B acid solution, temperature is to add gac under the 10-50 ℃ of condition to stir and adsorbed impurity and decolouring in 30-60 minute, filter the 4B aqueous acid of purifying, the amount that adds gac is the 30-50wt% that is purified 4B acid amount;
(4), with the decolouring the 4B acid solution under agitation be acidified with acid to PH=1～2, separate out white crystals, filter, wash high-purity 4B acid.
2. a kind of synthetic technology that reaches purification para-totuidine-3-sulfonic acid as claimed in claim 1 is characterized in that described acid is mineral acid.
3. a kind of synthetic technology that reaches purification para-totuidine-3-sulfonic acid as claimed in claim 2 is characterized in that described mineral acid is sulfuric acid or nitric acid.
4. a kind of synthetic technology that reaches purification para-totuidine-3-sulfonic acid as claimed in claim 1 is characterized in that described alkali is mineral alkali.
5. a kind of synthetic technology that reaches purification para-totuidine-3-sulfonic acid as claimed in claim 4 is characterized in that described mineral alkali is yellow soda ash, salt of wormwood, sodium bicarbonate, saleratus, sodium hydroxide or potassium hydroxide.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200810080152A CN101747236A (en) | 2008-12-13 | 2008-12-13 | Technology for synthesizing and purifying p-toluidine-3-sulfonic acid |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200810080152A CN101747236A (en) | 2008-12-13 | 2008-12-13 | Technology for synthesizing and purifying p-toluidine-3-sulfonic acid |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN101747236A true CN101747236A (en) | 2010-06-23 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN200810080152A Pending CN101747236A (en) | 2008-12-13 | 2008-12-13 | Technology for synthesizing and purifying p-toluidine-3-sulfonic acid |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107438582A (en) * | 2015-03-31 | 2017-12-05 | 罗门哈斯公司 | Handle sulfuric acid |
| CN109053500A (en) * | 2018-09-10 | 2018-12-21 | 宜宾市南溪区红源化工有限公司 | A kind of method of liquid alkaline purification 4B acid |
-
2008
- 2008-12-13 CN CN200810080152A patent/CN101747236A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107438582A (en) * | 2015-03-31 | 2017-12-05 | 罗门哈斯公司 | Handle sulfuric acid |
| CN109053500A (en) * | 2018-09-10 | 2018-12-21 | 宜宾市南溪区红源化工有限公司 | A kind of method of liquid alkaline purification 4B acid |
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Open date: 20100623 |