CN1130624A - Synthetic method and purifying technique for high-purity p-toluidine-3-sulfonic acid (4B acid) - Google Patents
Synthetic method and purifying technique for high-purity p-toluidine-3-sulfonic acid (4B acid) Download PDFInfo
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- CN1130624A CN1130624A CN 95115450 CN95115450A CN1130624A CN 1130624 A CN1130624 A CN 1130624A CN 95115450 CN95115450 CN 95115450 CN 95115450 A CN95115450 A CN 95115450A CN 1130624 A CN1130624 A CN 1130624A
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Abstract
A synthesis and purification process of high-purity p-toluidine-3-sulfonic acid (4B acid) as intermediate to synthesize pigment includes such steps as direct roasting of p-toluidine and concentrated sulfuric acid to obtain coarse 4B acid, dissolving in aqueous solution by alkali neutralization, adsorbing impurities in sodium salt solution of 4B acid and decolouring by activated carbon, and acid educing to obtain 99% 4B acid. It features simple synthetic method, low cost and high purity.
Description
The present invention relates to a kind of synthetic method and purification techniques of pigment organic synthesis intermediate.
4B acid is important organic synthesis intermediate, is mainly used in pigment such as producing 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 ℃, uses instead in recent years in high boiling solvent to prepare in 175～195 ℃ of 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 decomposed under this condition, thereby can not get high purity product, and solvent method solvent consumption cost is higher.DE3401572 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 shortcoming of cost in a large amount of sulfuric acid of need.
The objective of the invention is to solve the problem that product purity is low or cost is high that exists in the existing synthetic method, a kind of improved synthetic and purification process is provided, reach and reduce cost, improve purity and synthetic easy purpose.
Of the present invention synthesizing with method of purification is: be raw material with the para-totuidine and the vitriol oil at first, prepare the 4B acid crude through direct baking process(of sulfonation), in the aqueous solution, make the dissolving of 4B acid crude again with the alkali neutralization, with gac the 4B acid sodium-salt aqueous solution is carried out impurity absorption, the decolouring purifying, last acid out gets high-purity 4B acid.
The present invention is synthetic, the detailed route map of purifying is as follows:
Now method steps of the present invention is further described in conjunction with above-mentioned route map.
Step I
Para-totuidine is added in the vitriol oil of equivalent, stirring reaction is 2 hours under 210 °～220 ℃ temperature condition, and cooling, curing get the 4B acid crude.
Step II
(1) the 4B acid crude of preparation or general industry product 4B acid are stirred in water and add alkali neutralization, make that 4B acid is whole dissolves.Be used for and the alkali of 4B acid can be all kinds of mineral alkalis, as: yellow soda ash, salt of wormwood, sodium bicarbonate, saleratus, sodium hydroxide and potassium hydroxide etc. are preferably yellow soda ash, and the pH value of neutralization back solution is 7～9, is preferably 8;
(2) the above-mentioned 4B acid sodium-salt aqueous solution is added gac and stir 30 minutes after-filtration, get the 4B acid sodium-salt aqueous solution of purifying.The consumption that is used to adsorb the gac of impurity and decolouring is to be purified 15～20% of 4B acid amount.
(3) be acidified with acid to PH=1～2 under the 4B acid sodium-salt solution stirring with purifying, separate out white crystals, filter, wash high-purity 4B acid.The acid that is used for acid out can be all kinds of mineral acids, as: sulfuric acid, hydrochloric acid and nitric acid etc. are preferably sulfuric acid.
The temperature of the neutralization of (1) alkali, (2) activated carbon decolorizing and (3) acid out is 10～80 ℃ in the Step II; Be preferably 60～70 ℃.
The invention has the advantages that 4B acid synthetic method is easy, cost is low, product purity height (content is greater than 99%).
Embodiment 1:
Be heated to 210 °～220 ℃ under the vitriol oil stirring with 100g para-totuidine and 100g92%, reacted 2 hours, cooling, curing get crude product 4B acid 185g.4B acid crude with above-mentioned 100g, adding the stirring of 500m1 water all dissolves in 65 ℃ of adding 32g yellow soda ash neutralizations (PH=8) to solid down, add then after the 20g gac continue to stir half an hour, filter the filtrate stirring and add the vitriol oil of 30g98% to PH=1 down, separate out white crystals, filter, wash 76g elaboration 4B acid.
Embodiment 2:
100g industrial goods 4B acid is added 500ml water, stir down and add 29g yellow soda ash in 65 ℃, PH=8, adding the 15g gac again to the solid dissolving continues to stir half an hour, filter filtrate and stir that the dense stream that adds 30g98% down is sour separates out white crystals to PH=1, filter, wash, get 84g elaboration 4B acid.
Claims (5)
1. the method for synthetic, a purifying para-totuidine-3-sulfonic acid (4B acid), it is characterized in that being raw material with para-totuidine and dense stream acid earlier, prepare the 4B acid crude through direct baking process(of sulfonation), in the aqueous solution, use again in the alkali and and dissolve crude product or general industry product 4B acid, with gac the 4B acid sodium-salt aqueous solution is carried out impurity absorption, decolouring purifying, get high-purity 4B acid with acid out at last.
2. the method for synthetic, purifying para-totuidine-3-sulfonic acid (4B acid) according to claim 1 is characterized in that being used for and the alkali of 4B acid, can be all kinds of mineral alkalis, is preferably yellow soda ash, and the pH value of neutralization back solution is 7～9, is preferably 8.
3. the method for synthetic, purifying para-totuidine-3-sulfonic acid (4B acid) according to claim 1, the consumption that it is characterized in that adsorbing the gac of impurity and decolouring usefulness be purified 4B acid amount 15～20%.
4. the method for synthetic, purifying para-totuidine-3-sulfonic acid (4B acid) according to claim 1 is characterized in that the acid that acid out is used can be all kinds of mineral acids, is preferably sulfuric acid, and the pH value of solution is 1～2 after the acidifying.
5. according to the method for claim 1 or 2,3,4 described synthetic, purifying para-totuidine-3-sulfonic acid (4B acid), the temperature that it is characterized in that alkali neutralization, activated carbon decolorizing and acid out is 10 °～80 ℃, is preferably 60～70 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 95115450 CN1130624A (en) | 1995-09-07 | 1995-09-07 | Synthetic method and purifying technique for high-purity p-toluidine-3-sulfonic acid (4B acid) |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 95115450 CN1130624A (en) | 1995-09-07 | 1995-09-07 | Synthetic method and purifying technique for high-purity p-toluidine-3-sulfonic acid (4B acid) |
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| Publication Number | Publication Date |
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| CN1130624A true CN1130624A (en) | 1996-09-11 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN 95115450 Pending CN1130624A (en) | 1995-09-07 | 1995-09-07 | Synthetic method and purifying technique for high-purity p-toluidine-3-sulfonic acid (4B acid) |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102718687A (en) * | 2012-05-29 | 2012-10-10 | 吴江市屯村颜料厂 | Method for preparing 4B acid |
| CN102718688A (en) * | 2012-05-29 | 2012-10-10 | 吴江市屯村颜料厂 | Method for preparing 2B 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 |
-
1995
- 1995-09-07 CN CN 95115450 patent/CN1130624A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102718687A (en) * | 2012-05-29 | 2012-10-10 | 吴江市屯村颜料厂 | Method for preparing 4B acid |
| CN102718688A (en) * | 2012-05-29 | 2012-10-10 | 吴江市屯村颜料厂 | Method for preparing 2B 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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