CN1229075A - Production method for intermediate 2,5-diaryl-amine-terephthalic acid - Google Patents
Production method for intermediate 2,5-diaryl-amine-terephthalic acid Download PDFInfo
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- CN1229075A CN1229075A CN 98112388 CN98112388A CN1229075A CN 1229075 A CN1229075 A CN 1229075A CN 98112388 CN98112388 CN 98112388 CN 98112388 A CN98112388 A CN 98112388A CN 1229075 A CN1229075 A CN 1229075A
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- terephthalic acid
- diaryl
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Abstract
A process for preparing 2,5-diarylamino-terephthalic acid as the intermediate for preparing quinacrilinone series of organic pigments includes such technological steps as condensating dimethyl succinylsuccinate (DMSS),adding oxidant, alkali and water, oxidizing, addition of water, filtering, acidifying, press filtering, water washing and drying to obtain DATA or DTTA. Its advantagesare high purity, stable quality and high output rate of product.
Description
The invention belongs to the allied compound of making organic dye, is to make the production method that quinacridone is shown the intermediate of machine pigment.
2,5-diaryl-amine base-terephthalic acid, promptly DATA and DTTA are to produce the necessary intermediate of high-grade serial pigment dyestuff quinacridone, and its production technology still belongs to blank at home, also has only major company of several family to produce abroad, and its production technology is maintained secrecy.
The present invention discloses a kind of intermediate 2, the production method of 5-diaryl-amine base-terephthalic acid.
Technical solution of the present invention is as follows: be characterised in that raw material be DMSS (DMSS) in organic solvent and have acid in the presence of with the condensation of arylamine class material; Directly add oxygenant then, oxidation under the situation that alkali and water are arranged generates 2, the basic salt of 5-diaryl-amine base-terephthalic acid; Add the water filtration residue, add acid again and carry out acidification, PH is controlled at 3～6, carries out press filtration, washing then, and the crushed after being dried packing promptly gets product 2, and 5-diaryl-amine base-terephthalic acid (DATA) (DTTA).The used above-mentioned organic solvent of the present invention, the alcohols as methyl alcohol, ethanol, propyl alcohol, ethylene glycol etc. so all is fit to, and it is 3～10 times that the consumption of these organic solvents needs with weight with respect to material quantity usually.The acid that exists in the above-mentioned organic solvent can be acetic acid, hydrochloric acid, sulfuric acid, phosphoric acid etc., and its usage quantity seldom, and is common with respect to 1～10% of material quantity.Above-mentioned arylamine class material can be aniline, para-totuidine, p-Nitroaniline etc., and its usage quantity is usually with respect to 0.5～1.5 times of material quantity.Above-mentioned oxygenant is m-nitrobenzene sodium sulfonate, oil of mirbane, p-Nitrophenyl chloride, para-nitrotoluene etc., and its usage quantity is with respect to 0.5～1.5 times of material quantity.Above-mentioned alkali is sodium hydroxide, potassium hydroxide, yellow soda ash, salt of wormwood, and its consumption is with respect to 1～2 times of material quantity, and the consumption of above-mentioned water is with respect to 1～5 times of the alkali consumption.Above-mentioned acid as acidification is hydrochloric acid, sulfuric acid, acetic acid, phosphoric acid etc., and the consumption of acid mainly is to be as the criterion by control solution pH value, and the scope of pH value is generally 3～6.
Technology of the present invention is reasonable.Product purity height, steady quality, the yield height.Provide indispensable intermediate as raw materials for production for producing serial pigment dyestuff quinacridone.
Fig. 1 is a process flow sheet of the present invention.
Following illustrative example, " part " in the example are by weight.Embodiment 1:2, the preparation of 5-hexichol amido-terephthalic acid (DATA): in reactor, add 120 parts of alcohol solvents, 23 parts of aniline, 1 part of hydrochloric acid, and 25 parts of DMSS (DMSS), start stirring, heat up, refluxed 3～6 hours, cooling, add 24 parts of m-nitrobenzene sodium sulfonates again, 20 parts of sodium hydroxide, 20 parts of water heat up, and reflux 4～8 hours, add 200 parts in water, filter, filtrate is used hcl acidifying, pH value 4～6, press filtration then, washing, oven dry is pulverized, sieve 36.8 parts of product DATA (in DMSS, yield 96.44%).
Embodiment 2:2, the preparation of 5-dimethylbenzene amido-terephthalic acid (DTTA): in reactor, add 100 parts of alcohol solvents, 20 parts of para-totuidine, 0.8 part of acid, and 20 parts of DMSS (DMSS), start stirring, heat up, refluxed 3～6 hours, cooling adds 23 parts of m-nitrobenzene sodium sulfonates, 20 parts of potassium hydroxide and 20 parts of water again, heat up again, refluxed 5～8 hours, and added 200 parts in water, filter.Filtrate adds hcl acidifying, press filtration, and washing, oven dry is pulverized, and gets 31.7 parts of product DTTA (in DMSS, yield 96.11%).
Claims (1)
1. intermediate 2, and the production method of 5-diaryl-amine base-terephthalic acid is characterized in that: raw material be DMSS (DMSS) in organic solvent and have acid in the presence of, with the condensation of arylamine class material; Directly add oxygenant then, oxidation under the situation that alkali and water are arranged generates 2, the basic salt of 5-diaryl-amine base-terephthalic acid; Add the water filtration residue, add acid again and carry out acidification, PH is controlled at 3～6, carries out press filtration, washing then, and the crushed after being dried packing promptly gets product 2, and 5-diaryl-amine base-terephthalic acid (DATA) (DTTA).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 98112388 CN1229075A (en) | 1998-03-12 | 1998-03-12 | Production method for intermediate 2,5-diaryl-amine-terephthalic acid |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 98112388 CN1229075A (en) | 1998-03-12 | 1998-03-12 | Production method for intermediate 2,5-diaryl-amine-terephthalic acid |
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| Publication Number | Publication Date |
|---|---|
| CN1229075A true CN1229075A (en) | 1999-09-22 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 98112388 Pending CN1229075A (en) | 1998-03-12 | 1998-03-12 | Production method for intermediate 2,5-diaryl-amine-terephthalic acid |
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| CN (1) | CN1229075A (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101823978A (en) * | 2010-05-17 | 2010-09-08 | 淮安苏瑞精细化工有限公司 | Method for preparing 2, 5-diphenyl amino acid DATA |
| CN101830820A (en) * | 2010-05-17 | 2010-09-15 | 淮安苏瑞精细化工有限公司 | Method for preparing 2,5-diparamethylaniline terephthalic acid (DTTA) |
| CN101844996A (en) * | 2010-05-17 | 2010-09-29 | 淮安苏瑞精细化工有限公司 | Method for preparing 2,5-di(p-chloroanilino)-terephthalic acid (DpCTA) |
| CN105693536A (en) * | 2016-03-08 | 2016-06-22 | 温州永宏科技孵化有限公司 | Preparation method for synthesizing quinacridone pigment intermediate DXTA |
| CN114751837A (en) * | 2022-03-22 | 2022-07-15 | 唐继勇 | Preparation method of intermediate 2, 5-diarylamine-terephthalic acid |
-
1998
- 1998-03-12 CN CN 98112388 patent/CN1229075A/en active Pending
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101823978A (en) * | 2010-05-17 | 2010-09-08 | 淮安苏瑞精细化工有限公司 | Method for preparing 2, 5-diphenyl amino acid DATA |
| CN101830820A (en) * | 2010-05-17 | 2010-09-15 | 淮安苏瑞精细化工有限公司 | Method for preparing 2,5-diparamethylaniline terephthalic acid (DTTA) |
| CN101844996A (en) * | 2010-05-17 | 2010-09-29 | 淮安苏瑞精细化工有限公司 | Method for preparing 2,5-di(p-chloroanilino)-terephthalic acid (DpCTA) |
| CN101844996B (en) * | 2010-05-17 | 2013-06-05 | 淮安苏瑞精细化工有限公司 | Method for preparing 2,5-di(p-chloroanilino)-terephthalic acid (DpCTA) |
| CN101823978B (en) * | 2010-05-17 | 2013-08-21 | 淮安苏瑞精细化工有限公司 | Method for preparing 2, 5-diphenyl amino acid DATA |
| CN101830820B (en) * | 2010-05-17 | 2013-12-18 | 淮安苏瑞精细化工有限公司 | Method for preparing 2,5-diparamethylaniline terephthalic acid (DTTA) |
| CN105693536A (en) * | 2016-03-08 | 2016-06-22 | 温州永宏科技孵化有限公司 | Preparation method for synthesizing quinacridone pigment intermediate DXTA |
| CN114751837A (en) * | 2022-03-22 | 2022-07-15 | 唐继勇 | Preparation method of intermediate 2, 5-diarylamine-terephthalic acid |
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