Purified 1-hydroxy-4-arylaminoanthraquinone product and preparation method thereof
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An arylaminoanthracene and dihydroxyanthraquinone technology is applied in the field of purified 1-hydroxy-4-arylaminoanthraquinone products and their preparation, and can solve the problems of high price, uneconomical single condensed dyes and the like
Active Publication Date: 2017-03-29
宁波龙欣精细化工有限公司
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Problems solved by technology
The purity of the product synthesized by this process should be relatively high, but the price of NMP is relatively high, and it is not economical
Method used
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Embodiment 1
[0027] In a 1.0L autoclave equipped with special stirring, add 520ml of water, 3.2 grams of sodium dodecylbenzenesulfonate, 44 grams of aniline, 80 grams of quinizarin, 28 grams of quinizarin leuco, and the mixture is heated under air isolation to 110°C, keep it for 15 hours, cool down to 60°C, discharge and filter, wash the filter cake with 80°C hot water, and dry at 100°C to obtain 133.3 grams of purple powdery product. The above product was added to 355 grams of 60% DMF-containing aqueous solution, heated and refluxed for 2 hours under stirring, then cooled to room temperature, filtered, washed with hot water, and dried at 105° C. to obtain 126.4 grams of reddish-purple crystalline powder. analyzed by liquid chromatography (see figure 1 ), the main product is 1-hydroxy-4-anilinoanthraquinone content of 97.8%, impurity 1,4-dianilino anthraquinone content of 1.3%, 1,4-dihydroxy anthraquinone content of 0.13%, and other unknown impurities. 0.37% max.
Embodiment 2
[0029] The procedure described in Example 1 was repeated, but using 3.8 g of sodium cetyl sulphate, to give the same product.
Embodiment 3
[0031]In a 1.0L autoclave equipped with special stirring, add 600ml of water, 2.6g of diffusing agent N and 49.8g of p-toluidine, 80g of quinizarin, 28g of quinizarin leuco, and the mixture is heated to 110°C under the isolation of air , kept for 18 hours, cooled to 60°C, filtered the discharge, washed the filter cake with hot water, and dried at 100°C to obtain 140.6 grams of dark purple powdery product. The above product was added to 350 grams of an aqueous solution containing 80% DMF, heated and refluxed for 2 hours under stirring, then cooled to room temperature, filtered, washed with hot water, and dried at 105°C to obtain 128.6 grams of blue-purple crystalline powder, which was analyzed by liquid chromatography (see figure 2 ), the main product is 1-hydroxy-4-p-toluidino anthraquinone with a content of 98.2%, the impurity 1,4-di-p-toluidino anthraquinone with a content of 1.20%, 1,4-dihydroxy anthraquinone with a content of 0.17%, and others unknown The sum of impuriti...
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Abstract
The invention relates to a novel method for preparing 1-hydroxy-4-arylamino-anthraquinone. The method comprises the following steps: performing condensation reaction on a mixture of quinizarin and leucoquinizarin and a slight excess of aromatic amine in water containing an anionic surfactant, wherein boric acid or other condensation agents are not used in the reaction; and performing refining treatment on a condensation product with a DMF water solution to obtain 1-hydroxy-4-arylamino-anthraquinone with the purity being above 97.0%, wherein the content of a secondary condensation product in the product is lower than 2.0% and the residual amount of 1, 4-dihydroxyanthraquinone is lower than 1.0%. According to the novel method provided by the invention, by strictly controlling condensation reaction conditions, such as selecting the slight excess of aromatic amine and the anionic surfactant, the condensation reaction stays in the primary condensation state, the secondary condensation reaction is effectively controlled, the generation of double condensation products is reduced, the product purity is improved and the refining difficulty in the late stage is further reduced. Aromatic amine is strictly controlled to be slightly excessive, i.e., the amount meets the reaction requirements and does not need to be recovered; and by using the anionic surfactant, the condensation reaction is effectively promoted and the cost and reaction difficulty are reduced.
Description
technical field [0001] The invention relates to the technical field of chemical products, in particular to a purified 1-hydroxy-4-arylaminoanthraquinone product and a preparation method thereof. Background technique [0002] Generally speaking, the condensation reaction activity of quinizarin and its leucosomes with arylamines with little hindrance is relatively high, and the reaction is controlled in the single condensation stage to produce 1-hydroxyl-4-arylamine with higher purity (97.0% or more). Anthraquinone has certain difficulties and requires a strict formula combination and operating conditions. The color light of the single condensation product is usually purple or blue, and the color light of the double condensation product is usually blue to green. If the double condensation product content in the single condensation product is high, it will inevitably lead to dark shade when it is colored; in addition, in the product, the 1,4-dihydroxyanthraquinone content is hi...
Claims
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