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Synthetic method for solvent violet 13

A synthesis method and technology of solvent violet, applied in the field of synthesis of solvent violet 13, can solve problems such as endangering the health of operators, low reaction conversion rate, and polluting the working environment, so as to achieve increased yield, save manpower and material resources, and save waste The effect of the process

Active Publication Date: 2016-01-13
JIANGSU DAOBO CHEM
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AI Technical Summary

Problems solved by technology

[0021] The existing synthetic method of solvent violet 13 has the following deficiencies: ① directly use p-toluidine as the starting material, and p-toluidine has extremely high toxicity, its freezing point is 44°C, it needs to be heated and dissolved before use, and it is highly volatile and easy to sublime , will pollute the working environment and endanger the health of operators; ②In the reduction reaction of 1,4-dihydroxyanthraquinone, zinc powder is used as the reducing agent in acidic medium, and the amount of zinc powder is large, and the reaction conversion rate is not high; insurance is used in alkaline medium Powder is used as a reducing agent, the leuco body needs to be post-treated, and the condensation reaction cannot be carried out directly, and the amount of three wastes is large and the pollution is serious

Method used

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  • Synthetic method for solvent violet 13
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  • Synthetic method for solvent violet 13

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preparation example Construction

[0048] A kind of synthetic method of solvent violet 13, concrete steps are as follows,

[0049] First put methanol, 1,4-dihydroxyanthraquinone, p-nitrotoluene, iron powder, and boric acid into a pressure vessel in sequence, seal the vessel and replace it with nitrogen, then stir and raise the temperature to 50-60°C, and then inject hydrogen for hydrogenation Reduction, when the reaction system stops absorbing hydrogen, control the heat preservation reaction at 60-70°C for more than 2 hours, heat up after the reaction, and carry out the condensation reaction at 90-100°C for more than 5 hours. pressure, lower the temperature, pass air to carry out the oxidation reaction, and finally add hydrochloric acid for beating, the beating temperature is 60-70°C, filter, wash, and dry to obtain Solvent Violet 13.

[0050] Wherein, the mass ratio of 1,4-dihydroxyanthraquinone to methanol is 1:(1.1~3.0); the mass ratio of 1,4-dihydroxyanthraquinone to p-nitrotoluene is 1:(0.5~0.7); 1 , The ...

Embodiment 1

[0052] In a 500mL autoclave with mechanical stirring and a thermometer, add 44g of methanol, 40g of 1,4-dihydroxyanthraquinone, 20g of p-nitrotoluene, 1.6g of iron powder, and 5.9g of boric acid, and seal the autoclave for nitrogen replacement. , and then stirred and raised the temperature to 50°C and began to feed hydrogen for hydrogenation reduction, and the temperature was controlled at 50°C. After the reaction system stopped absorbing hydrogen, it was controlled at 70°C for heat preservation reaction to strengthen hydrogen absorption, and the heat preservation reaction time was 2 hours. After the reaction was completed, the temperature was raised to 90° C. for condensation reaction, and the reaction time was 10 h. After the reaction, the temperature was lowered to 60°C, the pressure was released, and the air was introduced to oxidize the intermediate rapidly. Finally, 8g of hydrochloric acid was added for beating. 97%, yield 87%, DC 3.0, DH 2.5, intensity 100.42.

Embodiment 2

[0054]In a 500mL autoclave with mechanical stirring and a thermometer, add 120g of methanol, 40g of 1,4-dihydroxyanthraquinone, 28g of p-nitrotoluene, 4.8g of iron powder, and 12g of boric acid, and seal the autoclave for nitrogen replacement. Then stir and raise the temperature to 55°C and start feeding hydrogen to carry out hydrogenation reduction, and the temperature is controlled at 55°C. After the reaction system stopped absorbing hydrogen, it was controlled at 60°C for heat preservation reaction to strengthen hydrogen absorption, and the heat preservation reaction time was 4 hours. After the reaction was completed, the temperature was raised to 95° C. for condensation reaction, and the reaction time was 8 hours. After the reaction, the temperature was lowered to 60°C, the pressure was released, and the air was introduced to oxidize the intermediate rapidly. Finally, 32g of hydrochloric acid was added for beating. %, the yield was 88.7%, the DC was 2.0, the DH was 1.7, a...

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Abstract

The invention discloses a synthetic method for solvent violet 13, and develops a new route for synthesizing violet 13 by employing a one-pot process. The method comprises successively adding methanol, 1,4-dihydroxyanthraquinone, 4-nitrotoluene, iron powder and boric acid into a pressure container, sealing the container and performing nitrogen displacement, then heating with stirring, introducing hydrogen for hydrogenation reduction, after the reaction system stops absorbing hydrogen, performing warm-keeping reaction, heating after the reaction is finished, performing condensation reaction, cooling after the reaction is finished, releasing the pressure, introducing air and performing oxidation reaction, and finally adding hydrochloric acid for beating, filtering, washing and drying, so as to obtain violet 13. According to the method, the initial raw material p-toluidine is replaced by 4-nitrotoluene, direct usage of the highly-toxic raw material p-toluidine is avoided, and the synthetic technology is low in toxicity and friendly to environment. By pouring all of the raw materials into the container, the postprocessing process of the intermediate step is saved, and a large amount of manpower and material resource is saved.

Description

technical field [0001] The invention relates to a synthesis method of solvent violet 13, which belongs to the technical field of chemical dye synthesis. Background technique [0002] Solvent Violet 13, also known as Fluorescent Violet B, has a chemical name of 1-hydroxy-4-p-tolylaminoanthraquinone, and is a black purple powder. It turns dark green when it encounters concentrated sulfuric acid, and produces olive to reddish blue precipitate after dilution. Solvent Violet 13 is mainly used for the raw pulp coloring of polyester fibers, and can also be used for the preparation of color masterbatches for polyester and the ordinary dyeing and rapid dyeing of polyester and its blended fabrics. [0003] Its molecular formula is C 21 h 15 NO 3 , molecular weight 329.35, structural formula: [0004] [0005] There are currently two commonly accepted synthetic routes / mechanisms for Solvent Violet 13: [0006] Route 1: 1,4-dihydroxyanthraquinone is first reduced to its leuco b...

Claims

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Application Information

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IPC IPC(8): C07C225/36C07C221/00
Inventor 徐松刘学峰郭维成汪港陈路云
Owner JIANGSU DAOBO CHEM
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