Permanent violet RL intermediate condensation product synthesis process

A synthesis process, a technology for permanent violet, applied in the field of synthetic technology of permanent violet RL intermediate condensate, can solve the problems of difficult washing of side reactants, affecting product quality, multiple raw materials, etc., to reduce impurity content, process stability, The effect of improving product quality

Inactive Publication Date: 2017-06-13
东台市新锦泰化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the common condensation process for preparing permanent violet RL intermediate condensate is to use non-polar ortho-dichlorobenzene as a solvent, and tetrachlorobenzoquinone and 3-amino-N-ethylcarbazole react under alkaline conditions; The condensate conversion rate of this process is about 90%. The unreacted 3-amino-N-ethylcarbazole, chlorobenzoquinone, and the salts generated by the reaction are directly brought into the next closed-loop reaction, which makes the closed-loop process consume less There are many raw materials, and the side reactants generated by the side reactions that lead to ring closure are difficult to wash, requiring a large amount of solvents, detergents, and water, which also greatly affects the quality of the product

Method used

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  • Permanent violet RL intermediate condensation product synthesis process

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Experimental program
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Effect test

Embodiment 1

[0023] The synthesis process of permanent violet RL intermediate condensate includes the following steps:

[0024] S1. Alkylation reaction: Add lye and chlorobenzene with a mass concentration of 43% in the reaction kettle, and after stirring for 10 minutes, add carbazole and benzyltriethylammonium bromide; divide bromoethane into 3 equal parts , adjust the temperature in the reactor to 20~25℃ under constant stirring, slowly add the first bromoethane dropwise, after stirring for 15min, slowly add the second bromoethane, stir for 15min, then adjust the temperature to 30~ Slowly add the third portion of bromoethane at 36°C, stir, cover and seal for 20 minutes, then adjust the temperature to 60~68°C, and react for 2~3 hours; - Ethylcarbazole;

[0025] S2. Nitration reaction: Add chlorobenzene and N-ethylcarbazole into the reaction kettle, and slowly add nitric acid with a mass concentration of 35%~36.5% under constant stirring, and the dropping time is 2~3.5h. After completion, ...

Embodiment ２

[0040]The process steps of this embodiment and embodiment 1 are the same, the difference is (2) in step S4 condensation reaction: adjust the temperature to 40 ~ 45 ° C, then open the lid of the kettle, put in 64 kg of sodium carbonate (industrial grade) with a content of 98%, The feeding time is controlled within 10-25 minutes. Among them, the weight ratio of materials 3-amino-N-ethylcarbazole: ethanol: chloranil: sodium carbonate = 1: (18~22): (0.58~0.60): (0.32~0.34).

Embodiment ３

[0042] The process steps of this embodiment are the same as that of Embodiment 1, the difference lies in the difference of step S1:

[0043] S1. Alkylation reaction: Add lye and dichlorobenzene with a mass concentration of 45% in the reaction kettle, and after stirring for 10 minutes, add carbazole and benzyltriethylammonium chloride; divide bromoethane into equal amounts of 3 part, under constant stirring, adjust the temperature in the reactor to 20~25°C, slowly add the first part of bromoethane dropwise, after stirring for 15 minutes, slowly add the second part of bromoethane, stir for 15 minutes, then adjust the temperature to 30 ~36°C, slowly add the third portion of bromoethane, stir, cover and seal for 20 minutes, then adjust the temperature to 60~68°C, and react for 2~3 hours; after the reaction, dichlorobenzene is recovered by distillation, and sodium bromide is separated by standing and N-ethylcarbazole.

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Abstract

The present invention discloses a permanent violet RL intermediate condensation product synthesis process, which comprises: alkylating carbazole to prepare N-ethyl carbazole, and carrying out nitrification and reduction to produce 3-amino-N-ethyl carbazole, and carrying out a condensation reaction in an organic solvent to obtain the permanent violet RL intermediate condensate. According t the present invention, the condensation reaction uses the alcohol solvent to replace the conventional o-dichlorobenzene, such that the conversion rate of 3-amino-N-ethyl carbazole is increased, the purity and the yield of the permanent violet RL crude product are improved, the process is stable, the operation is simple, and the safety coefficient is high.

Description

technical field [0001] The invention relates to the technical field of production of permanent violet, in particular to a synthesis process of permanent violet RL intermediate condensate. Background technique [0002] Permanent Violet RL is a high-grade organic pigment of the dioxazine class. It has outstanding coloring strength, brightness and excellent heat resistance, permeation resistance and light fastness. Its performance indicators are very good. Its use The range is very wide, and it is a popular variety in the fields of various coatings, plastics, plexiglass, rubber, textile printing, solvent volume, water-based ink and packaging printing, and is also suitable for offset printing, gravure printing, and flexographic printing. In the 20th century, my country relied on imports for the use of permanent violet RL for a long time. With the continuous improvement of technology, the permanent violet RL developed by my country in the early 1990s has improved product quality ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D209/88
CPCC07D209/88
Inventor 张蒙
Owner 东台市新锦泰化工有限公司
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