Environment-friendly production method for permanent violet RL

A production method, permanent violet technology, applied in the field of synthetic technology of permanent violet RL, can solve the problems of low conversion rate, harsh transportation and storage management conditions, high cost of use, etc., to achieve convenient temperature control, high product quality and The effect of economic benefits

Inactive Publication Date: 2012-11-21
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

[0009] Although there are also attempts to use the hydrogenation reduction process. Theoretically, the conversion rate of this process can reach 100%, and the sewage is zero discharge. However, hydrogenation is a high-risk process with relatively high risks. There are high equipment costs, strict site requirements, and operational The quality requirements of personnel are high, the transportation and storage management conditions are harsh, the cost of use is high, and a little carelessness can lead to safety accidents, etc., which are rare in actual production
[0010] In short, the existing permanent violet RL production method has serious environmental pollution, high unit consumption of raw material carbazole (2.0t / t product), low conversion rate, and long reaction time (requiring a total of more than 100 hours). The synthesis method of permanent violet RL with pollution, low product consumption, high conversion rate and short total reaction time is becoming more and more important

Method used

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  • Environment-friendly production method for permanent violet RL
  • Environment-friendly production method for permanent violet RL
  • Environment-friendly production method for permanent violet RL

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] 1. Alkylation

[0034] 1. Put 500kg of recovered liquid caustic soda into the enamel alkylation reaction kettle, with an alkalinity of 31~33% (mass percentage concentration), and then use 96~99% solid sodium hydroxide (industrial grade) to adjust the alkalinity to reach 40~42%;

[0035] 2. Adjust the temperature to 28~32°C while stirring, and then put in 200kg of carbazole and 3.2kg of catalyst benzyltriethylammonium chloride;

[0036] 3. After adding carbazole and catalyst, cover the lid of the kettle, and add 110kg of pure benzene (from the high level tank of pure benzene) under stirring;

[0037] 4. Then add bromoethane 133.5kg (from bromoethane high level tank) in 20~30 minutes, and control the temperature here at 30~35℃;

[0038] 5. After adding, heat up to 88~90°C in 70~90 minutes, and keep the temperature at 88~90°C for 4.5~5 hours;

[0039] 6. After the heat preservation reaction is completed, heat up to 126~130°C, and recover pure benzene by distillation; af...

Embodiment 2

[0087] 1. Alkylation

[0088] 1. Put 500kg of recovered liquid caustic soda into the enamel alkylation reaction kettle, with an alkalinity of 31-33% (mass percentage concentration), and then use 96-99% solid sodium hydroxide (industrial grade) to adjust the alkalinity to 40 ~42%;

[0089] 2. Adjust the temperature to 28~32°C while stirring, and then put in 200kg of carbazole and 3.2kg of catalyst benzyltriethylammonium chloride;

[0090] 3. After adding carbazole and catalyst, cover the lid of the kettle, and add 110kg of pure benzene (from the high level tank of pure benzene) under stirring;

[0091] 4. Then add bromoethane 140kg (from bromoethane high level tank) in 20~30 minutes, and control the temperature here at 30~35℃;

[0092] 5. After adding, heat up to 85~87°C in 70~90 minutes, and keep the temperature at 85~87°C for 4.5~5 hours;

[0093] 6. After the heat preservation reaction is completed, heat up to 126~130°C, and recover pure benzene by distillation; after the...

Embodiment 3

[0142] 1. Alkylation

[0143] 1. Put 500kg of recovered liquid caustic soda into the enamel reaction kettle, with an alkalinity of 31~33% (mass percentage concentration), and then use solid potassium hydroxide (industrial grade) with a content of 96~99% to adjust the alkalinity to 46~48% ;

[0144] 2. Adjust the temperature to 28~32°C while stirring, and then put in 200kg of carbazole and 3.2kg of catalyst benzyltriethylammonium chloride;

[0145] 3. After adding carbazole and catalyst, cover the lid of the kettle, and add 110kg of pure benzene (from the high level tank of pure benzene) under stirring;

[0146] 4. Then add bromoethane 140kg (from bromoethane high level tank) in 20~30 minutes, and control the temperature here at 30~35℃;

[0147] 5. After adding, heat up to 85~87°C in 70~90 minutes, and keep the temperature at 85~87°C for 4.5~5 hours;

[0148] 6. After the heat preservation reaction is completed, heat up to 126~130°C, and recover pure benzene by distillation;...

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Abstract

The invention discloses an environment-friendly production method for permanent violet RL, which comprises the following: (1) a step of alkylation which is to prepare liquid caustic soda, add a carbazole raw material, a catalyst and pure benzene in turn, drip bromoethane, stand the solution and separate out N-ethyl carbazole; (2) a step of nitration, which is to add the N-ethyl carbazole and chlorobenzene, drip nitric acid of which the weight percentage concentration is 36.5 to 37.5 percent, and separate out an intermediate 3-nitro-N-ethyl carbazole; (3) a step of reduction, which is to add chlorobenzene, 3-nitro-N-ethyl carbazole and an iron catalyst in turn, drip hydrazine hydrate to obtain a solution of 3-animo-N-ethyl carbazole and ortho-dichlorobenzene; (4) a step of condensation, which is to add ortho-dichlorobenzene into the solution of 3-animo-N-ethyl carbazole and ortho-dichlorobenzene, add tetrachlorobenzoquinone, drip sodium acetate and obtain a permanent violet RL condensation compound; and (5) a step of ring-closing reaction, which is to add benzene sulfonyl chloride, filter the solution, wash a filter cake, dry and obtain coarse permanent violet RL. The method has high conversion rate and is environment-friendly.

Description

technical field [0001] The invention relates to a production method of an organic pigment, in particular to a synthesis process of permanent violet RL. Background technique [0002] Permanent Violet RL is a high-grade organic pigment of dioxazine series. It has outstanding coloring strength, brightness and excellent heat resistance, permeation resistance and light fastness. It has excellent performance indicators and is widely used. Used in coatings, plastics, rubber, solvents, plexiglass, textile printing and dyeing, water-based ink and packaging printing, etc., it is currently one of the most expensive pigments in the world, and it is also the best purple pigment used in the plastics industry so far. [0003] Permanent Violet RL is made of N-ethylcarbazole by alkylation of carbazole, then nitrated and reduced to produce 3-amino-N-ethylcarbazole, and then condensed with chloranil in an organic solvent , closed loop, and finally through the process of pigmentation to obtain...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C09B19/00
CPCY02P20/584
Inventor 毕亚铃陈小强张蒙于春发
Owner 东台市新锦泰化工有限公司
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