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Permanent violet alkylating process

An alkylation and permanent violet technology, applied in organic dyes and other directions, can solve the problems of large manpower, material resources and energy consumption, cumbersome processes, and increased occupational hazard risks, saving manpower, reducing processes, and reducing occupational hazards. Effect

Inactive Publication Date: 2013-08-28
NANTONG LONGXIANG NEW MATERIALS TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This process is relatively cumbersome, and the manpower, material resources and energy consumption are relatively large, and benzene is added in the reaction process, which increases the risk of occupational hazards

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] The permanent violet alkylation process of the present invention comprises the following steps: 600g of liquid caustic soda, 100g of carbazole, 5g of polyethylene glycol, and 75.06g of partial bromoethane are dropped into three ports of a stirring and reflux condenser with a concentration of 30%. In the flask, slowly heat up to 35°C, drop the remaining 35g of ethyl bromide at this temperature, after the dropwise addition, continue to heat up with the reaction, keep the temperature below the boiling point of the system, and when the conversion rate of carbazole reaches 99.5% The above is regarded as the end of the reaction, stand still for 10 minutes, remove the lower layer of liquid alkali and apply mechanically to obtain molten N-ethylcarbazole.

Embodiment 2

[0016] The permanent violet alkylation process of the present invention comprises the following steps: 400g of liquid caustic soda, carbazole 100g, polyethylene glycol 2.18g, benzyltriethylammonium chloride 0.55g, ethanol 0.27g with a concentration of 40% 1. Put 71.80g of bromoethane into a three-necked flask with stirring and reflux condenser, heat slowly to 35°C, add the remaining 38.2g of bromoethane dropwise at this temperature, after the dropwise addition, continue to heat up with the reaction , the control temperature is always lower than the boiling point of the system. When the conversion rate of carbazole reaches more than 99.5%, the reaction is considered to be over, and it is left to stand for 20 minutes.

Embodiment 3

[0018] The permanent violet alkylation process of the present invention comprises the following steps: 300g of liquid caustic soda, 100g of carbazole, 0.83g of polyethylene glycol, 0.83g of benzyltriethylammonium chloride, and 0.34g of ethanol with a concentration of 40% 1. Put 68.53g of ethyl bromide into a three-necked flask with stirring and reflux condenser, heat slowly to 35-40°C, add the remaining 45.47g of ethyl bromide dropwise at this temperature, after the dropwise addition, proceed with the reaction Constantly raise the temperature and control the temperature to be lower than the boiling point of the system. When the conversion rate of carbazole reaches 99.5% or more, the reaction is considered to be over. After standing still for 30 minutes, the lower layer of liquid alkali is separated and applied mechanically to obtain molten N-ethyl carbazole.

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PUM

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Abstract

The invention discloses a permanent violet alkylating process. The permanent violet alkylating process is characterized by comprising the following steps of: feeding caustic soda liquid, carbazole, a catalyst and some bromoethane into a three-port flask with a stirring and reflux condenser; slowly heating until the temperature reaches 35 to 40 DEG C; dropping the rest bromoethane under such temperature; continuously heating along with the reaction after dropping; controlling the temperature to be below the boiling point of a system all the time; determining that the reaction is done after the conversion rate of carbazole is up to more than 99.5%; standing for 10 to 30 minutes; separating the lower caustic soda liquid for recycling over and over, thus obtaining molten N-ethyl carbazole. The permanent violet alkylating process has the advantages that a plurality of processes are decreased, the reaction time is shortened, the manpower, material resources and energy consumption are saved, the usage of benzene is removed, and nearly no occupational hazard is brought; and the molten alkylate directly enters the following nitrating process, so that the process of dissolving the chlorobenzene is saved.

Description

technical field [0001] The invention relates to the field of chemical industry, in particular to a permanent violet alkylation process. Background technique [0002] Permanent purple light bright, strong coloring power, good migration resistance and dispersion, acid resistance, alkali resistance, solvent resistance, and excellent light resistance, heat resistance, weather resistance, widely used in coatings, plastics, rubber , leather, ink, paint, etc. Chinese patent 200610088488.3 reports a method for producing permanent violet RL, including: alkylation, nitration, reduction, condensation, ring closure and ball milling, wherein the alkylation is carried out by carbazole and ethyl bromide in sodium hydroxide solution and benzene In the process, N-ethylcarbazole is reacted under the action of a catalyst, and the specific process includes: alkylation reaction, distillation and recovery of benzene, alkali separation, neutralization, crystallization, filtration and washing, etc...

Claims

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Application Information

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IPC IPC(8): C09B67/20
Inventor 倪伟
Owner NANTONG LONGXIANG NEW MATERIALS TECH CO LTD
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