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Novel phenol-free technology for producing basic violet 5BN

An alkaline and high-tech technology, which is applied in the field of new phenol-free production of Basic Violet 5BN, can solve the problems of not being suitable for large-scale industrial production, corrosion of phenol mucosa, and material clumping, so as to solve the problem of material clumping in the process of alkalization and heating up , Increase the concentration of active oxygen and improve production efficiency

Inactive Publication Date: 2019-12-10
丰城三友制笔科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the use of phenol also brings some problems that need to be solved urgently: 1. The smell of phenol is relatively large, which seriously affects the production environment during the feeding and discharging process, and also makes the product have an unpleasant and difficult to remove smell; 2. Phenol is harmful to skin, The mucous membrane has a strong corrosion effect, which brings safety hazards to the production operation; 3. The production waste liquid contains a large amount of phenols, which causes the waste water COD to seriously exceed the standard, and brings great difficulties to the sewage treatment. Once it enters the natural environment, it will harm the water body. Serious natural hazards to the environment and atmospheric environment
In the patent US 2,816,900, emulsifiers such as Aerosol C-6l, dodecyltrimethylammonium chloride, etc. are used to replace phenol to produce basic violet, but the oxidized material obtained by oxidative condensation is dense and hard when cold, and the alkali is It is difficult to get into the blocky oxide material, because the unalkaliized material is easy to stick when heated, which will cause the material to agglomerate during the alkalization heating process. In the patent, it is removed by hot water extraction and copper conversion into copper sulfide The refining scheme is not suitable for large-scale industrial production, because it is difficult to completely dissolve the oxidized material in hot water due to the adhesion of the oxidized material, and the process consumes a lot of water, and the copper impurities in the oxidized material are combined with the dye through chelation, etc., and the one-step method is very difficult. Difficult to remove copper completely
Patent CN 101381526A uses combined emulsifiers to produce basic violet products, and obtains basic violet products with low copper content. During the reaction process, organic solvents such as ethyl acetate, benzene, toluene, and chlorobenzene are used as compound components, and refined The process also uses organic solvents such as chlorobenzene to treat oxidized materials, and organic solvents such as chlorobenzene have serious health hazards and serious hazards to the environment. They can pollute water bodies, soil and the atmosphere, and are flammable and irritating. The residue of solvent will make the product have an unpleasant smell, and the recovery of solvent will bring more complicated additional process to the production
[0005] In addition, the traditional basic violet 5BN oxidative condensation time is too long, the patent CN 101381526A uses air as an oxidant to produce basic violet products under phenol-free conditions, and the oxidative condensation reaction time is as long as 40-45h
Long oxidation time will lead to long production cycle, high production energy consumption and labor cost, which seriously restricts production efficiency

Method used

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  • Novel phenol-free technology for producing basic violet 5BN
  • Novel phenol-free technology for producing basic violet 5BN
  • Novel phenol-free technology for producing basic violet 5BN

Examples

Experimental program
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Effect test

Embodiment 1

[0036] First add water, NaCl, copper sulfate pentahydrate to the oxidation pot, start the equipment and add N,N-dimethylaniline after stirring evenly, add combined emulsifier (OP-9 and dodecyltrimethylammonium chloride combined and into), stir for 2 hours until the material is in the form of a uniform emulsion, heat up to 70°C, blow in air and start to add sodium chlorate solution dropwise, the dropwise addition is completed within 4 hours, and the reaction is stopped until the color of the material is golden yellow and the pre-cooling becomes brittle. The total reaction time was close to 23h.

[0037] After the reaction is over, the oxidizing material is cooled to room temperature and put into a high-shear wet crushing kettle with liquid caustic soda (mass concentration: 30%), crushed for 4 hours until the particles are crushed without visible gold, and the powder is fine within 4 hours. The temperature is raised to 95°C (the first hour is raised to 60°C, the second hour is r...

Embodiment 2

[0041] First add water, NaCl, copper sulfate pentahydrate to the oxidation pot, start the equipment and stir evenly, add N,N-dimethylaniline, add combined emulsifier (OP-10 and cetyltrimethylammonium chloride combined and into), stir for 2 hours until the material is in the form of a uniform emulsion, heat up to 70°C, blow in air and start to add sodium chlorate solution dropwise, the dropwise addition is completed within 4 hours, and the reaction is stopped until the color of the material is golden yellow and the pre-cooling becomes brittle. The total reaction time is close to 20h.

[0042] After the reaction is over, the oxidizing material is cooled to room temperature and put into a high-shear wet crushing kettle with liquid caustic soda (mass concentration: 30%), crushed for 4 hours until the particles are crushed without visible gold, and the powder is fine within 4 hours. The temperature is raised to 95°C (the first hour is raised to 60°C, the second hour is raised to 70...

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Abstract

The invention relates to novel phenol-free technology for producing basic violet 5BN, which comprises the following steps: replacing phenol with a combined emulsifier consisting of a nonionic emulsifier and a cationic emulsifier for heterogeneous reaction of oxidative condensation; the oxidative condensation reaction time is shortened through joint oxidation of air and a chemical oxidant; adoptinghigh-shear wet crushing technology for treating an obtained oxidized material to increase the contact area of the oxidized material and alkali; removing copper ions through converting of copper ionsinto copper sulphide which is removed.

Description

technical field [0001] The present invention relates to the technical field of production of Basic Violet 5BN, in particular to a set of basic violet 5BN phenol-free environmental protection production process, specifically refers to a method of using combined emulsifier instead of phenol, using air and chemical oxidant to co-oxidize, using high shear The process flow of the wet pulverizer to pulverize the oxide material and then refine it to obtain the basic violet 5BN product with high purity and low copper content. Background technique [0002] Basic Violet 5BN (CAS: 548629) is a cationic triarylmethane dye. It is one of the main production varieties of basic dyes. It has strong dyeing ability, pure and bright shade, and moderate price. It has a wide range of applications and can be used in Dyeing of paper, leather, animal and plant fibers, etc., can also be used to manufacture color lakes, inks, and purple potion (gentian violet) commonly used in medicine. [0003] The ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09B11/18
CPCC09B11/18
Inventor 胡永辉
Owner 丰城三友制笔科技有限公司
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