After-treatment purification method of vinylcarbazole

A technology for vinylcarbazole and vinylcarbazole crude products, which is applied in the field of post-processing and purification of vinylcarbazole, can solve the problems of generally low yield, unsuitable extraction methods, and low product purity, and achieves purification accuracy. High, low cost, easy to operate effect

Inactive Publication Date: 2015-02-18
HUBEI HECHANG NEW MATERIAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At the same time, vinyl carbazole has a solubilizing effect on carbazole, and the extraction method is not applicable
Therefore, the general yield of the above methods is not high, and the product purity is not high.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Mix 17g of carbazole, 100ml of toluene, and 6g of potassium hydroxide in a 500ml high-pressure reactor, and pass in about 6.5g of vinyl chloride gas at 100°C and 0.2Mpa, and keep it warm for 6 hours. After the reaction, distill out the toluene under reduced pressure , add about 100g of water, the crude product of vinyl carbazole is precipitated, and the gas phase detection content is 92.4%.

[0019] The mixed solvent of sherwood oil (II type) and absolute ethanol with a mass ratio of 1: 10 for this crude product is the mobile phase, and the triethylamine containing 0.1wt% is contained in the mobile phase, and the diameter-to-height ratio is 2cm: two chromatographic columns of 20cm respectively Silica gel and activated carbon are used as stationary phases, used in series, and subjected to normal-pressure column chromatography to collect vinyl carbazole products. The content detected by gas chromatography is 99.2%.

Embodiment 2

[0021] Mix 17g of carbazole, 100ml of toluene, and 6g of potassium hydroxide in a 500ml high-pressure reactor, and pass in about 6.5g of vinyl chloride gas at 100°C and 0.2Mpa, and keep it warm for 6 hours. After the reaction, distill out the toluene under reduced pressure , add about 100g of water, the crude product of vinyl carbazole is precipitated, and the gas phase detection content is 92.4%.

[0022] The mixed solvent of sherwood oil (II type) and absolute ethanol with a mass ratio of 1: 10 for this crude product is the mobile phase, containing 0.3wt% triethylamine in the mobile phase, and the diameter-to-height ratio is 2cm: two chromatographic columns of 18cm respectively Silica gel and activated carbon are used as stationary phases, used in series, and subjected to normal-pressure column chromatography to collect vinyl carbazole products. The content detected by gas chromatography is 99.4%.

Embodiment 3

[0024] Mix 34g carbazole with 200g 50% sodium hydroxide solution, add 0.1g benzyltriethylammonium bromide, add 16.5g chloroethanol dropwise under vigorous stirring, continue stirring for 5 hours after the dropwise addition, filter out the solid, solid Drop into the mixture of 300g dehydrated ethanol and 30g potassium hydroxide for reflux reaction for 4 hours, add 400g water after the reaction is finished, and precipitate a solid, which is detected by gas chromatography after drying, and the vinyl carbazole content is 86.2%.

[0025] The petroleum ether (II class) and ethyl acetate mixed solvent of mass ratio 1:8 are used as the mobile phase for this crude product, and the triethylamine containing 0.2wt% is contained in the mobile phase, and the diameter-to-height ratio is 2cm: two chromatographic columns of 24cm respectively Silica gel and alumina are used as stationary phases, used in series, and subjected to atmospheric pressure column chromatography to collect vinyl carbazol...

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PUM

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Abstract

The invention provides an after-treatment purification method of vinylcarbazole. The method is high in purification precision and convenient to operate. Column chromatographic separation is performed on a vinylcarbazole crude product containing 5-50 wt% of raw carbazole material with two or more chromatographic columns, and a vinylcarbazole product is collected; an adopted mobile phase comprises two of petroleum ether, cyclohexane, benzene, diethyl ether, chloroform, ethyl acetate, n-butyl alcohol, acetone, ethyl alcohol and methyl alcohol and further comprises triethylamine; a stationary phase of each chromatographic column comprises one or more of silica gel, aluminium oxide, activated carbon, magnesium silicate and polyamide. According to the after-treatment purification method of the vinylcarbazole, the difference in polarities of various organic solvents is used, and the purification purpose is achieved with a column chromatography method with the multiple columns connected in series; the method is high in purification precision, convenient to operate and low in cost.

Description

technical field [0001] The invention relates to a purification method, in particular to a post-treatment purification method of vinyl carbazole. Background technique [0002] Vinyl carbazole is mainly used to synthesize polyvinyl carbazole (PVK). Polyvinyl carbazole (PVK) is a class of classical and important hole-based polymers. It has attracted people's attention and has been widely used in high-tech fields such as xerographic copying, laser printing, solar cells and light-emitting diodes. The electrophotographic photosensitive plate coated with it has a good copy effect on blue-purple drawings and images with more tonal levels; the thermoplastic holographic picture coated with it can be developed in situ and reused without darkroom operation; The light free radical polymerization photosensitive material prepared by it has the sensitivity of the silver salt material and can be used for fast photography. PVK can also be used as a high temperature resistant electrical insu...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D209/86C07D209/84
CPCC07D209/86C07D209/84
Inventor 丁博杨和平叶楚平
Owner HUBEI HECHANG NEW MATERIAL TECH
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