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A kind of purification method of ethylenic organic compound

A technology of organic compounds and purification methods, applied in the field of purification of organic compounds, can solve the problems of limited purification methods, few research reports, and high cost in the later stage, and achieve ideal impurity removal effects, mild process conditions, and easy operation

Active Publication Date: 2022-05-10
江苏广域化学有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This solution leads to many restrictions and high costs in the overall process
Moreover, the applicable post-purification method is extremely limited, and there are few relevant research reports before the present invention

Method used

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  • A kind of purification method of ethylenic organic compound
  • A kind of purification method of ethylenic organic compound
  • A kind of purification method of ethylenic organic compound

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0049] At room temperature, 20 g of compound 2A (which contains about 1.5%, ie about 0.00075 mol of impurity compound 2B) was dissolved in 80 g of toluene; then 0.1 g (about 0.0009 mol) of triethylenediamine was added and stirred evenly. Then take out 10g from the 100g solution prepared above and put it into a special tubular microwave reaction container with a volume of 20ml, then put it into the microwave reactor, turn on the 100w microwave to carry out the catalytic reaction and time it; when the liquid temperature is close to 60°C , turn off the microwave immediately. Take out the reaction vessel, place it in a water bath at room temperature to cool down, until the liquid temperature in the tube drops to close to room temperature. Use 100w microwave again for catalytic reaction and timing. When the liquid temperature is close to 60°C, turn off the microwave again and take out the reaction vessel to cool down. This is repeated until the cumulative time for the catalytic re...

Embodiment 2

[0064] At room temperature, 100 g of compound 2A (which contains about 32 ppm, that is, about 8.2×10 -6 The impurity compound 2B of mol, the impurity compound 2D of 6ppm), be dissolved in the toluene of 400g; Then add 0.09g (approximately 8.2x10 -4 mol) of triethylenediamine, and stir evenly. Then take out 10g from the above prepared 500g solution, put it into a tubular microwave special reaction vessel with a volume of 20ml, then put it into the microwave reactor, turn on the 100w microwave to carry out the catalytic reaction and time it. When the liquid temperature is close to 60°C, turn off the microwave immediately. The reaction vessel was taken out and placed in a water bath at room temperature to cool down until the liquid temperature in the tube dropped to close to room temperature. Use 100w microwave again for catalytic reaction and timing, when the liquid temperature is close to 60°C, turn off the microwave again, take out the reaction vessel to cool down. This is ...

Embodiment 3

[0072] At room temperature, 100g of compound 3A (which contains about 61ppm, that is, about 1.6x10 -5 mol of impurity compound 3B), first dissolved in 1000g of n-heptane; then add 0.018g (about 1.6x10 -4mol) of triethylenediamine, and stir well. Pre-cool the above solution to 10-15°C, then use a peristaltic pump to transport it through a threaded glass coil, and then flow into the receiving bottle; the main body of the threaded glass coil is located in the microwave reactor, and is continuously irradiated by 300w microwave irradiated. Control the flow rate of the peristaltic pump so that the time for the solution to pass through the threaded glass coil is about 6 seconds; it can be measured that the temperature of the solution after passing through the coil rises to 15-20°C. At room temperature, pass the solution flowing out of the coil through a silica gel column filled with 20g of 60-100 mesh silica gel with a diameter-to-height ratio of less than 1:4 for adsorption and se...

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Abstract

The invention discloses a method for purifying an alkene organic compound. The alkene organic compound to be purified contains any one or more of chlorinated, brominated, and iodo derivative impurities. The method adopts triethylenedi The amine and the ethylenic organic compound to be purified are mixed with an organic solvent, and catalyzed by microwaves, so that triethylenediamine reacts with chlorinated, brominated, and iodo derivative impurities to generate the corresponding organic amine salt, so as to facilitate the removal of the Derivative impurities. The present invention has mild reaction conditions, short reaction time, is suitable for industrialization, and fully reduces the ratio of the product of the salt-forming reaction (organic amine salt) to be continuously converted into the elimination of side reaction products, and has obvious impurity removal effect. When the total content of chlorinated and iodo impurities is very low, there are still obvious effects. The removal rate of a single treatment can reach more than 90%. After repeated treatments, the content of chloro, bromo and iodo impurities can be stably reduced. Even below 1ppm, it cannot even be detected.

Description

technical field [0001] The invention belongs to the technical field of purification of organic compounds, and relates to a method for purification of vinyl organic compounds. Background technique [0002] Alkenic organic compounds containing carbon-carbon double bonds are widely used in liquid crystal materials and organic electroluminescent materials. For liquid crystal materials and organic electroluminescent materials, if there are chlorinated, brominated, and iodized impurities above the ppm level, the chemical activity, insulation, light stability, thermal stability, etc. of the material will be affected. have obvious adverse effects. However, in the production and post-treatment process of olefinic organic compounds, impurities containing chloro, bromo, and iodo groups will inevitably be generated and remain. Therefore, appropriate purification methods must be adopted to remove such impurities to a level less than 1ppm, or even undetectable; and in the purification p...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C7/148C07C17/395C07C17/38C07C7/00C07C25/24C07C13/28C07B63/02
CPCC07C17/395C07C17/38C07C7/005C07C7/14875C07B63/02C07C2601/14C07C25/24C07C13/28
Inventor 蔡一超张招胜宋启发
Owner 江苏广域化学有限公司
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