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Purification method of biphenyl

A purification method and biphenyl technology are applied in the field of extracting high-purity biphenyl, which can solve the problems such as not being seen, and achieve the effects of convenient operation, low energy consumption, and reduction in the use of equipment.

Active Publication Date: 2007-10-03
BAOWU CHARCOAL MATERIAL TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Also do not see the report that obtains the biphenyl that purity reaches more than 99% from the intermediate product of coal tar processing

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] The vacuum rectification device adopts stainless steel bulk packing, and the number of trays is 40. Weigh 983gWO-R and add it to the still, adjust the vacuum pressure to 0.075MPa, start heating to reflux, and start to extract after the reflux is stable for 1-2hrs Fraction, the reflux ratio is 10, when the distilling temperature reaches 209°C, start to collect biphenyl fractions, stop extraction when the temperature reaches 213°C, and obtain 272.0g crude biphenyl crystals, after analysis, the biphenyl content in crude biphenyl It is 71.36wt%.

[0024] Weigh 41.3g of crude biphenyl crystallization fraction and 66.08g of absolute ethanol, put them into a stirring crystallizer with an anchor stirrer, heat to 55°C, and cool to crystallization at a cooling rate of 10K / h under stirring at a speed of 100rpm At a final temperature of 5°C, filter out the biphenyl crystals, add the filtered out biphenyl crystals and absolute ethanol into a stirred crystallizer with an anchor stirr...

Embodiment 2

[0026] The vacuum rectification device adopts stainless steel bulk packing, and the number of trays is 40. Weigh 983gWO-R and add it to the still, adjust the vacuum pressure to 0.075MPa, start heating to reflux, and start to extract after the reflux is stable for 1-2hrs Fraction, the reflux ratio is 10, when the distilling temperature reaches 209°C, start to collect biphenyl fractions, stop extraction when the temperature reaches 213°C, and obtain 272.0g crude biphenyl crystals, after analysis, the biphenyl content in crude biphenyl It is 71.36wt%.

[0027] Weigh 51.6g of crude biphenyl crystallization fraction and 103.2g of absolute ethanol, add it to a stirring crystallizer with an anchor stirrer, heat to 50°C, and cool to crystallization at a cooling rate of 10K / h under stirring at a speed of 120rpm The final temperature is 10°C, filter out the biphenyl crystals, add the filtered out biphenyl crystals and absolute ethanol into the stirring crystallizer with anchor stirrer a...

Embodiment 3

[0029] The vacuum rectification device adopts stainless steel bulk packing, and the number of trays is 50. Weigh 983gWO-R and add it to the still, adjust the vacuum pressure to 0.09MPa, start heating to reflux, and start to extract after the reflux is stable for 1-2hrs. Fraction, the reflux ratio is 8, when the distillation temperature reaches 175 ° C, start to collect biphenyl fractions, stop mining when the temperature reaches 187 ° C, and obtain 268.0 g of crude biphenyl crystals, after analysis, the biphenyl content in the crude biphenyl It is 67.1wt%.

[0030] Weigh 40.0g of crude biphenyl crystallization fraction and 120g of isopropanol, put them into a stirred crystallizer with an anchor stirrer, heat to 40°C, stir at 120rpm, and cool at a cooling rate of 5K / h until crystallization is complete. Temperature 0°C, filter out biphenyl crystals, add the filtered biphenyl crystals and isopropanol into a stirred crystallizer with an anchor stirrer at a ratio of 1:3, heat to 53...

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Abstract

A process for purifying dibenzene includes such steps as recovering the gas absorber oil, single-tower vacuum rectifying to obtain the coarse dibenzene fraction (55-75%), dissolving it in alcohol solvent, cooling for crystallizing while stirring, dissolving, and recrystallizing to obtain high purity (more than 99%).

Description

technical field [0001] The invention relates to a method for purifying biphenyl, more particularly to a method for extracting high-purity biphenyl from recovered washing oil. Background technique [0002] Biphenyl is an important organic raw material with a wide range of uses. It can be mixed with biphenyl ether as a heat carrier, and can also be used to prepare many products such as emulsifiers, fluorescent whitening agents, fabric dyes, synthetic resins, liquid crystal materials, pesticides and medicines. An important derivative product. The mass fraction of biphenyl in coal tar is about 0.2-0.4%, most of which is concentrated in the wash oil fraction, and the fraction in the wash oil is about 8%. Washing oil is one of the main fractions in the process of coal tar processing. The boiling point range of tar washing oil is 230-270°C. It is rich in organic chemical raw materials such as 2-methylnaphthalene, biphenyl, acenaphthene, indole and fluorene. Because of its good st...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C7/04C07C7/14C07C15/14
Inventor 侯文杰孙剑郑胜华汪旭
Owner BAOWU CHARCOAL MATERIAL TECH CO LTD
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