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1-phenyl-1-(p-tert-butyl methylphenyl)ethane and synthesis method thereof

A technology of p-tert-butyltoluene and a synthesis method, which is applied in chemical instruments and methods, carbon compound catalysts, and the production of hydrocarbons by addition of unsaturated hydrocarbons, etc. It is difficult to industrialize production and other problems, and achieves the effect of low freezing point, not easy to decompose, and less by-products.

Active Publication Date: 2016-08-03
JIANGSU ZHONGNENG CHEM TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

It has been reported in the literature that diaryl alkanes mainly use the following synthetic methods: one is to use concentrated sulfuric acid or anhydrous aluminum trichloride to catalyze the alkylation reaction of styrene and alkyl aromatics, but the reaction temperature is not easy to control, and the by-products Many, the yield is low, and the post-treatment needs alkaline water washing or hydrochloric acid decomposition treatment, which seriously pollutes the environment
Another method is to use superacid catalysis method, but because the preparation of superacid produces a large amount of waste water, and needs to be treated at 500-600 ℃ high temperature, so this method is difficult to carry out industrial production

Method used

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  • 1-phenyl-1-(p-tert-butyl methylphenyl)ethane and synthesis method thereof
  • 1-phenyl-1-(p-tert-butyl methylphenyl)ethane and synthesis method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0019] A kind of synthetic method of 1-phenyl-1-(p-tert-butyltolyl) ethane, comprises the steps:

[0020] 1) P-tert-butyltoluene is added into the flask, and a solid acidic catalyst is added under stirring conditions, and the solid acidic catalyst accounts for 2.5% of the total mass of the reaction solution. In the solid acid catalyst, the mass ratio of solid acid to bismuth p-toluenesulfonate is 1:1;

[0021] 2) Heating with a heating mantle, the temperature rose to 125°C, and slowly added styrene dropwise for 2 hours. In this example, the molar ratio of p-tert-butyltoluene:styrene=7.0:1;

[0022] 3) After the dropwise addition, continue to stir for 10 minutes, cool it to below 10°C to fully separate the catalyst, filter and recover the catalyst;

[0023] 4) adding magnesium oxide and activated clay with a mass ratio of 1:10 to the filtrate, the total amount of magnesium oxide and activated clay accounts for 1-2% of the weight of the entire reaction solution. Heat to 80°C a...

Embodiment 2

[0029] A kind of synthetic method of 1-phenyl-1-(p-tert-butyltolyl) ethane, comprises the steps:

[0030] 1) P-tert-butyltoluene is added into the flask, and a solid acidic catalyst is added under stirring conditions, and the solid acidic catalyst accounts for 4.5% of the total mass of the reaction solution. In the solid acid catalyst, the mass ratio of solid acid to bismuth p-toluenesulfonate is 1:1;

[0031] 2) Use a heating mantle to heat, the temperature rises to 150° C., and slowly add styrene dropwise for 2 hours. In this example, the molar ratio of p-tert-butyltoluene:styrene=5.5:1;

[0032] 3) After the dropwise addition, continue to stir for 10 minutes, cool it to below 10°C to fully separate the catalyst, filter and recover the catalyst;

[0033] 4) adding magnesium oxide and activated clay with a mass ratio of 1:10 to the filtrate, the total amount of magnesium oxide and activated clay accounts for 1-2% of the weight of the entire reaction solution. Heat to 80°C a...

Embodiment 3

[0039] A kind of synthetic method of 1-phenyl-1-(p-tert-butyltolyl) ethane, comprises the steps:

[0040] 1) P-tert-butyltoluene is added into the flask, and a solid acidic catalyst is added under stirring conditions, and the solid acidic catalyst accounts for 3% of the total mass of the reaction solution. In the solid acid catalyst, the mass ratio of solid acid to bismuth p-toluenesulfonate is 1:1;

[0041] 2) Use a heating mantle to heat, the temperature rises to 100° C., and slowly add styrene dropwise for 2 hours. In this embodiment, the molar ratio of p-tert-butyltoluene:styrene=6:1;

[0042] 3) After the dropwise addition, continue to stir for 10 minutes, cool it to below 10°C to fully separate the catalyst, filter and recover the catalyst;

[0043] 4) adding magnesium oxide and activated clay with a mass ratio of 1:10 to the filtrate, the total amount of magnesium oxide and activated clay accounts for 1-2% of the weight of the entire reaction solution. Heat to 80°C an...

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Abstract

The invention discloses 1-phenyl-1-(p-tert-butyl methylphenyl)ethane and a synthesis method thereof. The synthesis method comprises the following steps: 1) with styrene and p-tert-butyl toluene as raw materials and under the effect of a solid acid catalyst, performing an alkylation reaction, wherein the reaction formula is shown in the specification; and 2) after the reaction, separating the solid acid catalyst; performing further adsorption, neutralization and decoloration filtration using a solid material consisting of activated clay and magnesium oxide in a mass ratio of 10:1; performing reduced-pressure distillation through a water pump to recycle excess p-tert-butyl toluene; and performing reduced-pressure distillation through a vacuum pump to obtain 1-phenyl-1-(p-tert-butyl methylphenyl)ethane. In the invention, the adopted catalyst can be recycled to avoid environmental pollution; and meanwhile, the use of volatile, toxic and hard-to-treat catalysts such as sulfuric acid and aluminum trichloride is avoided. The preparation technology has the characteristics of mildness and controllability, few byproducts and high yield.

Description

technical field [0001] The invention relates to the category of green chemistry, belongs to the application field of high-temperature heat transfer oil, and specifically relates to 1-phenyl-1-(p-tert-butylmethylphenyl)ethane and a synthesis method thereof. Background technique [0002] Diaryl ethane derivatives are a very important class of high-temperature heat transfer oils, mainly used for high-temperature heat transfer. It has been reported in the literature that diaryl alkanes mainly use the following synthetic methods: one is to use concentrated sulfuric acid or anhydrous aluminum trichloride to catalyze the alkylation reaction of styrene and alkyl aromatics, but the reaction temperature is not easy to control, and the by-products Many, the yield is low, and the post-treatment needs alkaline water washing or hydrochloric acid decomposition treatment, which seriously pollutes the environment. Another method is to use a superacid catalysis method, but because the prepar...

Claims

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Application Information

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IPC IPC(8): C07C2/02C07C15/16
CPCY02P20/584C07C2/02C07C2531/025C07C15/16
Inventor 李金祥吴朝阳刘红飞陆鑫华
Owner JIANGSU ZHONGNENG CHEM TECH CO LTD
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