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1-phenyl-1-(p-tert-butyltolyl)ethane and its synthesis method

A technology of p-tert-butyltoluene and synthesis method, which is applied in the application field of high-temperature heat transfer oil, can solve the problems of needing alkaline water washing or hydrochloric acid decomposition, difficult control of reaction temperature, difficult industrial production, etc., and achieves low freezing point, difficult decomposition, side effects The effect of less product

Active Publication Date: 2018-06-29
JIANGSU ZHONGNENG CHEM TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

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-butyltolyl)ethane and its synthesis method
  • 1-phenyl-1-(p-tert-butyltolyl)ethane and its synthesis method

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) add p-tert-butyl toluene in the flask, add solid acidic catalyst under the condition of stirring, solid acidic catalyst accounts for 3% of reaction solution gross mass. 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 and stir for more than 1.5h, coo...

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Abstract

The invention discloses a kind of 1-phenyl-1-(p-tert-butyltolyl)ethane and a synthesis method thereof, the steps are as follows: 1) using styrene and p-tert-butyltoluene as raw materials, in the presence of a solid acid catalyst Under the action, through the alkylation reaction, the reaction formula is as follows: 2) After the reaction is completed, the solid acid catalyst needs to be separated, and the solid material composed of activated clay and magnesium oxide with a mass ratio of 10:1 is used for further adsorption and neutralization And decolorize and filter, recover excess p-tert-butyltoluene through water pump vacuum distillation, and then vacuum pump vacuum distillation to obtain. The catalyst selected in the invention can be recycled, does not pollute the environment, and simultaneously avoids the use of catalysts such as sulfuric acid, aluminum trichloride and the like which are volatile, poisonous and difficult to handle. The preparation process has the characteristics of mild and controllable, few by-products 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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Patent Type & Authority Patents(China)
IPC IPC(8): C07C2/02C07C15/16
CPCY02P20/584
Inventor 李金祥吴朝阳刘红飞陆鑫华
Owner JIANGSU ZHONGNENG CHEM TECH CO LTD
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