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A kind of synthetic method of 1,1,3-trimethyl-3-phenylindane

A technology of phenylindane and synthesis method, which is applied in the direction of chemical instruments and methods, hydrocarbons, hydrocarbons, etc., and can solve problems such as not being environmentally friendly, violent reactions, troublesome product separation, etc.

Active Publication Date: 2016-01-06
INSIGHT HIGH TECH (BEIJING) CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method not only overcomes the problems of violent reaction and many by-products in the solvent-free polymerization of α-methylstyrene, but also avoids the problems of troublesome product separation, high cost and environmental protection caused by the polymerization with solvents.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0013] Add 10g of 1,1,3-trimethyl-3-phenylindane and 0.5g of methanesulfonic acid into the reactor, heat to 100°C, then slowly add 100g of raw material α-methylstyrene, the addition is complete, Keep the reaction temperature at 100-120°C and continue the reaction for 3 hours. After the reaction is completed, the reaction solution A is obtained, and recrystallized from ethanol to obtain 108g of white crystals of 1,1,3-trimethyl-3-phenylindane, the content is 99.2%, and the melting point is 51- 53°C, yield 97.4%.

Embodiment 2

[0017] According to the operation of Example 1, the reaction liquid A was obtained, and 20 g was added to the reactor, and then 1 g of methanesulfonic acid was added, heated to 140 ° C, and then 100 g of raw material α-methylstyrene was slowly added, and the temperature was kept at 140 ° C, and the addition was completed , keep the reaction temperature at 140-150°C, continue the reaction for 3h, the reaction is completed, and the analytical purity is 98.2%. Recrystallization from ethanol gave 118 g of white crystals of 1,1,3-trimethyl-3-phenylindane with a content of 99.4% and a yield of 97.6%.

Embodiment 3

[0019] Add 5g of 1,1,3-trimethyl-3-phenylindane (obtained in Example 1), 0.5g of concentrated sulfuric acid into the reactor, heat to 130°C, and then slowly add 100g of raw material α-methylbenzene After the addition of ethylene, keep the reaction temperature at 130-140°C and continue the reaction for 4 hours. After the reaction is complete, stop stirring, separate the concentrated sulfuric acid after standing still, and distill under reduced pressure to obtain 1,1,3-trimethyl-3-phenylindane White solid 103g, content 99.3%, yield 97.1%.

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Abstract

The invention relates to a synthetic method of alpha-methylstyrene cyclodimer, that is 1,1,3-trimethyl-3-phenyl indane. The method comprises the following steps: adding a certain amount of 1,1,3-trimethyl-3-phenyl indane products, or a reaction solution containing the product, and a catalytic amount of acidic catalysts into a reactor, heating, adding a raw material of alpha-methylstyrene, reacting with heat insulation, and after the reaction, performing crystallization or distillation to obtain the target product with a content being more than 99%. The method has the characteristics of simple operation, no solvent consumption, low cost, and high product quality.

Description

technical field [0001] The invention relates to a method for synthesizing α-methylstyrene ring dimer, that is, 1,1,3-trimethyl-3-phenylindane. Background technique [0002] α-Methylstyrene ring dimer, also known as 1,1,3-trimethyl-3-phenylindane, is a colorless crystal, soluble in ethanol, ether, chloroform and other organic solvents, insoluble in water. Because it has good compatibility with many polymer materials, and because of its indane ring structure, it is not easy to degrade, and has good thermal stability and oxidation resistance. It can be used in many special occasions, such as lubricants, Heat transfer medium, plasticizer and processing aid, spice filler, etc., in addition, it can also be used as a transport medium for inorganic particles in the electronics industry. [0003] The synthesis of α-methylstyrene ring dimer is obtained by polymerizing α-methylstyrene under the action of an acidic catalyst. The polymerization reaction is carried out under normal pres...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C13/465C07C2/42
Inventor 赵文超闫庆金李静李家齐
Owner INSIGHT HIGH TECH (BEIJING) CO LTD