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Preparation method of benzyl methylbenzene

A technology of benzyltoluene and toluene, applied in the preparation field of benzyltoluene, can solve the problems of high preparation cost, complicated process, inability to overcome equipment corrosion, etc., and achieves high raw material cost, simple preparation process, catalytic reaction yield and selection high sex effect

Inactive Publication Date: 2017-05-10
郑文亚
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, neither heteropolyacids nor metal halide-supported catalysts can overcome the problem of equipment corrosion, and solid superacids, molecular sieves, and ionic liquids have problems such as high preparation costs and complicated processes.

Method used

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  • Preparation method of benzyl methylbenzene
  • Preparation method of benzyl methylbenzene
  • Preparation method of benzyl methylbenzene

Examples

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preparation example Construction

[0027] A, preparation of activated clay supported solid acid catalyst

[0028] Add 270g of water and 30g of concentrated sulfuric acid to a 1000mL four-necked bottle, then add 30g of calcium-based swelling, reflux and stir for 6 hours, cool down to room temperature for 12 hours, filter, and dry at 120°C for 8 hours to obtain solid activated clay, which is used as a catalyst carrier for future use;

[0029] B. Activated clay loaded with ZnCl 2 Preparation of solid acid catalyst

[0030] ZnCl 2 Dissolve in the acetonitrile solution, add the activated clay prepared by step A, the activated clay and ZnCl 2 The mass ratio is 10:1, stirred at room temperature for 24 hours, filtered, and then activated at 120°C for 4 hours to obtain activated clay-supported ZnCl 2 solid acid catalyst;

[0031] C. Alkylation reaction

[0032] ZnCl loaded with activated clay 2 The solid acid catalyst is added to the alkylation reaction system of benzyl chloride and toluene for catalytic reaction,...

Embodiment 1

[0041] A, preparation of activated clay supported solid acid catalyst

[0042] Add 270g of water and 30g of concentrated sulfuric acid to a 1000mL four-necked bottle, then add 30g of calcium-based swelling, reflux and stir for 6 hours, cool down to room temperature for 12 hours, filter, and dry at 120°C for 4 hours; obtain solid activated clay, which is used as a catalyst carrier for later use;

[0043] B. Activated clay loaded with ZnCl 2 Preparation of solid acid catalyst

[0044] Weigh anhydrous ZnCl 2 1.0g, dissolved in 30ml acetonitrile, fully stirred until ZnCl 2 Completely dissolve, add 10.0 g of activated clay prepared in step A, stir at room temperature for 24 hours, filter, wash the solid with 10 mL of n-hexane x 3 times, and dry at 120 ° C for 4 hours to obtain ZnCl loaded on activated clay 2 Solid acid catalyst (F / C catalyst);

[0045] C, the preparation of benzyltoluene

[0046]Take 3.2g of F / C catalyst and put it into a 500mL four-necked bottle, then add 29...

Embodiment 2

[0048] A, preparation of activated clay supported solid acid catalyst

[0049] Add 270g of water and 30g of concentrated sulfuric acid to a 1000mL four-necked bottle, then add 30g of calcium-based swelling, reflux and stir for 6 hours, cool down to room temperature for 12 hours, filter, and dry at 120°C for 8 hours to obtain solid activated clay, which is used as a catalyst carrier for future use;

[0050] B. Activated clay loaded with ZnCl 2 Preparation of solid acid catalyst

[0051] Weigh anhydrous ZnCl 2 1.0g, dissolved in 30ml acetonitrile, fully stirred until ZnCl 2 Completely dissolve, add 10.0 g of activated clay prepared in step A, stir at room temperature for 24 hours, filter, wash the solid with 10 mL of n-hexane x 3 times, and dry at 120 ° C for 4 hours to obtain ZnCl loaded on activated clay 2 Solid acid catalyst (F / C catalyst);

[0052] C, the preparation of benzyltoluene

[0053] Take 3.2g of F / C catalyst and put it into a 500mL four-necked bottle, then ad...

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Abstract

The invention relates to a preparation method of benzyl methylbenzene. The method comprises the following steps: adding concentrated sulfuric acid into calcium bentonite, stirring under reflux, and drying to obtain solid activated clay; dissolving ZnCl2 in an acetonitrile solution, adding the prepared activated clay, stirring at room temperature for 24 hours, filtering, and activating at 120 DEG C for 4 hours, thereby obtaining an activated-clay-supported ZnCl2 solid acid catalyst; adding the activated-clay-supported ZnCl2 solid acid catalyst into a benzyl chloride-methylbenzene alkylation reaction system, carrying out catalytic reaction, and filtering to recover the catalyst; and carrying out reduced pressure distillation and refinement on the benzyl methylbenzene crude product, thereby obtaining the benzyl methylbenzene. The catalyst has the advantages of abundant raw material sources, low cost, simple preparation technique and low energy consumption due to no need of high-temperature activation, and can be easily separated from the product; and when being used for carrying out synthetic reaction of benzyl methylbenzene, the catalyst has the advantages of high reaction conversion rate, high selectivity, mild conditions, low equipment corrosion and small environmental pollution, can be easily recovered and reutilized, and thus, has wide application prospects.

Description

technical field [0001] The invention belongs to the field of organic synthesis, and in particular relates to a preparation method of benzyltoluene. Background technique [0002] Benzyltoluene is a product obtained by reacting toluene with benzyl chloride in the presence of an acid catalyst, mainly including monobenzyl toluene (abbreviated as MBT) and dibenzyl toluene (abbreviated as DBT). Industrially, monobenzyltoluene and dibenzyltoluene can be used as insulating oil for power capacitors when mixed at a ratio of 3:1. The trade name is C101, and it is also called M / DBT in China. Because C101 has excellent performance and characteristics suitable for making all-film power capacitors, it is more and more widely used in the industry. Mono- and di-benzyltoluene can also be used in the preparation of SAS series power capacitor insulating oil, and as an excellent heat carrier in industry. Therefore, the application prospect of benzyltoluene is very broad. [0003] The catalyst...

Claims

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Application Information

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IPC IPC(8): C07C1/26C07C15/16B01J27/138
CPCC07C1/26B01J27/138C07C15/16
Inventor 杨连成陈明陈海波魏永刚郑文亚
Owner 郑文亚
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