Method for catalytic synthesis of benzyl toluene by activated clay-loaded ferric trichloride (FeCl3) solid acid catalyst

A technology of solid acid catalyst and activated clay, which is applied to carbon compound catalysts, physical/chemical process catalysts, catalysts, etc., can solve the problems of high preparation cost, inability to overcome equipment corrosion, complex process, etc., and achieves low preparation cost and catalytic reaction. The effect of high yield and selectivity, and simple preparation process

Inactive Publication Date: 2017-05-17
郑文亚
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  • Abstract
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  • Application Information

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Problems solved by technology

However, neither heteropolyacids nor metal halide-supported catalysts can overcome the problem of equipment corrosion, an...

Method used

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  • Method for catalytic synthesis of benzyl toluene by activated clay-loaded ferric trichloride (FeCl3) solid acid catalyst
  • Method for catalytic synthesis of benzyl toluene by activated clay-loaded ferric trichloride (FeCl3) solid acid catalyst
  • Method for catalytic synthesis of benzyl toluene by activated clay-loaded ferric trichloride (FeCl3) solid acid catalyst

Examples

Experimental program
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preparation example Construction

[0028] A, preparation of activated clay supported solid acid catalyst

[0029] 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 6h, cool down to room temperature for 12h, filter, and dry at 120°C for 8h; solid activated clay is obtained and used as a catalyst carrier for later use;

[0030] B. Activated clay loaded with FeCl 3 Preparation of solid acid catalyst

[0031] FeCl 3 Dissolve in the acetonitrile solution, add the activated clay prepared by step A, the activated clay and FeCl 3 The mass ratio is 12:1, stirred at room temperature for 24 hours, filtered, and then activated at 120°C for 4 hours to obtain FeCl loaded on activated clay 3 solid acid catalyst;

[0032] C. Alkylation synthesis reaction of benzyltoluene

[0033] Activated clay loaded FeCl 3 The solid acid catalyst is added to the alkylation reaction system of benzyl chloride and toluene for catalytic reacti...

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-neck 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;

[0043] B. Activated clay loaded with FeCl 3 Preparation of solid acid catalyst

[0044] Weigh anhydrous FeCl 3 1.0g, dissolved in 30mL acetonitrile, fully stirred until FeCl 3 Completely dissolve, use 12.0g of activated clay prepared in step A as a catalyst carrier, stir at room temperature for 12h, filter, wash the solid with 10mL of n-hexane x 3 times, and dry at 120°C for 4h to obtain FeCl loaded on activated clay 3 Solid acid catalyst (F / C catalyst);

[0045] C. Alkylation synthesis reaction of benzyltoluene

[0046]Take 4g of F / C catalyst and put it into a 500mL four-neck flask, then add 280g of toluene, raise the temperatu...

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;

[0050] B. Activated clay loaded with FeCl 3 Preparation of solid acid catalyst

[0051] Weigh anhydrous FeCl 3 1.0g, dissolved in 30mL acetonitrile, fully stirred until FeCl 3 Completely dissolve, use 12.0g of activated clay prepared in step A as a catalyst carrier, stir at room temperature for 12h, filter, wash the solid with 10mL of n-hexane x 3 times, and dry at 120°C for 4h to obtain FeCl supported on activated clay 3 Solid acid catalyst (F / C catalyst);

[0052] C. Take 3.2g of F / C catalyst and put it into a 500mL four-necked bottle, then add 240g of toluene, raise the temperature to 105°C, add 80g of benzyl chloride dropwi...

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Abstract

The invention relates to a method for catalytic synthesis of benzyl toluene by an activated clay-loaded ferric trichloride (FeCl3) solid acid catalyst. The method comprises the following steps: adding calcium-based bentonite with concentrated sulfuric acid, performing backflow stirring and drying to obtain solid activated clay; dissolving the FeCl3 in an acetonitrile solution, adding the prepared activated clay, stirring for 24 hours at a room temperature, filtering and activating at a temperature of 120 DEG C to obtain the activated clay-loaded FeCl3 solid acid catalyst; adding the activated clay-loaded FeCl3 solid acid catalyst in an alkylation reaction system of benzyl chloride and toluene for catalytic reaction, filtering and recovering the catalyst; performing reduced-pressure distillation and refinement on a benzyl toluene crude product to obtain benzyl toluene. The method provided by the invention has the advantages that the catalyst is rich in raw material source, low in cost, simple in preparation process, low in energy consumption due to no need of high temperature activation and easy for separation from the product; when the catalyst is used for the synthetic reaction of the benzyl toluene, the reaction conversion rate is high, the selectivity is strong, conditions are mild, the equipment corrosion is low, the catalyst is easy to recover and can be reused, and the environment pollution is less, so that the application prospect is wide.

Description

technical field [0001] The invention belongs to the field of organic synthesis, and relates to a method for preparing benzyltoluene, in particular to a method for catalytically synthesizing benzyltoluene with an active clay-supported ferric chloride solid acid catalyst. Background technique [0002] Benzyl toluene mainly includes monobenzyl toluene (Monobenzyl Toluene, abbreviated as MBT) and dibenzyl toluene (Dibenzyl Toluene, abbreviated as DBT). Industrially, monobenzyltoluene and bisbenzyltoluene can be used as insulating oil for power capacitors when mixed at a ratio of 3:1, and the trade name is C101. 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 b...

Claims

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Application Information

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IPC IPC(8): C07C15/16C07C2/86B01J27/128
CPCY02P20/52C07C2/861B01J27/128C07C2527/128C07C15/16
Inventor 杨连成陈明陈海波魏永刚郑文亚
Owner 郑文亚
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