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Preparation method for attapulgite clay-based cycloaddition reaction catalyst

A technology of attapulgite clay and catalyst, which is applied in chemical instruments and methods, physical/chemical process catalysts, chemical/physical processes, etc. It can solve problems such as equipment corrosion, environmental pollution, and separation of difficult products, and achieve low production costs. Reduce environmental pollution and save solvent

Inactive Publication Date: 2014-05-07
CHANGZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The technical problem to be solved by the present invention is: for some difficult Diels-Alder reactions, need to use Lewis acid ZnCl 2 As a catalyst to promote the reaction, but ZnCl 2 As a catalyst, it is not only difficult to separate from the product during use, but also causes problems such as equipment corrosion and environmental pollution.

Method used

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  • Preparation method for attapulgite clay-based cycloaddition reaction catalyst
  • Preparation method for attapulgite clay-based cycloaddition reaction catalyst
  • Preparation method for attapulgite clay-based cycloaddition reaction catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] 1. Weigh 100 grams of attapulgite after drying and 5 grams of anhydrous zinc chloride respectively, mix them and add them to the ball mill tank of the ball mill, open the ball mill, and after running for 0.5 hours, collect the powder after ball milling,

[0023] The planetary ball mill QM-1SP2 is used here, and the ball milling is carried out under the protection of argon atmosphere and anhydrous and oxygen-free conditions. When the amount of zinc mixture is large, the ball milling operation can be carried out several times);

[0024] 2. Move the ball-milled powder obtained in step (1) into the roasting furnace, 2 Under the atmosphere, the temperature is raised to 250°C at a rate of 3°C / min, roasted at a constant temperature for 2 hours, and cooled to obtain ZnCl 2 / Attapulgite-supported cycloaddition catalyst.

Embodiment 2

[0026] 1. Weigh 100 grams of attapulgite after drying and 20 grams of anhydrous zinc chloride respectively, mix them and add them to the ball mill tank of the ball mill, open the ball mill, and after running for 10 hours, collect the powder after ball milling,

[0027] The planetary ball mill QM-1SP2 is used here, and the ball milling is carried out under the protection of argon atmosphere and anhydrous and oxygen-free conditions. When the amount of zinc mixture is large, the ball milling operation can be carried out several times);

[0028] 2. Move the ball-milled powder obtained in step (1) into the roasting furnace, 2 Under the atmosphere, the temperature was raised to 250°C at a rate of 8°C / min, roasted at a constant temperature for 8 hours, and cooled to obtain ZnCl 2 / Attapulgite-supported cycloaddition catalyst.

Embodiment 3

[0030] 1. Weigh 100 grams of attapulgite after drying and 15 grams of anhydrous zinc chloride respectively, mix them and add them to the ball mill tank of the ball mill, open the ball mill, and after running for 6 hours, collect the powder after ball milling,

[0031] The planetary ball mill QM-1SP2 is used here, and the ball mill is carried out under the protection of argon atmosphere and anhydrous and oxygen-free conditions. When the amount of zinc mixture is large, the ball milling operation can be carried out several times);

[0032] 2. Move the ball-milled powder obtained in step (1) into the roasting furnace, 2 Under the atmosphere, the temperature is raised to 250°C at a rate of 5°C / min, roasted at a constant temperature for 4 hours, and cooled to obtain ZnCl 2 / Attapulgite-supported cycloaddition catalyst.

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Abstract

The invention belongs to the field of catalyst preparation and in particular relates to a preparation method for an attapulgite clay-based solid catalyst for green catalytic Diels-Alder reaction (cycloaddition reaction). The preparation method comprises the steps of loading a proper amount of zinc chloride serving as a raw material into inner holes of attapulgite clay serving as a raw material by a solid-phase reaction method (a high-speed ball-grinding method), and then performing roasting activation to obtain a catalyst for synthesizing attapulgite clay-based C22-ring fat glycerol ester. The prepared solid catalyst is easily separated from a product, so that equipment corrosion and environment pollution are alleviated; in a loaded type catalyst, ZnCl2 and the surface of the attapulgite clay generate chemical bonding action to form a new amorphous substance; the activity of the amorphous substance is higher than a sum of the activity of the ZnCl2 and the activity of the attapulgite clay.

Description

technical field [0001] The invention belongs to the field of catalyst preparation, in particular to a method for preparing an attapulgite clay-based solid catalyst used for green catalytic Diels-Alder reaction (cycloaddition reaction). Background technique [0002] The Diels-Alder reaction is one of the very important means of carbon-carbon bond formation in organic chemical synthesis reactions, and it is also one of the commonly used reactions in modern organic synthesis. For example, in the field of chemical industry, C22-cycloaliphatic triesters are prepared by Diels-Alder reaction. C22-cyclic fatty acid triester is a kind of biological plasticizer synthesized by using various vegetable oils as raw materials, using polyunsaturated fatty acids, and maleic acid esters through Diels-Alder reaction. This type of plasticizer has high flash point, low migration, low volatility, good compatibility with PVC, and significantly improved flexibility and durability of plasticized PV...

Claims

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Application Information

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IPC IPC(8): B01J27/138
Inventor 王车礼刘高伟姚超王建浩曾桂凤周永生李为民吴康
Owner CHANGZHOU UNIV
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