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Synthesis method of selenium-containing copolymer catalyst for catalyzing oxidative chemical degradation of olefin

A technology of oxidative cracking and copolymers, which is applied in the direction of organic compound/hydride/coordination complex catalysts, physical/chemical process catalysts, chemical instruments and methods, etc. It can solve problems such as difficult large-scale application and cumbersome preparation process. Achieve strong catalytic activity, simple catalyst process, and good application value

Active Publication Date: 2019-08-09
YANGZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, some selenium-containing high polymers, such as polystyrene-loaded selenic acid, are cumbersome to prepare and difficult to apply on a large scale.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] Catalyst synthesis: Add 10 mL of ethanol solution of sodium selenium hydride (0.1 mol / L, prepared on site from selenium powder and sodium borohydride) in a 50 mL round bottom flask, add 1.3 mmol of p-dichlorobenzyl at one time under stirring, (25 o C) After stirring for 2 hours, add 0.15 mmol perfluoroethylene glycol and 0.3 mmol ethylene glycol, 40 oC After heating and stirring under low temperature for 2 hours, cool to room temperature, let stand for 24 hours, obtain the precipitate, filter and dry it in the air, which is the selenium-containing copolymer catalyst material.

[0016] Catalyst activity characterization: 20 mg of the selenium-containing copolymer catalyst material, 1 mL of 1,1-stilbene in acetonitrile (1 mol / L), 1 mL of H 2 o 2 Acetonitrile solution (by 30% H 2 o 2 Prepared with acetonitrile, concentration 1 mol / L), 80 o C was heated for 24 hours, the solvent was evaporated to dryness, and the residue was separated by preparative thin-layer chromat...

Embodiment 2

[0018] Other conditions are the same as in Example 1, and the properties of the materials synthesized by using different dihalogenated hydrocarbons are tested, and the experimental results are shown in Table 1.

[0019] Table 1 Performance comparison table of materials synthesized by different dihalogenated hydrocarbons

[0020] Numbering Dihalohydrocarbons Olefin oxidative cracking reaction yield (%) 1 p-dichlorobenzyl 90 (Example 1) 2 p-Dibromobenzyl 67 3 m-dichlorobenzyl 54 4 o-dichlorobenzyl 42 5 Dichloroethane 66 6 1,3-Dichloropropane 52 7 1,2-Dichloropropane 34

[0021] From the above results, it can be seen that the catalytic performance of the material prepared by using p-dichlorobenzyl (Example 1) is the best.

Embodiment 3

[0023] Other conditions are the same as in Example 1, and the effects of different p-dichlorobenzyl and sodium selenium hydride molar ratios are tested, and the experimental results are shown in Table 2.

[0024] The effect comparison table of different p-dichlorobenzyl and sodium selenium hydride mol ratio of table 2

[0025] Numbering p-dichlorobenzyl to sodium selenium hydride molar ratio Olefin oxidative cracking reaction yield (%) 1 1.1:1 52 2 1.2:1 72 3 1.3:1 (Example 1) 90 4 1.4:1 77 5 1.5:1 66

[0026] It can be seen from the above results that the catalytic activity of the prepared material is the highest when the molar ratio of dichlorobenzyl to sodium selenium hydride is 1.3:1 (Example 1).

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Abstract

The invention discloses a synthesis method of a selenium-containing copolymer catalyst for catalyzing oxidative chemical degradation of olefin. The method comprises the following steps that benzylidene chloride and sodium hydrogen selenide are mixed uniformly in a molar ratio of (1.2-1.4):1, stirring is performed at the room temperature for 2 hours, then perfluoroethylene glycol with 0.1-0.2 timeof the molar weight of the sodium hydrogen selenide and ethylene glycol with 0.2-0.4 time of the molar weight of the sodium hydrogen selenide are added, after heating and stirring are performed at 40DEG C for 2 hours, cooling is performed to the room temperature, standing is performed for 24 hours, a precipitate is obtained, filtered and dried, and the selenium-containing copolymer catalyst material is obtained. The material has strong catalytic activity and can catalyze the oxidative chemical degradation reaction of the olefin.

Description

technical field [0001] The invention relates to a synthesis method of a selenium-containing copolymer catalyst which catalyzes oxidative cracking of olefins, and belongs to the field of preparation of catalytic materials. Background technique [0002] Selenium-catalyzed chemistry is a new field emerging in recent years. my country is rich in selenium resources, and the development of new applications of selenium can give full play to the advantages of resources, which is in line with my country's resource characteristics. Selenium is an essential trace element for the human body. It can be metabolized by organisms and will not be deposited in the body. Therefore, it is friendly to the environment. The reaction catalyzed by selenium usually uses a green and clean oxidant, the reaction process is environmentally friendly, and has good industrial application value. [0003] However, most of the selenium-catalyzed reactions reported so far use homogeneous selenium catalysts, w...

Claims

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Application Information

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IPC IPC(8): B01J31/06C07C45/28C08G79/00C07C49/786
CPCB01J31/06B01J2231/70C07C45/28C08G79/00C07C49/786
Inventor 张旭俞亮郑英豪孙杨阳曹洪恩俞磊
Owner YANGZHOU UNIV
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