Preparation method and application of corn amylose supported catalyst

A supported catalyst and corn starch technology, applied in catalytic reactions, chemical instruments and methods, physical/chemical process catalysts, etc., can solve problems such as difficult recycling, environmental pollution, etc., and achieve simple preparation, low price, and natural abundance Effect

Inactive Publication Date: 2016-11-09
NANJING FORESTRY UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In addition, because homogeneous catalysts are difficult to separate contaminated products from the reaction system, are not easy to recycle, and m...

Method used

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  • Preparation method and application of corn amylose supported catalyst
  • Preparation method and application of corn amylose supported catalyst
  • Preparation method and application of corn amylose supported catalyst

Examples

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preparation example Construction

[0017] A kind of preparation method of amylose cornstarch supported catalyst, its preparation method reaction formula is:

[0018]

[0019] The specific preparation method comprises the following steps:

[0020] (1) The amylose cornstarch is firstly expanded to increase the specific surface area and pore volume to prepare rigid and porous expanded cornstarch;

[0021] (2) react with 3-aminopropyl triethoxy silicon to prepare aminated cornstarch,

[0022] (3) Schiff base reaction with acetylacetone metal complex, and condensation to obtain amylose corn starch-supported catalyst.

[0023] The step (1) prepares rigid and porous expanded corn starch: add 2-8 g of amylose corn starch, add 20-200 mL of deionized water, and heat at 100-130°C for 40-50 min to obtain a gel, and placed in a refrigerator at 5°C for 24 h; after filtration, the solid was washed with ethanol to obtain rigid and porous expanded cornstarch.

[0024] The step (2) prepares the aminated expanded cornstarch...

Embodiment 1

[0035] Preparation of Amylose Corn Starch Supported Catalyst.

[0036] Preparation of rigid and porous expanded corn starch: 5 g of high-amylose corn starch was added to 100 mL of deionized water, heated at 120 °C for 45 min to obtain a gel, and placed in a refrigerator at 5 °C for 24 h. After filtration, the solid was washed with ethanol to obtain a rigid porous expanded cornstarch.

[0037] Preparation of aminated expanded cornstarch: 4.23 g of expanded cornstarch, 35 mL of dry toluene, under the protection of nitrogen, slowly add 4.82 g of 3-aminopropyltriethoxysilane dropwise, and react under reflux for 24 h, after the reaction is finished, cool to room temperature, add 135 mL of ethanol, after filtering, wash with ethanol to obtain aminated expanded cornstarch;

[0038] Preparation of amylose-loaded catalyst: 2 g of aminated expanded corn starch, 0.3 g of molybdenum acetylacetonate, reflux reaction in toluene solution under nitrogen protection for 24 h, filtered after th...

Embodiment 2

[0043] Applications of amylose-supported catalysts.

[0044] Preparation of anhydrous tert-butyl hydroperoxide (TBHP): 1 mL of TBHP was extracted three times with 1 mL of toluene, the organic phases were combined and dried with anhydrous sodium sulfate to obtain anhydrous tert-butyl hydroperoxide (TBHP) .

[0045] Add 0.97 g of anhydrous TBHP to 1 g of tallow catalpa oil, 0.29 g of amylose-loaded catalyst, and react for 2 h under toluene reflux. After the reaction, remove the catalyst by filtration, put the filtrate in an ice bath, and add 15% Sodium thiosulfate aqueous solution, and indicated by starch solution with iodine added, the organic phase was separated, dried with anhydrous sodium sulfate, filtered, and the solvent was distilled off under reduced pressure to obtain epoxidized vegetable oil with a conversion rate of 78.5%. The yield was 67.1%, and the selectivity was 85.5%.

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Abstract

The invention discloses a preparation method and an application of a corn amylose supported catalyst. The preparation method comprises steps as follows: firstly, corn amylose is puffed for increasing the specific surface area and pore volume; then, the puffed corn amylose and 3-aminopropyltriethoxysilane are subjected to a reaction, and ammonified corn starch is obtained; finally, the ammonified corn starch and an acetylacetone metal complex are subjected to a Schiff base reaction, and the corn starch immobilized catalyst is obtained through condensation. The corn amylose supported catalyst can be applied to catalysis of vegetable oil for an epoxidation reaction, and epoxidized plant oil is obtained. The solid catalyst synthesized with the preparation method overcomes the defect of a homogeneous catalyst, and has the advantages of being easy to prepare, green, environment-friendly, high in catalytic activity, reusable and low in cost, and is a good solid catalyst for an olefin carboamidation reaction, oxicracking of an aryl epoxy compound, oxidation of thioether, an epoxidation reaction of olefin and the like.

Description

technical field [0001] The invention specifically relates to a preparation method and application of an amylose cornstarch-loaded catalyst. The invention belongs to the technical field of preparation of solid catalysts. Background technique [0002] Acetylacetone metal complexes are important homogeneous catalysts that have been widely used in many organic synthesis reactions, such as aminocarbonylation of alkenes, oxidative cleavage of aryl epoxides, oxidation of thioethers, and epoxides of alkenes. chemical reaction, etc. Recently, it has been reported that the catalytic activity and selectivity of supported acetylacetonate metal complexes are superior to the corresponding homogeneous acetylacetonate metal complexes. In addition, because homogeneous catalysts are difficult to separate contaminated products from the reaction system, are not easy to recycle, and may cause environmental pollution, there are constant attempts to immobilize acetylacetone metal complexes on ca...

Claims

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Application Information

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IPC IPC(8): B01J31/22B01J31/06C11C3/00
CPCB01J31/2234B01J31/063B01J2231/72C11C3/006
Inventor 洪梅颜俊敏
Owner NANJING FORESTRY UNIV
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