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Method for preparing glyzinc under high pressure

A technology of zinc glycerol and conditions, which is applied in the preparation of metal alcohols, etc., can solve the problems of environmental protection and waste water, and achieve the effect of easy operation

Inactive Publication Date: 2011-06-15
JIANGNAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In the above methods, zinc acetate is used as a raw material, waste water will be generated during the production process, and toxic solvents are used in the later treatment of the product, and the product separation process is not environmentally friendly.

Method used

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  • Method for preparing glyzinc under high pressure
  • Method for preparing glyzinc under high pressure
  • Method for preparing glyzinc under high pressure

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Weigh 60g of glycerol and place it in a 250mL round bottom flask, heat it to 80°C under stirring conditions, add 3g of zinc oxide after reaching the temperature, mix and heat under reflux at this temperature for 5h, then move the mixture into a high-pressure reactor, The reaction was continued at ℃ for 60 h. After the reaction was completed, the reaction product was cooled to room temperature, washed with water and ethanol and repeated 3 times, and the solid was dried at 100 ℃ to constant weight after filtration to obtain the zinc glycerol product.

Embodiment 2

[0021] Weigh 60g of glycerin and place it in a 250mL round bottom flask, heat it to 120°C under stirring conditions, add 3g of zinc oxide after reaching the temperature, mix and heat under reflux at this temperature for 4h, then move the mixture into a high-pressure reactor, Continue to react at ℃ for 18 hours. After the reaction is completed, the reaction product is cooled to room temperature, washed with water and ethanol and repeated 3 times. After filtration, the solid is dried at 100 ℃ to constant weight to obtain the zinc glycerol product.

Embodiment 3

[0023] Weigh 60g of glycerol and place it in a 250mL round bottom flask, heat it to 120°C under stirring conditions, add 3g of zinc oxide after reaching the temperature, mix and heat at this temperature to reflux for 3h, then move the mixture into an autoclave, The reaction was continued at ℃ for 6 h. After the reaction was completed, the reaction product was cooled to room temperature, washed with water and ethanol and repeated 3 times, and the solid was dried at 100 ℃ to constant weight after filtration to obtain the zinc glycerol product.

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Abstract

The invention discloses a method for preparing glyzinc under the high pressure, which belongs to the technical field of chemosynthesis. In the method, the glyzinc is prepared from living being or animal and plant oil base hydrolysis byproduct glycerin serving as a raw material. The method comprises the following steps of: stirring and heating zinc oxide and glycerin for a reflux reaction, wherein the mass ratio of the zinc oxide to the glycerin is 1:10-30; and transferring a reaction mixture into a high-pressure reaction kettle for continued reacting, washing, separating and drying to obtain white product of glyzinc. The structure of the glyzinc is represented and proved by infrared spectrum and X-ray diffraction. By TEM (Transmission Electron Microscope) observation, obtained glyzinc particles have tablet irregular polygonal structures with the side lengths of between 0.5 mu m and 3.5 mu m. The obtained glyzinc can be taken as a novel main component of a non-toxic heat stabilizer. The invention has the advantages of readily available raw materials, low cost, easy synthesis, easiness and convenience in operating and easy biodegradation of a product.

Description

technical field [0001] The invention relates to a method for preparing zinc glycerol through the synthesis reaction of polyhydric groups and transition metals, in particular to a method for directly reacting ordinary zinc oxide with glycerol to synthesize zinc glycerol, which has the characteristics of economy and environmental protection. The preparation method is to directly heat zinc oxide and glycerin to reflux for a period of time, and then move the mixture into a high-pressure reactor to continue the reaction. After the reaction is completed, the white solid zinc glycerol is obtained by washing, separating, and drying. The zinc glycerol has a sheet-like micron structure. The zinc glycerol obtained by the invention can be used for polyvinyl chloride heat stabilizers, and is harmless to humans and the environment. It belongs to the technical field of chemical synthesis. Background technique [0002] Glycerol is a by-product of the hydrolysis of many animal and vegetable...

Claims

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Application Information

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IPC IPC(8): C07C31/28C07C29/70
Inventor 蒋平平宋银银董玉明薛华郭朝彬
Owner JIANGNAN UNIV
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