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Zinc hydroxy acid complex catalyst for copolymerization of carbon dioxide and propylene oxide and preparation method

A technology of propylene oxide and zinc hydroxy acid, which is applied in the field of zinc hydroxy acid complex catalysts and its preparation, can solve the problems of cumbersome preparation, low polymer glass transition temperature, and low efficiency, and achieve good selectivity and preparation Simple process and high catalytic efficiency

Inactive Publication Date: 2012-09-26
广州科梦催化材料有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the classic catalytic system of this reaction has the following categories: (1) diethyl zinc and water of equimolar number, the main catalyst diethyl zinc of this system is very sensitive to trace water vapor and oxygen, is difficult to operate, and still needs to use Large quantities of strictly dry solvent dioxane, which is costly and inefficient
(2) Adopting porphyrin metal complexes as catalysts, although the catalytic efficiency is greatly improved, the preparation of such complexes and raw materials thereof is cumbersome, and the price is also quite high, and the glass transition temperature of the polymer prepared is very high. Low

Method used

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  • Zinc hydroxy acid complex catalyst for copolymerization of carbon dioxide and propylene oxide and preparation method
  • Zinc hydroxy acid complex catalyst for copolymerization of carbon dioxide and propylene oxide and preparation method
  • Zinc hydroxy acid complex catalyst for copolymerization of carbon dioxide and propylene oxide and preparation method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] 1.25g (0.01mol) of zinc carbonate was dissolved in 10mL of 2M dilute hydrochloric acid, then the zinc carbonate hydrochloric acid solution was added dropwise to 1.52g (0.02mol) of α-hydroxyacetic acid in 10mL of ionic aqueous solution, refluxed for 5h, cooled and placed for 10h to precipitate zinc α- Glycolic acid complex Zn 2+ {CH 2 (O)COO-} 2 ·2H 2 O. It was collected with a Buchner funnel, and subjected to elemental analysis after drying. Theoretical values: C, 19.10; H, 4.01. Tested: C, 19.28; H, 4.01. The dried zinc α-hydroxyacetic acid complex was treated in a drying oven at 200° C. for 10 h, and then placed in a desiccator for cooling for later use.

[0026] Catalytic activity evaluation: add 0.5g of catalyst in a 500ml autoclave, vacuum dry at 70°C for 24 hours, then cool down to room temperature, then add 100ml of propylene oxide (PO), fill with carbon dioxide and heat, and finally make the pressure in the autoclave reach 4.5MPa, the temperature in the ke...

Embodiment 2

[0028] 1.25g (0.01mol) of zinc carbonate was dissolved in 10mL of 2M dilute hydrochloric acid, then the zinc carbonate hydrochloric acid solution was added dropwise to 2.08g (0.02mol) of α,α-dimethyl-α-hydroxyacetic acid in 15mL of ionic aqueous solution, and the reaction was refluxed for 5h , cooled and placed for 10h to precipitate zinc α,α-dimethyl-α-hydroxyacetic acid complex Zn 2+ {CH 3 CH 3 C(O)COO -} 2 ·2H 2 O. It was collected with a Buchner funnel, and subjected to elemental analysis after drying. Theoretical values: C, 31.24; H, 5.90. Tested: C, 31.28; H, 5.95. The dried zinc α,α-dimethyl-α-hydroxyacetic acid complex was treated in a drying oven at 200° C. for 10 hours, and then placed in a desiccator for cooling for later use.

[0029] Catalytic activity evaluation: add 0.5g of catalyst in a 500ml autoclave, vacuum dry at 70°C for 24 hours, then cool down to room temperature, then add 100ml of propylene oxide (PO), fill with carbon dioxide and heat, and final...

Embodiment 3

[0031] 1.25g (0.01mol) of zinc carbonate was dissolved in 10mL of 2M dilute hydrochloric acid, then the zinc carbonate hydrochloric acid solution was added dropwise to 2.08g (0.02mol) of α-hydroxybutyric acid in 15mL of ionic aqueous solution, refluxed for 5h, cooled and placed for 10h to precipitate zinc α -Hydroxybutyric acid complex Zn 2+ {CH 3 CH 2 CH(O)COO -} 2 ·2H 2 O. Collect with Buchner funnel, collect with Buchner funnel, carry out elemental analysis after drying, theoretical value: C, 31.24; H, 5.90. Tested: C, 31.30; H, 5.95. The dried zinc α-hydroxybutyric acid complex was treated in a drying oven at 200° C. for 10 hours, and then placed in a desiccator for cooling for later use.

[0032]Catalytic activity evaluation: add 0.5g of catalyst in a 500ml autoclave, vacuum dry at 70°C for 24 hours, then cool down to room temperature, then add 100ml of propylene oxide (PO), fill with carbon dioxide and heat, and finally make the pressure in the autoclave reach 4....

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Abstract

The invention discloses a zinc hydroxy acid complex catalyst for the copolymerization of carbon dioxide and propylene oxide and a preparation method. The catalyst is a zinc hydroxy acid complex catalyst and is obtained through the following steps of: using zinc carbonate, diluted hydrochloric acid and hydroxyl substituted aliphatic acid as initiators; preparing a zinc hydroxy acid complex througha hydrothermal process; and activating the zinc hydroxy acid complex at high temperature. The catalyst is convenient to use, after the catalyst is put in a high-pressure kettle and dried in vacuum, the temperature of the catalyst is dropped to be below reaction temperature, and then the propylene oxide and the carbon dioxide are added and heated under high pressure to react for 20-40 hours to obtain polyalkalene carbonic ester with a polymer of a number-average molecular weight larger than 50 thousands. The catalyst has simple use, high catalytic activity being larger than 80 gram polymer / gram zinc, good selectivity and high catalytic efficiency.

Description

technical field [0001] The invention belongs to the field of chemical industry, and in particular relates to a zinc hydroxy acid complex catalyst and its preparation technology and application. Background technique [0002] Polycarbonate is a common material in daily life. Due to its colorless transparency and excellent impact resistance, it is widely used in the field of chemical products. Common applications include disposable plastic water bottles and reused plastic water bottles, optical discs, spectacle lenses, Water bottles, bulletproof glass, goggles, bank bulletproof glass, headlights, etc. The research and development of polycarbonate belongs to the new material project of my country's high-tech industrialization, and it is a project supported by the national industrialization policy. [0003] Aliphatic polycarbonate can be obtained by alternating copolymerization of epoxy compound and carbon dioxide, among which polyalkylene carbonate is an important one, which ca...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G64/34C07C51/41C07C59/06C07C59/01
Inventor 李秀华孟跃中肖敏王拴紧韩东梅权胜利
Owner 广州科梦催化材料有限公司