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Preparation method capable of reducing melt index of carbon dioxide-based polyester-polycarbonate copolymer

A technology of carbon dioxide and polycarbonate, which is applied in the field of polymer copolymerization, can solve problems such as gelation, and achieve the effects of improving thermal performance, economical and efficient metal residues, and reducing melt index

Inactive Publication Date: 2022-01-07
SUN YAT SEN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The results show that a small amount of cross-linking agent is beneficial to a significant improvement in molecular weight, thereby improving the mechanical properties of PPC, but the addition of excessive cross-linking agent produces a gel

Method used

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  • Preparation method capable of reducing melt index of carbon dioxide-based polyester-polycarbonate copolymer

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] With a 50 mL autoclave as the reaction vessel, 4 g of phthalic anhydride, 12.55 g of propylene oxide, 15 mg of tetraethylammonium chloride, 67.6 mg of diphenylmethane di Isocyanate, 170 μL tripropyl boron solution, added to the autoclave in sequence, then filled with 1.0 MPa high-purity carbon dioxide, reacted in an oil bath at 80 °C for 6 h, released the residual carbon dioxide after the reaction, and diluted the product with dichloromethane , and the catalyst was quenched with dilute hydrochloric acid / ethanol solution, the polymer was precipitated in ethanol, and dried in a vacuum oven. After drying, carry out molecular weight test, nuclear magnetic analysis and thermal property test. M n =135 kDa, PDI = 2.80, 40% polyester, 57% polycarbonate, 3% polyether, T g = 48.7 °C, and the melt index measured at 170 °C under a load of 2.16 kg was 7.3 g / 10 min.

Embodiment 2

[0025] With a 50 mL autoclave as the reaction vessel, 4 g of phthalic anhydride, 12.55 g of propylene oxide, 15 mg of tetraethylammonium chloride, and 135.2 mg of diphenylmethane di Isocyanate and 170 μL tripropyl boron solution were added to the autoclave in sequence, and then filled with 1.0 MPa high-purity carbon dioxide, and reacted in an oil bath at 80 °C for 6 h. After the reaction, the residual carbon dioxide was released, and the product was diluted with dichloromethane , and the catalyst was quenched with dilute hydrochloric acid / ethanol solution, the polymer was precipitated in ethanol, and dried in a vacuum oven. After drying, carry out molecular weight test, nuclear magnetic analysis and thermal property test. M n =154 kDa, PDI = 5.83, polyester content 41%, polycarbonate content 56%, polyether content 3%, T g = 50.0 °C, the melt index measured at 170 °C under a load of 2.16 kg is 6.5 g / 10 min.

Embodiment 3

[0027] With a 50 mL autoclave as the reaction vessel, 4 g of phthalic anhydride, 12.55 g of propylene oxide, 15 mg of tetraethylammonium chloride, and 135.2 mg of diphenylmethane di Add isocyanate and 170 μL tripropyl boron solution into the autoclave in sequence, then fill it with 3 MPa high-purity carbon dioxide, and react in an oil bath at 80 °C for 6 h, release the residual carbon dioxide after the reaction, and dilute the product with dichloromethane , and the catalyst was quenched with dilute hydrochloric acid / ethanol solution, the polymer was precipitated in ethanol, and dried in a vacuum oven. After drying, carry out molecular weight test, nuclear magnetic analysis and thermal property test. M n =210 kDa, PDI = 6.81, polyester content 36%, polycarbonate content 63%, polyether content 1%, T g =52.0 °C, the melt index measured at 170 °C under a load of 2.16 kg is 5.6 g / 10 min.

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Abstract

The invention discloses a preparation method of a carbon dioxide-based polyester-polycarbonate copolymer. The method comprises the following steps: adding reaction monomers phthalic anhydride, epoxypropane, a branching agent and a catalyst into a high-pressure reaction kettle, then introducing high-purity carbon dioxide gas, and heating to carry out ring-opening copolymerization reaction; and after the reaction is finished, performing precipitating, drying and crushing to obtain the purified branched copolymer. The copolymer is formed by copolymerization of propylene oxide, carbon dioxide, phthalic anhydride and a small amount of branching agent, and PPC-P is modified. The branching agent can open a ring and connect a polymer chain, so that the molecular weight and the distribution index of the copolymer are improved; the melt index is obviously reduced compared with that of the copolymer without adding the branching agent, so that the mechanical strength of the copolymer is improved; and the copolymer has good light transmission.

Description

technical field [0001] The invention relates to the field of polymer copolymerization, in particular to a preparation method for reducing the melt index of carbon dioxide-based polyester-polycarbonate copolymer (PPC-P). Background technique [0002] With the onset of the Industrial Revolution, carbon dioxide (CO2), the main component of the greenhouse gas 2 ) The amount emitted into the atmosphere is increasing year by year, accompanied by the intensification of the greenhouse effect. Researchers try to reduce CO in several ways 2 concentration, one of which is to use it as a raw material for a chemical reaction to synthesize CO 2 base copolymer. This provides a sustainable way to reduce the total reliance on petroleum-based raw materials in the synthesis of plastics. As a fully biodegradable material, Polypropylene Carbonate (PPC) is CO 2 Copolymer of propylene oxide (PO), good barrier properties, transparent and non-toxic. [0003] However, the glass transition temp...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G63/685C08G63/64C08G63/87C08G63/84C08G63/42
CPCC08G63/6856C08G63/64C08G63/87C08G63/84C08G63/42
Inventor 孟跃中王文静叶淑娴梁嘉欣肖敏王拴紧韩东梅黄盛
Owner SUN YAT SEN UNIV
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