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Low-smoke low-heat intrinsic flame-retardant copolycarbonate as well as preparation method and application thereof

A technology for flame-retardant copolycarbonate and copolycarbonate, which is applied in the field of copolycarbonate and its preparation and application, can solve the problems of undisclosed heat release data, reduced polycarbonate smoke emission, and no obvious contribution, etc. Easy to control and industrialized production, durable flame retardant performance, good anti-melting effect

Active Publication Date: 2022-05-10
SICHUAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

When the copolycarbonate containing halogen is burned, although it can capture active H and OH free radicals by releasing halogen free radicals X to achieve low smoke, low heat release and high-efficiency flame retardancy, the combustion process produces The biologically toxic halogen-containing compounds HX and HOX are harmful to the environment and the human body (PolymInt. 2005, 54, 981–998), and are facing the situation of being phased out
Other disclosed flame-retardant copolycarbonates, such as the silicon-containing copolycarbonate prepared by ZL202110098391.5, can pass the V-0 grade and the limiting oxygen index can reach 36-38%, but on the one hand, for the other two flame-retardant Important indicators—smoke and heat release data are not disclosed. On the other hand, it is prepared by the interface method with the participation of triphosgene. This method will produce organic waste liquid containing ethanol and methylene chloride during the preparation process. and alkaline wastewater, polluting the environment
Another example is ZL201911165116.X, which introduces flame retardant monomers containing DOPO structure into polycarbonate through melt copolymerization. Although it can pass the V-0 level test, the flame retardant monomers with DOPO structure are mainly gas phase flame retardant mechanisms. , has no significant contribution to reducing polycarbonate smoke emissions

Method used

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  • Low-smoke low-heat intrinsic flame-retardant copolycarbonate as well as preparation method and application thereof
  • Low-smoke low-heat intrinsic flame-retardant copolycarbonate as well as preparation method and application thereof
  • Low-smoke low-heat intrinsic flame-retardant copolycarbonate as well as preparation method and application thereof

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Experimental program
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Effect test

Embodiment 1

[0038] Add 73.1g of bisphenol A, 92.5g of diphenyl carbonate, and 14.9g of 4,4'-dihydroxybiphenyl into the polymerization device, and raise the temperature to 160°C under the protection of a nitrogen atmosphere. After it is completely melted, add the catalyst 4-dihydroxybiphenyl Aminopyridine 2mg, carry out transesterification reaction under 3000Pa vacuum degree for 30min; heat up to 200°C, adjust vacuum degree to 2000Pa, react for 30min; start prepolymerization after transesterification, adjust temperature to 220°C, vacuum degree to 1200Pa, prepolymerization reaction for 30min; then add polycondensation catalyst sodium hydroxide 0.8mg, antioxidant tetrakis [β-(3,5-di-tert-butyl-4-hydroxyphenyl)] pentaerythritol ester and octyl under the protection of nitrogen atmosphere 0.15g each of diphenylamine and 5.3g of hydroxyl-terminated polysiloxane, the vacuum degree was gradually adjusted to <100Pa and the polycondensation reaction was carried out for 30 minutes; the temperature was...

Embodiment 2

[0041] Add 73.1g of bisphenol A, 92.5g of diphenyl carbonate, and 12.8g of 2,7-dihydroxynaphthalene into the polymerization device, and raise the temperature to 180°C under the protection of a nitrogen atmosphere. After it is completely melted, add the catalyst 4-dimethyl Aminopyridine 2 mg, carry out transesterification reaction under a vacuum of 2500Pa for 30min; raise the temperature to 200°C, adjust the vacuum to 2000Pa, and react for 30min; start prepolymerization after the transesterification is completed, adjust the temperature to 240°C, and adjust the vacuum to 1500Pa , prepolymerization reaction for 30min; then under the protection of nitrogen atmosphere, add antioxidant tetrakis [β-(3,5-di-tert-butyl-4-hydroxyphenyl)] pentaerythritol ester 0.3g, polycondensation catalyst cesium carbonate 0.8mg and end group 5.2g of hydroxyl-terminated polysiloxane, the vacuum degree was gradually adjusted to <100Pa, and the polycondensation reaction was carried out for 30 minutes; the...

Embodiment 3

[0044] Add 73.1g of bisphenol A, 92.5g of diphenyl carbonate, and 84.1g of bisphenol fluorene into the polymerization device, and raise the temperature to 180°C under the protection of a nitrogen atmosphere. After it is completely melted, add 2mg of the catalyst 4-dimethylaminopyridine, Under the vacuum of 2300Pa, the transesterification reaction was carried out for 60min; the temperature was raised to 220°C, the vacuum degree was adjusted to 1000Pa, and the prepolymerization reaction was carried out for 30min; then the antioxidant tetrakis[β-(3,5-di-tert-butyl -4-Hydroxyphenyl)] pentaerythritol ester 0.3g, polycondensation catalyst 0.8mg and end-group hydroxyl-terminated polysiloxane 6.9g, vacuum gradually adjusted to <100Pa, polycondensation reaction 30min; temperature rises to 280 ° C, continue React for 30 minutes. Finally, keep vacuuming and cool to room temperature to obtain copolycarbonate.

[0045] GPC test shows that the number average molecular weight of copolycarbo...

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Abstract

The low-smoke low-heat-release intrinsic flame-retardant polycarbonate is composed of structural units represented by I, II and III, the structural unit of II accounts for 1-99% of the mole number of the structural unit of [I], and [III] accounts for 0.5-20 wt% of the mass of [I + II]; the number-average molecular weight of the copolycarbonate is 12000-20000, the limit oxygen index of the copolycarbonate is 30.0-55.0%, and the vertical combustion grade of the copolycarbonate is V-0 grade; in the cone calorimetry test process, the peak heat release rate is 40%-90% lower than that of pure PC, and the total smoke release amount is 10%-90% lower than that of pure PC. The invention further discloses a preparation method of the copolycarbonate, the copolycarbonate has a good smoke heat release inhibiting effect and high char forming property, molten drops can be effectively inhibited, smoke heat release can be effectively reduced, the preparation process is environmentally friendly, and the obtained polymer has good injection molding processability, can be subjected to industrial production and is suitable for industrial production. And the flame retardant can also be used as a macromolecular flame retardant to be added into a polymer to realize flame retardance.

Description

technical field [0001] The invention belongs to the technical field of copolycarbonate and its preparation and application, and specifically relates to a class of intrinsically flame-retardant copolycarbonate with low-smoke and low-heat release characteristics and its preparation method and application. The copolycarbonate is an aromatic polycarbonate , by introducing a third monomer and modified polysiloxane to greatly improve the performance of aromatic polycarbonate in inhibiting smoke and heat release. Background technique [0002] Polycarbonate (PC) is a thermoplastic engineering plastic with excellent mechanical properties and heat resistance, widely used in aerospace, electronics, automobiles and machinery and other fields. [0003] Polycarbonate itself has a certain flame retardancy, the limiting oxygen index (LOI) is 24-26%, and the UL-94 test is V-2 level, with melting drops (ACS Appl. Nano Mater., 2019, 2, 4859-4868) . However, with the improvement of public saf...

Claims

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Application Information

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IPC IPC(8): C08G64/18C08G64/30C08G77/448C08L69/00C08L83/10
CPCC08G64/18C08G77/448C08G64/307C08L69/00C08L83/10C08L2201/02
Inventor 王玉忠肖翔心刘博文陈力陈梓浔王紫霓白彤予
Owner SICHUAN UNIV