Preparation method and application of inorganic hybrid flame retardant with high thermal stability

A technology with high thermal stability and flame retardant, applied in the direction of phosphorus oxyacid, hypophosphorous acid, etc., can solve the problems of difficult dispersibility, poor comprehensive flame retardant performance, etc., and achieve good comprehensive flame retardant performance and good comprehensive flame retardant performance. , the effect of high yield

Inactive Publication Date: 2015-09-02
HEBEI UNIVERSITY
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The purpose of the present invention is to provide a preparation method and application of a high thermal stability inorganic hybrid flame retardant, to develop a new inorganic hybrid flame retardant, to solve the problem that the existing inorganic flame retardants generally have poor comprehensive flame retardant properties. Poor, the problem that it is not easy to disperse when added in the polymer matrix

Method used

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  • Preparation method and application of inorganic hybrid flame retardant with high thermal stability
  • Preparation method and application of inorganic hybrid flame retardant with high thermal stability
  • Preparation method and application of inorganic hybrid flame retardant with high thermal stability

Examples

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Effect test

Embodiment 1

[0032] Dissolve 120mg of graphite oxide (GO) in 400mL of distilled water and ultrasonically disperse to obtain a concentration of 0.3mg·mL -1 Graphene oxide suspension; 4.83g AlCl 3 ·6H 2 O (0.02mol) was dissolved in the above 400mL graphene oxide suspension so that the concentration of aluminum salt was 50mmol L -1 , stirred at 25°C for 30min to obtain a mixed solution; add 6.36g of NaH to the above mixed solution 2 PO 2 ·H 2 O (0.06mol) to obtain a reaction solution; pour this reaction solution into a polytetrafluoroethylene reactor, transfer the reactor to an oven, set the reaction temperature to 180°C, and set the reaction time to 3h; the reaction is over Finally, the reaction solution was cooled to room temperature, subjected to suction filtration, water washing, and alcohol washing, and the obtained solid was put into a vacuum oven at a drying temperature of 50°C for 12 hours to obtain an inorganic hybrid flame retardant.

[0033] Taking Example 1 as an example, the...

Embodiment 2

[0035] Dissolve 200mg of graphite oxide (GO) in 400mL of distilled water and ultrasonically disperse to a concentration of 0.5mg·mL -1 Graphene oxide suspension; 26.66g Al 2 (SO 4 ) 3 18H 2 O (0.04mol) was dissolved in the above 400mL graphene oxide suspension so that the concentration of aluminum salt was 0.1mol L -1 , stirred at 25°C for 30min to obtain a mixed solution; add 12.72g of NaH to the above mixed solution 2 PO 2 ·H 2 O (0.12mol) to obtain a reaction solution, pour the reaction solution into a polytetrafluoroethylene reactor, transfer the reactor to an oven, set the reaction temperature to 180°C, and set the reaction time to 3h. After the reaction, the reaction solution was cooled to room temperature, filtered, washed with water, and washed with alcohol, and the obtained solid was put into a vacuum oven at a drying temperature of 50°C for 12 hours to obtain an inorganic hybrid flame retardant.

Embodiment 3

[0037] Dissolve 120mg of graphite oxide (GO) in 400mL of distilled water and ultrasonically disperse to obtain a concentration of 0.3mg·mL -1 Graphene oxide suspension; 30.01g Al(NO 3 ) 3 9H 2 O (0.08mol) was dissolved in the above 400mL graphene oxide suspension so that the concentration of aluminum salt was 0.2mol L -1 , stirred at 25°C for 30min to obtain a mixed solution; add 25.44g of NaH to the above mixed solution 2 PO 2 ·H 2 O (0.24mol) to obtain a reaction solution; pour this reaction solution into a polytetrafluoroethylene reactor, transfer the reactor to an oven, set the reaction temperature to 180°C, and set the reaction time to 3h; the reaction ends Finally, the reaction solution was cooled to room temperature, subjected to suction filtration, water washing, and alcohol washing, and the obtained solid was put into a vacuum oven at a drying temperature of 50°C for 12 hours to obtain an inorganic hybrid flame retardant.

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Abstract

The invention discloses a preparation method of an inorganic hybrid flame retardant with high thermal stability. The preparation method comprises the following steps: a), preparing oxidized graphene suspending liquid; b), adding soluble aluminium salt into the oxidized graphene suspending liquid, controlling the concentration of the soluble aluminium salt to be 50-400 mmol / L, uniformly stirring, adding soluble phosphinate at the temperature of 0-80 DEG C, and stirring, so as to obtain reaction liquid, wherein the molar ratio of the soluble aluminium salt to the soluble phosphinate is 1:(3-4); c), enabling the reaction liquid to be subjected to hydrothermal reaction for 3-12 h at the temperature of 170-190 DEG, and cooling, filtering, washing and drying the obtained product, so as to obtain the inorganic hybrid flame retardant with high thermal stability. In addition, the invention also discloses a PBT composite material comprising the flame retardant. The preparation method for the flame retardant, provided by the invention, is simple, mild in reaction condition, high in productivity and low in price, and facilitates large-scale production and control; an experiment result shows that the PBT composite material, prepared by adding the flame retardant into PBT, has the advantages of being high in limited oxygen index, good in anti-dripping effect, high in char forming property and thermal stability, good in heat insulation performance and the like; the comprehensive flame retardancy of the flame retardant is excellent.

Description

technical field [0001] The invention relates to the preparation and application of flame retardant materials, in particular to a preparation method and application of a highly thermally stable inorganic hybrid flame retardant. Background technique [0002] Inorganic flame retardants are currently the most widely used flame retardants. They have the advantages of being green, non-toxic, long-lasting, non-volatile, wide in source, low in price, and easy to prepare. Poor material compatibility and other shortcomings. Therefore, research and development of inorganic flame retardants with small additions, high flame retardant efficiency, and easy compatibility with polymer matrices are current research hotspots and difficulties in the industry. [0003] Hypophosphite flame retardant represented by aluminum hypophosphite (AHP) is an emerging inorganic phosphorus-containing flame retardant in recent years, and has attracted much attention due to its low cost and high efficiency. ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08K3/04C08K3/32C08K3/16C08K3/30C08K3/28C08L67/02C01B25/165
Inventor 屈红强齐艳侠刘晓威姜鑫鑫陈茜徐建中
Owner HEBEI UNIVERSITY
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