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Phosphaphenanthrene group modified zirconium phosphate-based flame retardant and preparation method thereof

A technology of phosphaphenanthrene group and zirconium phosphate, which is applied in the field of flame retardants based on phosphaphenanthrene group modified zirconium phosphate and its preparation, can solve the problem of poor carbon quality, low flame retardant efficiency, and loose carbon layer strength. Low problems, to achieve the effect of taking into account chemical stability, high flame retardant efficiency, and a wide range of applications

Inactive Publication Date: 2020-03-20
WUHAN INSTITUTE OF TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] The main purpose of the present invention is to provide a flame retardant based on phosphaphenanthrene group-modified zirconium phosphate to solve the problems of poor char formation quality, low loose strength of charcoal layer and low flame retardant efficiency of existing flame retardants. The exfoliated zirconium phosphate nanosheets were modified with formaldehyde and DOPO to synthesize a flame retardant based on phosphaphenanthrene group-modified zirconium phosphate, and the silane coupling agent was used to graft benzaldehyde to make the flame retardant molecule have P-O-C-N flame retardant synergistic effect ; This flame retardant integrates flame retardant and smoke suppression and enhanced functions, and has low cost, good halogen-free char formation, environmental protection and wide applicability. At the same time, the preparation method involved is simple and suitable for popularization and application

Method used

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  • Phosphaphenanthrene group modified zirconium phosphate-based flame retardant and preparation method thereof
  • Phosphaphenanthrene group modified zirconium phosphate-based flame retardant and preparation method thereof
  • Phosphaphenanthrene group modified zirconium phosphate-based flame retardant and preparation method thereof

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Embodiment 1

[0040] A flame retardant based on phosphaphenanthrene group-modified zirconium phosphate, the synthetic route involved is shown in figure 1 , the specific preparation method comprises the following steps:

[0041] 1) TBA exfoliation of zirconium phosphate: in a 500ml four-neck flask, 3.00g of zirconium phosphate and 300ml of deionized water were fully dispersed by mechanical stirring and ultrasonication. TBA (tetrabutylammonium hydroxide aqueous solution, 25wt%) was added dropwise in the four-necked flask at a constant speed within 30min, and continued to react for 2h after the dripping, and then the 4mol / L concentrated phosphoric acid of 15ml was added dropwise at a constant speed in the flask within 30min. After the reaction (2h), the mixed solution was centrifuged for solid-liquid separation to obtain a translucent gel precipitate and washed with dioxane;

[0042] 2) Grafted silane coupling agent KH550: Add the translucent gel washed in step 1) into a four-necked flask, an...

Embodiment 2

[0047] A kind of flame retardant based on phosphaphenanthrene group modified zirconium phosphate, its preparation method comprises the steps:

[0048] 1) TBA exfoliation of zirconium phosphate: In a 500ml four-necked flask, 6.00ml of zirconium phosphate and 300ml of deionized water were fully dispersed by mechanical stirring and ultrasonication. The process lasted for 30min and kept at a temperature of 5°C. Tetrabutylammonium hydroxide 25wt% aqueous solution), in 30min, be added dropwise in the four-necked flask at a constant speed, continue to react for 2h after dropping, then the 4mol / L concentrated phosphoric acid of 15ml is added dropwise in the flask at a constant speed in 30min, after the reaction finishes, The mixed solution is subjected to solid-liquid separation by centrifugation, and a translucent gel precipitate is obtained and washed with dioxane;

[0049] 2) Grafted silane coupling agent KH550: Add the washed translucent gel into a four-neck flask, add 4.43g KH550...

Embodiment 3

[0052] A kind of flame retardant based on phosphaphenanthrene group modified zirconium phosphate, its preparation method comprises the steps:

[0053] 1) TBA exfoliation of zirconium phosphate: In a 500ml four-necked flask, 1.00g of zirconium phosphate and 150ml of deionized water were fully dispersed by mechanical stirring and ultrasonication. The process lasted for 30min and kept at a temperature of 5°C. (Tetrabutylammonium hydroxide 25wt% aqueous solution), was added dropwise at a constant speed in the four-necked flask within 30min, and continued to react for 2h after the dripping, and then 15ml of 4mol / L concentrated phosphoric acid was added dropwise at a constant speed of 30min in the flask. (2h), the mixed solution is subjected to solid-liquid separation by centrifugation, and a translucent gel precipitate is obtained and washed with dioxane;

[0054] 2) Grafted silane coupling agent KH550: Add the washed translucent gel into a four-necked flask, add 0.74g KH550 and 15...

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Abstract

The invention discloses a flame retardant based on phosphaphenanthrene group modified zirconium phosphate. According to the invention, tetrabutylammonium hydroxide and phosphoric acid are used for stripping zirconium phosphate to expose hydroxyl groups among zirconium phosphate layers, then a silane coupling agent is used for grafting zirconium phosphate, and benzaldehyde and DOPO are used for modifying stripped zirconium phosphate nanosheets. In the obtained flame retardant, the zirconium phosphate plays a flame retardant role on a substrate, realizes rapid carbon formation on the surface ofthe substrate so as to fill in gaps among sheet layers and form a large number of micro-nano carbon cages, and seals a large number of substrate degradation products in the micro-nano carbon cages forsufficient catalysis and carbonization via the zirconium phosphate in a high-temperature oxygen-deficient environment; meanwhile, free radicals of DOPO can be captured and take action in microscopiccarbon cages, so the flame-retardant effect is achieved on a microstructure level. The obtained flame retardant integrates the functions of flame retardance, smoke suppression and enhancement, and isfree of halogen, low in cost, good in char forming property, friendly to environment and wide in applicability; and a preparation method of the flame retardant is simple in process and suitable for application and promotion.

Description

technical field [0001] The invention belongs to the technical field of new flame-retardant and smoke-suppressing additives, and relates to a novel flame-retardant and smoke-suppressing additive of organic and inorganic hybridization, and in particular to a flame retardant based on phosphaphenanthrene group-modified zirconium phosphate and its preparation method. Background technique [0002] Polymer / layered nano-inorganic composite materials have structures that conventional composite materials do not have (such as layered adjustable structures, etc.) and have more excellent properties, which have attracted more and more attention of researchers in recent years. Among them, inorganic nano-powder modified polymers are used in the largest amount, which is currently a hot spot in the field of new materials. The special structure of nanomaterials determines special properties (such as small size effect, macroscopic tunnel effect, etc.), and can provide a good method to improve ...

Claims

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Application Information

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IPC IPC(8): C09D5/18C09D133/04C09D7/61
CPCC08K2003/2241C08K2003/323C08K2003/328C08L2201/02C09D5/185C09D133/04C09D7/61C08L1/284C08K13/06C08K9/06C08K9/04C08K3/32C08K5/053C08K5/34922C08K3/22
Inventor 刘治田王成张旗
Owner WUHAN INSTITUTE OF TECHNOLOGY
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