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Preparation and application of zno@mof@polyphosphazene flame retardant

A technology of flame retardant and flame retardant performance, which is applied in the field of flame retardant preparation, can solve the problems of low thermal stability, low smoke generation, influence on mechanical properties of polyurea, inability to meet requirements, etc. Synergistic, evenly distributed effect

Active Publication Date: 2022-05-06
QINGDAO TECHNOLOGICAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, if the nitrogen-based flame retardant is added to polyurea alone, as the amount of addition increases, although the flame retardant performance can be improved, it will also be accompanied by a decline in mechanical properties.
Invention patent application 201711385243.1 discloses "a halogen-free flame retardant and flame-retardant polyurea elastomer coating". The flame retardant forms a carbonized layer after burning to prevent the substrate from continuing to burn. However, in the polyurea elastomer coating, the flame retardant is added in an amount of 10-30 parts, which is a large amount, which will have a certain impact on the mechanical properties of polyurea
Today, as the world pays more and more attention to environmental protection, this kind of flame retardant can no longer meet the demand

Method used

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  • Preparation and application of zno@mof@polyphosphazene flame retardant
  • Preparation and application of zno@mof@polyphosphazene flame retardant
  • Preparation and application of zno@mof@polyphosphazene flame retardant

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] ZnO@MOF@polyphosphazene flame retardant for polyurea is prepared by the following method:

[0029] (1) Preparation of ZnO@MOF nanoparticles: disperse cobalt nitrate and dimethylimidazole in DMF aqueous solution, and magnetically stir until uniformly dispersed; add ZnO powder to it, ultrasonically disperse evenly, and then transfer to an autoclave for solvothermal reaction Return to room temperature after the reaction is completed, freeze-dry after washing to obtain ZnO@MOF nanoparticles. Wherein, the mass concentration of the DMF aqueous solution is 700g / L; the mass ratio of the cobalt nitrate and dimethylimidazole in DMF is 1:20, and the concentration of ZnO in DMF is 10g / L, and the magnetic stirring The speed is 300rpm; the temperature condition of the solvothermal reaction is 50°C, and the reaction time is 3h; the temperature condition of the freeze-drying is -50°C.

[0030](2) Preparation of ZnO@MOF@polyphosphazene: First, hexachlorocyclotriphosphazene was dissolve...

Embodiment 2

[0033] Embodiment 2: Different from Embodiment 1,

[0034] ZnO@MOF@polyphosphazene flame retardant for polyurea is prepared by the following method:

[0035] (1) Preparation of ZnO@MOF nanoparticles: the mass concentration of the DMF aqueous solution is 780g / L; the ratio of cobalt nitrate and dimethylimidazole in DMF is 1:23, and the concentration of ZnO in DMF is 16g / L, the speed of the magnetic stirring is 350rpm; the temperature condition of the solvothermal reaction is 60°C, and the reaction time is 2h; the temperature condition of the freeze-drying is -53°C.

[0036] (2) Preparation of ZnO@MOF@polyphosphazene: Firstly, hexachlorocyclotriphosphazene was dissolved in tetrahydrofuran to obtain hexachlorocyclotriphosphazene solution; ZnO@MOF nanoparticles were dispersed in the aforementioned solvent by ultrasonic to obtain a suspension liquid. 4,4'-diaminodiphenyl sulfone and triethylamine were respectively added to the suspension; then the hexachlorocyclotriphosphazene so...

Embodiment 3

[0039] Embodiment 3: Different from Embodiment 1,

[0040] ZnO@MOF@polyphosphazene flame retardant for polyurea is prepared by the following method:

[0041] (1) Preparation of ZnO@MOF nanoparticles: the mass concentration of the DMF aqueous solution is 820g / L; the ratio of cobalt nitrate and dimethylimidazole in DMF is 1:25, and the concentration of ZnO in DMF is 12g / L, the speed of the magnetic stirring is 450rpm; the temperature condition of the solvothermal reaction is 55°C, and the reaction time is 2.5h; the temperature condition of the freeze-drying is -63°C.

[0042] (2) Preparation of ZnO@MOF@polyphosphazene: firstly, hexachlorocyclotriphosphazene was dissolved in acetonitrile to obtain hexachlorocyclotriphosphazene solution; ZnO@MOF nanoparticles were dispersed in the aforementioned solvent by ultrasound to obtain a suspension liquid. 4,4'-diaminodiphenyl ether and triethylamine were respectively added to the suspension; then the hexachlorocyclotriphosphazene solut...

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Abstract

The invention provides a ZnO@MOF@polyphosphazene flame retardant for polyurea materials. Add ZnO@MOF@polyphosphazene flame retardant to the mixture of amino-terminated polyether and amine chain extender, ultrasonically disperse it evenly, and then add isocyanate prepolymer to the system for reaction to obtain a flame retardant with excellent flame retardant properties. polyurea material. The ZnO@MOF@polyphosphazene flame retardant contains amino groups, which can participate in the reaction of polyurea; therefore, on the one hand, it improves the dispersion of nanoparticles in polyurea, making their distribution more uniform, and on the other hand, it also It is ensured that the flame retardant will not precipitate or volatilize over time, so as to achieve the improvement of flame retardant performance under the premise of ensuring mechanical properties. In addition, the three components in the ZnO@MOF@polyphosphazene flame retardant have a good synergistic effect in combustion, greatly improving its flame retardant effect, which is of great importance to the industrial development of polyurea materials. significance.

Description

technical field [0001] The invention belongs to the technical field of organic polymer flame retardants, and in particular relates to a method for preparing a flame retardant for reactive polyurea. Background technique [0002] Polyurea is an elastomer material produced by the reaction of isocyanate and amino compound. It has high stability, is not sensitive to environmental humidity, and has excellent corrosion resistance. Due to its excellent performance, polyurea is widely used in many fields such as concrete protection, steel structure anticorrosion, and roof waterproofing. However, polyurea is a polymer material, which is flammable and has certain safety hazards during use. To solve this problem, it is necessary to add flame retardant components to polyurea materials. [0003] In the prior art, common flame retardants are mainly halogen-based flame retardants, phosphorus-based flame retardants and nitrogen-based flame retardants. Among them, halogenated flame retarda...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08L75/02C08L85/02C08L87/00C08K3/22
CPCC08L75/02C08L2201/02C08K2003/2296C08L85/02C08L87/00C08K3/22
Inventor 马明亮王荣珍刘燕燕黄微波
Owner QINGDAO TECHNOLOGICAL UNIVERSITY