Solid superacid, preparation method thereof and flame-retardant epoxy resin

A technology of solid superacid and epoxy resin, which is applied in the field of flame-retardant epoxy resin, and can solve problems such as difficult to meet requirements

Active Publication Date: 2020-11-27
NORTH CHINA INST OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although this method improves the flame retardant effect of epoxy resin to a certain extent, with the development of flame retardant materials, the requirements for flame retardant effect are getting higher and higher, and the above method has been difficult to meet the requirements

Method used

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  • Solid superacid, preparation method thereof and flame-retardant epoxy resin
  • Solid superacid, preparation method thereof and flame-retardant epoxy resin
  • Solid superacid, preparation method thereof and flame-retardant epoxy resin

Examples

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preparation example Construction

[0048] The present invention also provides the preparation method of the solid superacid described in the technical scheme, comprising the steps of:

[0049] (1) Mix organic titanium salt, glacial acetic acid and absolute ethanol to obtain the first mixed solution;

[0050] (2) mixing the first mixed solution obtained in the step (1) with a dispersant to obtain a second mixed solution;

[0051] (3) adding the aqueous solution of the water-soluble salt of M dropwise to the second mixed solution obtained in the step (2), and performing hydrolysis to obtain a sol; the M is Cu, Zr, Fe, Mn or Mo;

[0052] (4) aging and filtering the sol obtained in the step (3) in sequence to obtain a hybrid material;

[0053] (5) mixing the hybrid material obtained in the step (4) with the phosphoethanol solution to obtain a precursor solution;

[0054] (6) Filtering and calcining the precursor solution obtained in the step (5) in sequence to obtain a solid superacid.

[0055] The invention mix...

Embodiment 1

[0087] (1) Mix butyl titanate, glacial acetic acid and absolute ethanol to obtain a first mixed solution; wherein the ratio of the amounts of butyl titanate, glacial acetic acid and absolute ethanol is 1:2:17;

[0088] (2) Stir and mix the first mixed solution obtained in the step (1) with polyvinylpyrrolidone in a water bath at 60° C. for 2 hours to obtain a second mixed solution; wherein, the mass fraction of polyvinylpyrrolidone in the second mixed solution is 3 %;

[0089] (3) Add the aqueous solution of iron sulfate to the second mixed solution obtained in the step (2) dropwise at a rate of 2 mL / s, and hydrolyze it for 4 hours while stirring at 60° C. to obtain a sol; wherein, the aqueous solution of iron sulfate The ratio of the amount of metal ions to the amount of butyl titanate in the second mixed solution is 1:1;

[0090] (4) Put the sol obtained in the step (3) to stand and age for more than 12 hours, stratification occurs, filter, and dry in a vacuum oven at 100°C...

Embodiment 2

[0094] (1) Mix butyl titanate, glacial acetic acid and absolute ethanol to obtain a first mixed solution; wherein the ratio of the amounts of butyl titanate, glacial acetic acid and absolute ethanol is 1:2:17;

[0095] (2) Stir and mix the first mixed solution obtained in the step (1) with polyvinylpyrrolidone in a water bath at 60° C. for 2 hours to obtain a second mixed solution; wherein, the mass fraction of polyvinylpyrrolidone in the second mixed solution is 3 %;

[0096] (3) Add the aqueous solution of zirconium sulfate dropwise to the second mixed solution obtained in the step (2) at a rate of 2 mL / s, and hydrolyze it for 4 hours while stirring at 60° C. to obtain a sol; wherein, the aqueous solution of zirconium sulfate The ratio of the amount of metal ions to the amount of butyl titanate in the second mixed solution is 1:1;

[0097] (4) Put the sol obtained in the step (3) to stand and age for more than 12 hours, stratification occurs, filter, and dry in a vacuum ove...

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Abstract

The invention provides a solid superacid. The solid superacid is PO4 <3-> / TiO2-MXOY, and M in the PO4 <3-> / TiO2-MXOY is Cu, Zr, Fe, Mn or Mo. According to the solid superacid provided by the invention, phosphate radicals are loaded on a bimetallic oxide carrier; by adopting phosphate radicals, the growth of a bimetallic oxide crystal phase can be inhibited; the particle size of the solid superacidis further refined; specific surface area is increased, and the catalytic action on esterification and dehydration reactions is further improved; in the material pyrolysis process, the cross-linkingcarbonization of the material can be promoted through the strong catalysis effect on esterification and dehydration reactions, generation of combustible gas in the pyrolysis process is reduced, so that a compact carbon layer is formed, the purpose of improving the flame retardant property of the material is achieved, the phosphorus element with excellent flame retardant property is added into thesolid superacid, and the flame retardant property of the material is further improved.

Description

technical field [0001] The invention relates to the technical field of flame-retardant epoxy resin, in particular to a solid superacid, a preparation method thereof, and a flame-retardant epoxy resin. Background technique [0002] Flame retardant epoxy resin, also known as self-extinguishing epoxy resin, contains flame retardant groups or is mixed with flame retardants in the resin, and there are two types: reactive type and additive type. The former method is a resin containing a flame retardant group made from a halogen-containing monomer, and the latter method is to add a flame retardant to the epoxy resin to obtain a flame retardant cured product. The resin prepared by the former method is a halogen-containing resin, which will produce a large amount of toxic and corrosive smoke when burned, which seriously pollutes the environment, so the latter method is usually used. [0003] The flame retardants added to epoxy resin are divided into inorganic flame retardants, organ...

Claims

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Application Information

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IPC IPC(8): C08L63/00C08K3/32C08K9/12
CPCC08K3/32C08K9/12C08K2201/005C08K2003/329C08K2003/323C08L2201/02C08L63/00
Inventor 高明万梅岳丽娜
Owner NORTH CHINA INST OF SCI & TECH
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