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Flame-retardant epoxy resin based on iron-containing nickel silicate and preparation method of flame-retardant epoxy resin

A technology of epoxy resin and nickel silicate, which is applied in the field of halogen-free flame-retardant epoxy resin, can solve the problems of reduced bending strength and fracture strain, reduced other properties of the epoxy matrix, and failure to meet high flame-retardant requirements. Improvement of combustion effect, improvement of vertical combustion performance, and excellent smoke suppression effect

Active Publication Date: 2020-05-15
ANHUI UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

According to "Materials & Design" (Materials & Design 178 (15), 107834, 2019), when the montmorillonite accounts for 2% of the total mass percentage of the system and the nanocomposite flame retardant accounts for 8% of the total system mass, although the prepared The oxygen index of flame-retardant epoxy resin is 11.1% higher than that of pure epoxy resin, but the prepared flame-retardant epoxy resin still cannot meet the high flame-retardant requirements, and compared with pure epoxy resin, the bending Strength and strain at break are also reduced
According to "Journal of Fire Sciences" (Journal of Fire Sciences 34 (3): 212-225, 2016), when adding 10% ammonium polyphosphate-montmorillonite nanocomposites by mass percentage, although it can improve the epoxy resin Flame retardancy, but the other properties of the epoxy matrix are affected due to the large amount of flame retardant required
[0003] In order to solve the problem of easy dripping and high flammability of epoxy resin, the method of adding nitrogen-containing and phosphorus flame retardants to the epoxy matrix is ​​often used. Although this can better improve the flame retardant performance of epoxy resin, but Due to the large amount of flame retardant added, other properties of the epoxy matrix are correspondingly reduced, and the production cost is high

Method used

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  • Flame-retardant epoxy resin based on iron-containing nickel silicate and preparation method of flame-retardant epoxy resin
  • Flame-retardant epoxy resin based on iron-containing nickel silicate and preparation method of flame-retardant epoxy resin

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preparation example Construction

[0032] The specific preparation method of the silicon source is: NH with a volume ratio of 1 to 4:80:30 3 ·H 2 O, C 2 h 5 OH and deionized water to form a solution, and slowly add silane compound and C with volume ratio of 1 to 4:80 under stirring 2 h 5 The mixed solution made of OH is continuously stirred for 6-12 hours to fully hydrolyze the silane compound, then the product is centrifuged, washed with ethanol and dried to obtain the silicon source.

[0033] The silane compound is one or more of TMOS, TEOS, KH550, KH560, KH570.

[0034] Nickel source is NiCl 2 , Ni(NO 3 ) 2 , Ni(CH 3 COO) 2 one or more of.

[0035] The preparation method of the flame-retardant epoxy resin based on iron-containing nickel silicate in the present invention comprises the following steps:

[0036] (1) Mix the silicon source and deionized water with a mass ratio of 0.02-0.09:20, and ultrasonicate to a uniform suspension to obtain a silicon source solution; mix the nickel source and NH w...

Embodiment 1

[0041] A preparation method based on iron-containing nickel silicate flame retardant epoxy resin, comprising the following steps:

[0042] (1) First mix 30mL deionized water, 80mL absolute ethanol and 2mL NH 3 ·H 2 O mixed and stirred, then slowly drop the mixture of 1mL TEOS, 1mL KH550 and 80mL absolute ethanol into the above alkaline solution, the dropping speed is as slow as possible. After stirring for 12 hours, the white turbid liquid was centrifuged, washed with ethanol, and dried in an oven at 80°C for 12 hours to obtain white SiO 2 microsphere powder.

[0043] Then 0.05g SiO 2 Mix microsphere powder with 20mL deionized water and sonicate for 30 minutes to obtain SiO 2 solution; another 1mLNH 3 ·H 2 O, 30mL deionized water, 0.18g NiCl 2 ·6H 2 O, 0.53g NH 4 After Cl was made into a solution, it was mixed with SiO 2 The solutions were mixed and poured into a polytetrafluoroethylene-lined stainless steel reactor for hydrothermal reaction at a reaction temperature...

Embodiment 2

[0049] A preparation method based on iron-containing nickel silicate flame retardant epoxy resin, comprising the following steps:

[0050] Iron-containing nickel silicate was prepared according to the method described in Example 1. Stir 30g of E-51 epoxy resin in an oil bath at 70°C, and at the same time add 0.9g of iron-containing nickel silicate into 30mL of acetone, sonicate for 30 minutes and pour into E-51 epoxy resin, and continue stirring for 2 hours. In addition, 7.74g of 4,4'-diaminodiphenylmethane was melted at 100°C and added to the mixture of iron-containing nickel silicate and E-51, stirred vigorously for 5 minutes, then placed in a vacuum oven, and poured into the Put it into the mold, then put it into an oven to cure, cure at 100°C for 2 hours, and continue to cure at 150°C for 2 hours to obtain a halogen-free flame-retardant epoxy resin containing iron-nickel silicate.

[0051] According to the standard ASTM D 2863-2017a, a standard sample of 127mm×6.5mm×3.2mm...

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Abstract

The invention provides flame-retardant epoxy resin based on iron-containing nickel silicate and a preparation method of the flame-retardant epoxy resin, and belongs to the technical field of halogen-free flame-retardant epoxy resin; the flame-retardant epoxy resin contains 93-99.9% by mass of epoxy resin and 0.1-7% by mass of iron-containing nickel silicate; the epoxy resin is composed of an epoxyresin monomer and a curing agent, the mass percentage of the epoxy resin monomer is 70-80%, and the mass percentage of the epoxy curing agent is 20-30%. According to the invention, the addition amount of a flame retardant is reduced as much as possible to weaken adverse effects caused by introduction of the flame retardant into the epoxy resin while efficient flame retardance, no dripping and lowsmoke effect are ensured, and the production cost is reduced.

Description

technical field [0001] The invention belongs to the technical field of halogen-free flame-retardant epoxy resin, and in particular relates to a flame-retardant epoxy resin based on iron-containing nickel silicate and a preparation method thereof. Background technique [0002] Epoxy resin, as one of the traditional thermosetting plastics, is widely used in chemical, construction, electrical, Transportation, aerospace, military and other fields. However, epoxy resin is extremely flammable, and its limiting oxygen index is only about 21%, which seriously limits its application in fields with high flame retardancy requirements. Generally, the flame retardancy of epoxy resin is improved by adding phosphorus, nitrogen, silicon, boron and other halogen-free flame retardants. In addition, layered silicates such as montmorillonite have also been reported to be used to prepare flame-retardant epoxy resins. According to "Materials & Design" (Materials & Design 178 (15), 107834, 2019...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08L63/02C08K3/34C08K3/28
CPCC08K3/34C08K3/28C08L2201/02C08L2201/22C08L63/00C08K5/0025C08K5/17C09K21/02
Inventor 聂士斌金蝶杨继年徐煜轩杨威
Owner ANHUI UNIV OF SCI & TECH
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