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A kind of flame-retardant epoxy resin based on iron-containing nickel silicate and preparation method thereof

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: 2022-06-28
ANHUI UNIV OF SCI & TECH
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Problems solved by technology

According to "Materials & Design" (Materials & Design 178 (15), 107834, 2019), when the montmorillonite accounted for 2% of the total mass percentage of the system and the nanocomposite flame retardant accounted for 8% of the total system mass percentage, 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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  • A kind of flame-retardant epoxy resin based on iron-containing nickel silicate and preparation method thereof

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preparation example Construction

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

[0033] The silane compound is one or more of TMOS, TEOS, KH550, KH560, and 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 a silicon source with a mass ratio of 0.02 to 0.09:20 and deionized water, and ultrasonicate to a uniform suspension to obtain a silicon source solution; mix a nickel source w...

Embodiment 1

[0040] A preparation method of a flame-retardant epoxy resin based on iron-containing nickel silicate, comprising the following steps:

[0041] (1) First mix 30 mL of deionized water, 80 mL of absolute ethanol and 2 mL of NH 3 ·H 2 Mix and stir, and then slowly add the mixture of 1 mL of TEOS, 1 mL of KH550 and 80 mL of anhydrous ethanol into the above alkaline solution, and the drop rate 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.

[0042] Then 0.05g of SiO 2 The microsphere powder was mixed with 20 mL of deionized water and sonicated for 30 minutes to obtain SiO 2 solution; another 1 mL of NH 3 ·H 2 O, 30mL deionized water, 0.18g NiCl 2 ·6H 2 O, 0.53g NH 4 After Cl is made into a solution, it is then mixed with SiO 2 The solution was mixed and poured into a polytetrafluoroethylene-lined stainless steel reaction k...

Embodiment 2

[0048] A preparation method of a flame-retardant epoxy resin based on iron-containing nickel silicate, comprising the following steps:

[0049] Iron-containing nickel silicate was prepared according to the method described in Example 1. 30 g of E-51 epoxy resin was stirred in an oil bath at 70 °C, and 0.9 g of iron-containing nickel silicate was added to 30 mL of acetone. After sonication for 30 minutes, it was poured into E-51 epoxy resin, and the stirring was continued 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, placed in a vacuum oven, and poured into a vacuum oven after removing air bubbles. The mold is then put into an oven to be cured, cured at 100° C. for 2 hours, and further cured at 150° C. for 2 hours to obtain a halogen-free flame retardant epoxy resin containing iron nickel silicate.

[0050] According to the standard ASTM ...

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Abstract

The invention provides a flame-retardant epoxy resin based on iron-containing nickel silicate and a preparation method thereof, which belongs to the technical field of halogen-free flame-retardant epoxy resin. Oxygen resin and 0.1-7% iron-containing nickel silicate; the epoxy resin is composed of epoxy resin monomer and curing agent, the epoxy resin monomer mass percentage is 70-80%, the epoxy curing agent mass percentage The percentage is 20-30%; while ensuring high-efficiency flame retardant, drip-free and low-smoke effects, the present invention minimizes the amount of flame retardant added to weaken the adverse effects of introducing flame retardants into epoxy resin , and reduce production costs.

Description

technical field [0001] The invention belongs to the technical field of halogen-free flame retardant epoxy resin, and particularly relates to a flame retardant epoxy resin based on iron-containing nickel silicate and a preparation method thereof. Background technique [0002] As one of the traditional thermosetting plastics, epoxy resin is widely used in chemical, architectural, electrical, Transportation, aerospace, military and other fields. However, epoxy resin is extremely flammable, and the limiting oxygen index is only about 21%, which severely limits its application in the field of high flame retardancy. Generally, the flame retardancy of epoxy resin is improved by adding halogen-free flame retardants such as phosphorus, nitrogen, silicon, boron, etc. 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), when mont...

Claims

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Application Information

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Patent Type & Authority Patents(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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