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Cage-shaped oligomeric silsesquioxane modified flame-retardant vinyl ester resin composition and preparation method and application thereof

A technology of vinyl ester resin and sesquioxane, which is applied in the field of flame retardancy, can solve the problems of poor flame retardancy and large amount of reinforcing fiber, and achieve the effect of simple preparation method and strong operability

Inactive Publication Date: 2019-01-04
BEIJING INSTITUTE OF TECHNOLOGYGY
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the flame retardancy of pure vinyl ester resin is poor, and the oxygen index is only about 19%.
[0003] In the prior art, the Chinese patent publication No. CN103396657A discloses that a composite material is prepared by blending bisphthalonitrile resin with modified vinyl resin, and adding reinforcing fibers to the blended resin solution to prepare a barrier Combustible low-smoke vinyl resin composite material, but the amount of reinforcing fiber added is large, accounting for 55% to 75% of the total weight percentage; the Chinese patent with publication number CN105037642A provides a kind of plastic with good impact resistance and high temperature resistance Vinyl resin-based composite materials, but in order to ensure the compatibility of each additive with the resin base, it is necessary to add 4 to 8 parts of solubilizer, and there are many kinds of additives

Method used

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  • Cage-shaped oligomeric silsesquioxane modified flame-retardant vinyl ester resin composition and preparation method and application thereof
  • Cage-shaped oligomeric silsesquioxane modified flame-retardant vinyl ester resin composition and preparation method and application thereof
  • Cage-shaped oligomeric silsesquioxane modified flame-retardant vinyl ester resin composition and preparation method and application thereof

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preparation example Construction

[0086] The present invention also provides the preparation method of the clathrate oligomeric silsesquioxane modified flame retardant vinyl ester resin composition described in the above technical scheme, comprising the following steps:

[0087] Mix the vinyl ester resin, cage POSS and accelerator by weight fraction to obtain a vinyl ester resin system;

[0088] The vinyl ester resin system is mixed with a curing agent and cured to obtain a clathrate oligomeric silsesquioxane modified flame retardant vinyl ester resin composition.

[0089] In the present invention, the vinyl ester resin, cage POSS and accelerator are mixed according to the weight fraction to obtain the vinyl ester resin system. In the present invention, the mixing temperature is preferably 25-100°C.

[0090] After the vinyl ester resin system is obtained, the present invention mixes the vinyl ester resin system with a curing agent and then cures to obtain a cage-shaped oligomeric silsesquioxane modified flame...

Embodiment 1

[0097] Preparation of caged POSS

[0098] Under an air atmosphere, mix 28.42 g of 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide triethoxysilane, 2.38 g of vinyltriethoxysilane and 250 mL of methanol And fully stirred, 3mL of concentrated hydrochloric acid (mass fraction: 36.5%) was added dropwise, after the system was uniformly mixed, the temperature was raised to 70°C, 4mL of deionized water was added dropwise, and reacted for 24h. After the reaction, the product was slowly dropped into deionized water to precipitate according to the volume ratio of 1:11, filtered, washed and dried to obtain a white powder, which was dissolved in a sufficient amount of chloroform, and then mixed according to the volume ratio of 1 : 5 the mixed system is added in normal hexane, filter after sufficient precipitation, wash, dry, obtain the clathrate oligomeric silsesquioxane (cage POSS) that has phosphorus and double bond group simultaneously, denote as cage Oligomeric silsesquioxanes (1)....

Embodiment 2

[0109] Cage POSS preparation

[0110] Under an air atmosphere, mix 28.42 g of 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide triethoxysilane, 13.3 g of vinyltriethoxysilane and 300 mL of methanol And fully stirred, 3mL of concentrated hydrochloric acid (mass fraction: 36.5%) was added dropwise, after the system was uniformly mixed, the temperature was raised to 65°C, 6mL of deionized water was added dropwise, and reacted for 20h. After the reaction, the product was slowly dropped into deionized water for precipitation according to the volume ratio of 1:10, filtered, washed and dried to obtain a white powder, which was dissolved in a sufficient amount of chloroform, and then mixed according to the volume ratio of 1 : 6 mixed system is joined in normal hexane, filter after sufficient precipitation, wash, dry, obtain the clathrate oligomeric silsesquioxane (cage POSS) that has phosphorus and double bond group simultaneously, denote as cage Oligomeric silsesquioxanes (2). At...

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Abstract

The invention provides a cage-shaped oligomeric silsesquioxane modified flame-retardant vinyl ester resin composition, and belongs to the field of flame retardancy. Cage-shaped POSS is cage-shaped oligomeric silsesquioxane with a phosphorus-containing group and a double-bond-containing group, the ratio of the phosphorus-containing group to the double-bond-containing group in a flame retardant is adjusted, the type of the phosphorus-containing group and the type of the double-bond-containing group can also be adjusted, and a purpose of controlling phosphorus content and reaction group amount isachieved; and the double-bond group of the cage-shaped POSS can chemically react with various groups, the double-bond group and the corresponding group reaction can be regulated and controlled according to performance requirement of different polymer, and finally, multi-functionalization and high performance of the composition are realized finally; and meanwhile, by the silicon-phosphorus synergistic effect of polyorganosiloxane, the flame retardancy can be high at low content, the flame retardancy of the vinyl ester resin composition can be improved under the condition that the adding amountis quite small, and the cage-shaped POSS is compatible to the vinyl ester resin well.

Description

technical field [0001] The invention belongs to the technical field of flame retardancy, and in particular relates to a cage-shaped oligomeric silsesquioxane modified flame-retardant vinyl ester resin composition and a preparation method and application thereof. Background technique [0002] Vinyl ester resin is a kind of modified epoxy resin obtained by the reaction of bisphenol type or novolac type epoxy resin and methacrylic acid, also known as epoxy acrylic resin, which is a thermosetting resin. Vinyl ester resin has good curability and formability, high temperature resistance, acid and alkali corrosion resistance, and is often made into corrosion-resistant products, such as FRP tanks, pipes, towers and corrosion-resistant grids. However, the flame retardancy of pure vinyl ester resin is poor, and the oxygen index is only about 19%. [0003] In the prior art, the Chinese patent publication No. CN103396657A discloses that a composite material is prepared by blending bisp...

Claims

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Application Information

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IPC IPC(8): C08L63/10C08L83/08C08K5/14C08K5/098
CPCC08L63/10C08L2201/02C08L2201/22C08L83/08C08K5/14C08K5/098
Inventor 杨荣杰王小霞张文超何吉宇
Owner BEIJING INSTITUTE OF TECHNOLOGYGY
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