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Boron nitride comprising phosphonitrile structure and preparation method thereof

A hexagonal boron nitride and phosphazene-containing technology, which is applied in the treatment of dyed organic silicon compounds, dyed low-molecular organic compounds, and fibrous fillers, can solve the problems of flame retardancy and low thermal expansion coefficient, and achieve low thermal expansion coefficient, The effect of simple operation process and wide applicability

Active Publication Date: 2014-09-17
苏州法思特新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, based on hexagonal boron nitride and phosphazene, the development of new functional bodies with high flame retardancy, low thermal expansion coefficient and good interfacial force with resins has not been reported.

Method used

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  • Boron nitride comprising phosphonitrile structure and preparation method thereof
  • Boron nitride comprising phosphonitrile structure and preparation method thereof
  • Boron nitride comprising phosphonitrile structure and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] in N 2 Under protection, 150 g of toluene and 3 g of hexagonal boron nitride were mixed in 1# reactor to obtain a uniform suspension. Add 0.15g of γ-aminopropyltriethoxysilane into the reactor, and then reflux at 100°C for 8h. After the reaction, filter with suction, wash with toluene and absolute ethanol for 5 times, and dry to obtain hexagonal boron nitride treated by coupling.

[0025] In the 2# reactor, 3 g of coupling-treated hexagonal boron nitride and 150 g of tetrahydrofuran were mixed to obtain a uniform suspension. 24g triethylamine is added into 2# reactor, under N 2 Under atmosphere and cooling with ice water, the reactant was stirred for 1.5 h. Dissolve 9g of chlorophosphazene in 50g of tetrahydrofuran, slowly add to 2# reactor within 1h, heat the 2# reactor, and make the material in the reactor react at 75°C for 8h. After the reaction, wash with tetrahydrofuran and absolute ethanol three times respectively, filter, remove the solvent, excess chlorophos...

Embodiment 2

[0045] in N 2 Under protection, 200g of toluene and 10g of hexagonal boron nitride were mixed in 1# reactor to obtain a uniform suspension. Add 0.50g of γ-aminopropyltrimethoxysilane into the reactor, and then reflux at 110°C for 12 hours; after the reaction, filter with suction, wash with toluene and absolute ethanol three times respectively, and dry to obtain the coupling treatment of hexagonal boron nitride.

[0046] In the 2# reactor, 5 g of coupling-treated hexagonal boron nitride and 200 g of tetrahydrofuran were mixed to obtain a uniform suspension. 25g triethylamine is added into 2# reactor, under N 2 Stir under atmosphere and ice water conditions for 2h. Dissolve 10g of chlorophosphazene in 100g of xylene, slowly add to 2# reactor within 2h, and then heat the 2# reactor, so that the material in the reactor should be kept at 80°C for 12h. After the reaction, wash with tetrahydrofuran and absolute ethanol three times respectively, filter, remove the solvent, excess ...

Embodiment 3

[0049] in N 2 Under protection, 200g of toluene and 3g of hexagonal boron nitride were mixed in 1# reactor to obtain a uniform suspension. Add 0.50 g of γ-aminopropyltriethoxysilane to the reactor, and then reflux at 100° C. for 8 h. After the reaction, filter with suction, wash with toluene and absolute ethanol three times respectively, and dry to obtain hexagonal boron nitride treated by coupling.

[0050] In the 2# reactor, mix 3g of coupling-treated hexagonal boron nitride with 100g of xylene and 50g of benzene to obtain a uniform suspension. 15g triethylamine is added into 2# reactor, under N 2 Under atmosphere and cooling with ice water, the reactant was stirred for 0.5h. Dissolve 8g of chlorophosphazene in a mixed solution of 25g of benzene and 50g of xylene, slowly add it to 2# reactor within 1.5h, then heat the 2# reactor, and make the material in the reactor react at 75°C for 8h. After the reaction, filter with suction, wash with benzene and absolute ethanol thre...

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Abstract

The invention discloses boron nitride comprising a phosphonitrile structure and a preparation method thereof. The preparation method comprises the following steps: uniformly mixing boron nitride and toluene and adding a silane coupling agent to obtain coupled boron nitride; mixing the coupled boron nitride into a solvent and adding a catalyst to obtain a mixture; dissolving phosphonitrilic chloride into a solvent of tetrahydrofuran and the like, slowly adding the obtained product into the mixture so as to obtain boron nitride subjected to phosphonitrilic chloride treatment; and after mixing reagents such as a solvent, p-phenylenediamine and the like and the boron nitride subjected to phosphonitrilic chloride treatment, adding a catalyst to obtain the boron nitride comprising the phosphonitrile structure. The boron nitride comprising the phosphonitrile structure is a functional body capable of simultaneously having high flame retardance of organic resin and low coefficient of thermal expansion, comprises a great amount of active reaction groups and has wide application prospect on the aspects of development of a novel high polymer material, modification of a polymer, high performance, multifunctionality and the like. The boron nitride comprising the phosphonitrile structure also has the characteristics of wide applicability of the preparation method and simple operation process and is easy for industrialization.

Description

technical field [0001] The invention relates to a modification technology for hexagonal boron nitride, in particular to boron nitride containing a phosphazene structure and a preparation method thereof. Background technique [0002] In recent years, with the rapid development of the electronic information industry, the demand for polymer materials with both low thermal expansion coefficient and high flame retardancy has surged. In the face of this demand, two problems stand out. First of all, polymer materials themselves often do not have good low thermal expansion coefficient and high flame retardancy; secondly, a lot of research and development work is carried out for a single performance (low thermal expansion coefficient or high flame retardancy). The research and development of high flame retardancy is rarely reported. [0003] Studies have shown that adding flame retardants or inorganic fillers with low thermal expansion coefficients to polymers is an effective way t...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C09C1/00C09C3/08C09C3/12C08K9/04C08K3/38
Inventor 梁国正金文琴顾嫒娟袁莉
Owner 苏州法思特新材料有限公司