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Preparation method of modified expanded graphite grafted with silicon-phosphorous element

A technology of expanded graphite and modification, which is applied in the field of materials, can solve the problems of deterioration of mechanical properties of polymer materials, destruction of cell structure integrity, and influence of EG flame retardancy, etc., to improve interface compatibility and simple modification method Easy-to-use, easy-to-control effects

Inactive Publication Date: 2016-11-02
TONGJI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] However, as an inorganic flame retardant, EG has poor interfacial compatibility with the polymer matrix, which will destroy the integrity of the cell structure and lead to the deterioration of the mechanical properties of the polymer material; The layer is easy to fall off under the disturbance of flame impact, which seriously affects the flame retardant effect of EG

Method used

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  • Preparation method of modified expanded graphite grafted with silicon-phosphorous element
  • Preparation method of modified expanded graphite grafted with silicon-phosphorous element
  • Preparation method of modified expanded graphite grafted with silicon-phosphorous element

Examples

Experimental program
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Effect test

Embodiment 1

[0032] Step 1: Treatment of expanded graphite with silane coupling agent vinyltriethoxysilane (A-151)

[0033] Prepare 60mL of 90% ethanol aqueous solution, add dilute hydrochloric acid to adjust the pH to 5, then add 2gA-151, mechanically stir at 300r / min at 30°C for 20min, add 20g of expanded graphite with a size of 80 mesh, and heat up to 80°C. 400r / min mechanical stirring for 2 hours, so that the silicon hydroxyl group reacts with the hydroxyl group on the surface of the expanded graphite to form a C-O-Si bond. The reaction equation is as follows:

[0034]

[0035] Step 2: Treatment of A-151 Modified Expanded Graphite with Dilute Phosphoric Acid

[0036] Add 4g of dilute phosphoric acid with a mass fraction of 42.5% to the solution, keep it at 80°C, and stir it mechanically at 400r / min for 2 hours to make it react with silicon hydroxyl groups to form Si-O-P bonds. The reaction equation is as follows:

[0037]

[0038] Then, it was washed and filtered with absolute e...

Embodiment 2

[0041] Step 1: Treatment of expanded graphite with γ-aminopropyltriethoxysilane (KH-550)

[0042] Prepare 50mL of 90% ethanol aqueous solution, add acetic acid to adjust the pH to 5, then add 2g KH-550, stir mechanically at 300r / min at 30°C for 20min, then add 20g of expanded graphite with a size of 100 mesh, heat up to 60°C, 400r / min Mechanical stirring for 4 hours, so that the silicon hydroxyl group reacts with the hydroxyl group on the surface of the expanded graphite to form a C-O-Si bond;

[0043] Step 2: Treat KH-550 modified expanded graphite with dilute phosphoric acid

[0044] Add 4g of dilute phosphoric acid with a mass fraction of 25% to the solution, keep at 80°C, and mechanically stir at 400r / min for 4 hours, so that it can react with silicon hydroxyl groups to form Si-O-P bonds, then wash and filter with absolute ethanol for 5 times, at 80°C Dry in an oven for 12 hours to obtain modified expanded graphite grafted with Si and P elements.

[0045] Table 1 is the...

Embodiment 3

[0049] Same as Example 1, but the silane coupling agent is replaced by a mixture of 2g vinyltriethoxysilane (A-151) and KH560, the molar ratio of the two is 1:1, and other conditions remain unchanged.

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Abstract

The invention belongs to the field of materials technology and specifically relates to a preparation method of modified expanded graphite grafted with silicon-phosphorous element. The preparation method comprises the following specific steps: hydrolyzing by the use of a silane coupling agent in an organic solvent containing water so as to produce silicon hydroxyl; carrying out a dehydration-condensation reaction between silicon hydroxyl and hydroxyl or carboxyl functional group on the surface of EG so as to generate C-O-Si bond, adding phosphoric acid to carry out a reaction between phosphoric acid and silicon hydroxyl on the surface of EG so as to generate Si-O-P bond, washing with ethanol or water, filtering, and drying to obtain modified EG. Heat resistance of the product is obviously enhanced. As the surface of EG is grafted with organic matter, interfacial compatibility between the EG and a polymer matrix is improved, the EG has good dispersity in the polymer matrix. Thus, flame retardant property of the EG can be fully performed. The prepared modified EG can be applied to many polymer matrixes, thus realizing expanding polymer flame-retardant modification application.

Description

technical field [0001] The invention belongs to the technical field of materials, and in particular relates to a preparation method of modified expanded graphite grafted with silicon and phosphorus elements. Background technique [0002] With the wide application of polymer materials, people have higher and higher requirements for their flame retardancy. Flame retardants, as the most effective flame retardant modification additives, have developed into a wide variety of systems with various properties. According to the form of flame retardant in the polymer matrix, it can be divided into two types: additive type and reactive type. Among them, the additive flame retardant is only simply dispersed in the matrix, and does not chemically react with the matrix and other components during the flame retardant process; while the reactive flame retardant often participates in chemical reactions in the form of monomers or crosslinking agents, and eventually It exists in the polymer s...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08K9/06C08K9/04C08K7/24C09C1/46C09C3/12C09C3/06
CPCC08K9/06C01P2006/32C08K7/24C08K9/04C09C1/46C09C3/006C09C3/06C09C3/12
Inventor 刘琳马祥军
Owner TONGJI UNIV
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