Flame-retardant modified silane coupling agent and preparation method thereof

A silane coupling agent and modification technology, applied in the field of flame retardants, can solve problems such as human hazards, achieve moderate reaction temperature, mild reaction conditions, and improve compatibility

Inactive Publication Date: 2014-02-12
JIANGHAN UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] In order to solve the problem that the synthetic raw materials of the silane coupling agent in the prior art are harmful to the human body, the embodiment of the present invention provides a flame-retardant modified silane coupling agent and its preparation method

Method used

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  • Flame-retardant modified silane coupling agent and preparation method thereof
  • Flame-retardant modified silane coupling agent and preparation method thereof
  • Flame-retardant modified silane coupling agent and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0040]Put 50g of 2-methyl-2,5-dioxo-1,2-oxaphospholane (OP) and 200ml of n-heptane into a 250ml three-necked flask, which is equipped with a reflux condenser and a stirrer and a constant pressure dropping funnel, then add 5ml of triethylamine, raise the temperature to 95°C, add 80g of 3-aminopropyltriethoxysilane (KH550) into the constant pressure dropping funnel and slowly drop it while stirring, and react for 4h . The reaction mixture was taken out and left to cool, and the mother liquor was separated with a separatory funnel to obtain a viscous product in the lower layer, which was dried in a vacuum oven at 100°C for about 3 hours to obtain the final product, which was specifically γ-(3-(formazan Hydroxyphosphono)-propionamido)propyl triethoxysilane, R in this product is γ-(3-(methylhydroxyphosphono)-propionamido)propyl, that is, alkylene, referred to as P -KH550.

[0041] Use attenuated total reflection (Attenuated Total Reflection, ATR) to conduct infrared analysis on t...

Embodiment 2

[0044] Weigh 100 parts by mass of silicon dioxide (purity 99.0%, particle size 4.9 μm), 8 parts by mass of P-KH550 provided in Example 1 of the present invention, add them to 500 mL of ethanol, where ethanol is a dispersant, and then add 2 parts by mass Glacial acetic acid, dispersed under 700W ultrasonic conditions for 20min, and then refluxed at 80°C for 2h under the condition of strong stirring, after 2h, suction filtration and drying to obtain P-KH550 modified SiO 2 ; Replace P-KH550 with KH550, repeat the above experimental steps to obtain KH550 modified SiO 2 .

[0045] SiO without any treatment 2 , KH550 modified SiO 2 and P-KH550 modified SiO 2 Add 15 parts by mass to three epoxy resins (EP) of 100 parts by mass, and carry out the following experiments respectively. After dispersing and mixing with 700W ultrasonic waves at 90°C for 30 minutes, add 25 parts by mass of diaminodiphenylmethane to form Curing system, the system is cured under the process conditions of 1...

Embodiment 3

[0047] Add 50g of 2-methyl-2,5-dioxo-1,2-oxaphospholane and 120ml of cyclohexane into a 250ml three-necked flask equipped with a reflux condenser, a stirrer and a constant pressure dropping funnel , then add 10ml of tri-n-propylamine, raise the temperature to 20°C, add 97g of N-(2-aminoethyl)-3-aminopropyltriethoxysilane (KH7910) into the constant pressure dropping funnel and drop it slowly, at the same time Stirring, reaction 24h. The reaction mixture was taken out and left to cool, and the mother liquor was separated with a separatory funnel to obtain a viscous product in the lower layer, which was dried in a vacuum oven at 100°C for about 3 hours to obtain the final product, specifically N-(2-aminoethyl base)-3-(methylhydroxyphosphono)propionamido)propyltriethoxysilane (R in this product is N-(2-aminoethyl)-3-(methylhydroxyphosphono)propionamide Base) propyl, that is, R is a secondary aminoalkylene). It is called P-KH791 for short.

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Abstract

The invention discloses a flame-retardant modified silane coupling agent and a preparation method thereof, and belongs to the field of fire retardants. The molecular structural formula of the flame-retardant modified silane coupling agent is as follows: R is alkylidene and alkane arylene or secondary amino group alkylidene, and x is alkoxy. The preparation method comprises the following steps of: (1) adding 2-methyl-2.5-dioxy-1.2-dioxaphospholane and an organic solvent to a reactor, then adding a catalyst, uniformly stirring, and dropping amino siloxane to react at the temperature of 20-120 DEG C for the time of 4-24 hours to obtain reaction liquid; (2) separating the reaction liquid obtained from the step (1) by using a separating funnel to obtain a sticky matter, then removing the solvent of the sticky matter, and carrying out vacuum drying for 3 hours to finally obtain the flame-retardant modified silane coupling agent which contains phosphorus and nitrogen. The flame-retardant modified silane coupling agent disclosed by the invention has better flame-retardant effect.

Description

technical field [0001] The invention relates to the field of flame retardants, in particular to a flame retardant modified silane coupling agent and a preparation method thereof. Background technique [0002] The silane coupling agent is obtained by addition of silicon chloroform (HSiCl3) and unsaturated olefins with reactive groups under the catalysis of platinum chloride acid, followed by alcoholysis. Silane coupling agents are flammable, and there are great safety hazards in the application process. Therefore, it is of great significance to modify the flame retardant of silane coupling agent. [0003] In the existing experiments on flame retardant modification of silane coupling agents, phosphorus and nitrogen elements are introduced into the molecules of silane coupling agents. Specifically, dichloromethane is used as a solvent, and some polyhydric alcohols or polyphenols are used as a reaction substrate, and a phosphorus compound containing an active reactive group is...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F7/18C08K5/5455
Inventor 刘继延刘学清陈佳
Owner JIANGHAN UNIVERSITY
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