Silicious expanding fire retardant and its prepn process

A technology of intumescent flame retardant and silane, applied in the field of silicon-containing intumescent flame retardant and its preparation, can solve the problems of application limitation of intumescent flame retardant, easy water absorption of phosphate compounds, etc., and achieve good flame retardant performance, heat Good stability and not easy to absorb water

Inactive Publication Date: 2007-06-06
凌庆平
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Traditional intumescent flame retardants generally use phosphate compounds as the acid source, the most commonly used is ammonium polyphosphate, but phosphate compounds are easy to absorb water, which limits the application of intumescent flame retardants

Method used

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  • Silicious expanding fire retardant and its prepn process
  • Silicious expanding fire retardant and its prepn process
  • Silicious expanding fire retardant and its prepn process

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] A. Add 21.6g (0.1mol) of 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide and 7.2g (0.1mol) of acrylic acid into a three-necked flask, stir and heat to dissolve , control the temperature to 80°C, and reflux for 6 hours to obtain a light yellow and transparent mixed product; separate the mixed product by precipitation, dissolve the mixed product with 100ml acetone, add 1000ml chloroform as a precipitant, and filter to obtain a white solid product. Vacuum-dried in a vacuum oven at 80°C for 2 hours to obtain 10.8 g (0.004 mol) of the product 10-propionic acid-9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide. Fig. 1 is the infrared spectrogram of this product: FTIR (KBr, cm -1 ): 2800-3000 (-CH 2 ,-CH 3 ), 1729 (C=O), 1200 (C-O), 922 (P-O-Ph), 1595 (P-Ph).

[0037] B. Weigh the amino-containing silane (R 1 for (CH 2 ) 3 NH(CH 2 ) 2 , R 2 for CH 3 O) 20.6g (0.1mol), add 3.6g (0.2mol) of water, 0.1g (0.002mol) of potassium hydroxide, heat up to 80°C, under the p...

Embodiment 2

[0041] A. Add 21.6g (0.1mol) of 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide and 7.2g (0.1mol) of acrylic acid into a three-necked flask, stir and heat to dissolve , control the temperature at 70°C, reflux for 8 hours to obtain a light yellow and transparent mixed product; separate the mixed product by precipitation, dissolve the mixed product with 80ml acetone, add 800ml chloroform as a precipitant, filter to obtain a white solid product, and vacuum Vacuum-dry in an oven at 80°C for 2 hours to obtain 10.5 g (0.004 mol) of the product 10-propionic acid-9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide.

[0042] B. Weigh the amino-containing silane (R 1 for (CH 2 ) 3 , R 2 for CH 3 O) 19.1g (0.1mol), add 3.6g (0.2mol) of water, 0.5g (0.01mol) of potassium hydroxide, heat up to 100°C, under the protection of nitrogen, keep the temperature constant for 12 hours, remove the water, and obtain amino-containing silane 17.4 g (0.02 mol) of the hydrolyzed product.

[0043]...

Embodiment 3

[0046] Silicon-containing intumescent flame retardant 19.5g and polycarbonate (PC) 31.85g obtained according to the method for embodiment 1, acrylonitrile-butadiene-styrene terpolymer (ABS) 13.65g in internal mixer Mix uniformly, the mixing temperature is 220° C., and the mixing time is 5 minutes to obtain a flame-retardant PC / ABS alloy. Its oxygen index is 27.0 (PC / ABS alloy oxygen index is 21.0), and at 800 ° C, a higher carbon formation rate (13.2% in nitrogen, 9.9% in air, and PC / ABS without flame retardant alloys were 8.2% and 0), in addition to effectively reducing the heat release rate of PC / ABS alloy combustion (from 252.39kW / m 2 down to 152.64kW / m 2 ).

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Abstract

The present invention discloses silicious expanding fire retardant in the structure as shown and its preparation process. Being superior to traditional fire retardant, which contains halogen and hydroscopic, the silicious expanding fire retardant has three essentials as expanding fire retardant, and 9, 10-dihydro-9-oxo-10-phospha phenanthryl-10-oxide without phosphate ester structure as acid source, and possesses excellent fire retarding performance.

Description

Technical field: [0001] The invention relates to a flame retardant and a preparation method thereof, in particular to a silicon-containing expansion flame retardant and a preparation method thereof. Background technique: [0002] Flame retardants can be divided into halogenated flame retardants and halogen-free flame retardants. As people's awareness of environmental protection continues to increase, halogen-free flame retardants have become an inevitable trend in the development of flame retardants. Halogen-free flame retardants generally include: aluminum hydroxide, magnesium hydroxide, phosphorus-based flame retardants, nitrogen-containing flame retardants, and silicone flame retardants. [0003] With the continuous advancement of flame retardant technology, flame retardant compounds containing a single element are increasingly unable to meet the application requirements. The development of flame retardant compounds has gradually focused on compounds that use multiple fla...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09K21/14C08G77/50C08G77/395
Inventor 吴丹韦平江平开仲含芳李强
Owner 凌庆平
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