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High-temperature-resistant nuclear-shell structure type flame retardant, and preparation method and application thereof
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A core-shell structure, high temperature resistant technology, applied in the field of materials to achieve the effects of good compatibility, high flame retardant efficiency, and increased reaction area
Inactive Publication Date: 2012-05-02
GUANGZHOU CHEM CO LTD CHINESE ACADEMY OF SCI
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However, Song et al found (Song L, Wu K, Wang Y, Wang ZZ, Hu Y. Flammability and Thermo-oxidative Decomposition of Epoxy Resin Containing Ammonium Polyphosphate and Metallic Oxide. J. Macromol. Sci. Part A-Pure Appl. Chem .2009; 46: 290-295), because the molecular structure of epoxy resin contain
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Embodiment 1
[0042] (1) Preparation of polymethylphenylsiloxane modified epoxy resin: In a four-necked round-bottomed flask equipped with a mechanical stirrer, a thermometer, an addition funnel, and a reflux condenser, add 70 grams of bisphenol A type epoxy Resin E-44, after heating and thinning, add 30 grams of polymethylphenylsiloxane (DowCorning, DC3074) and 0.15 grams of tetraisopropyl titanate, and heat up to 130 ° C for 4 hours to obtain polymethylphenyl Silicone modified epoxy resin.
[0043](2) Preparation of flame retardant: 80 grams of ammonium polyphosphate (APP) was mechanically stirred and uniformly dispersed in 200 ml of absolute ethanol solution. Add 20 grams of the polymethylphenylsiloxane-modified epoxy resin prepared in step (1) at 25°C, and slowly raise the temperature (the heating rate is 3°C / min), and slowly add it dropwise (30 minutes) to dissolve Ethanol solution (20ml ) (curing agent consumption is 0.38 times of epoxy resin quality, is about to dissolve the curing...
Embodiment 2
[0046] (1) Preparation of polymethylphenylsiloxane modified epoxy resin: same as step (1) of Example 1.
[0047] (2) Preparation of flame retardant: same as Example 1 step (2), but with xylene as the dispersion system, and in the process of microencapsulation, add dropwise the xylene solution (20ml) that has dissolved the equivalent m-phenylenediamine .
[0048] The solubility of the obtained product at 25°C is 0.06g / 100mlH 2 O. The flame retardant composite material was prepared by blending the flame retardant with the addition amount of 30% by mass with polypropylene, and the oxygen index was 27.5%. And after immersing the composite material in hot water at 50°C for 24 hours, the oxygen index of the material is 26.5%.
Embodiment 3
[0050] (1) Preparation of polymethylphenylsiloxane modified epoxy resin: same as step (1) of Example 1.
[0051] (2) Preparation of flame retardant: same as step (2) of embodiment 1, but the quality of APP is 60 grams.
[0052] The solubility of the obtained product at 25°C is 0.05g / 100mlH 2 O. The flame retardant composite material was prepared by blending the flame retardant with the addition amount of 30% by mass with polypropylene, and the oxygen index was 26.5%. And after soaking the composite material in hot water at 50°C for 24 hours, the oxygen index of the material is 25.5%.
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Abstract
The invention discloses a high-temperature-resistant nuclear-shell structure type flame retardant, and a preparation method and an application thereof. The flame retardant takes polymethyl-phenyl siloxane modified epoxy resin as a capsule material and takes ammonium polyphosphate as a capsule core. The preparation method comprises the following steps of: mixing bisphenol A-type epoxy resin, polymethyl-phenyl siloxane and a catalyst, reacting for 3-5 hours at the temperature of 120-140 DEG C and obtaining the polymethyl-phenyl siloxane modified epoxy resin; then suspending ammonium polyphosphate powdery particles in a dispersing agent, adding the polymethyl-phenyl siloxane modified epoxy resin and a curing agent, stirring and reacting for 1-4 hours at the temperature of 60-100 DEG C, after the reaction is finished, stirring, reducing the temperature, suction filtering, drying and obtaining the high-temperature-resistant nuclear-shell structure type flame retardant. Compared with the traditional IFR (intumescent flame retardant) system, the flame retardant has better performances such as compatibility, flame retardance and water resistance; simultaneously the capsule material and the capsule core have the flame-retardant synergistic effect; and since the reaction area is increased, compared with the uncovered complex flame-retardant system, the microencapsulated expansion type flame retardant has higher flame-retardant efficiency.
Description
technical field [0001] The invention relates to the field of materials, in particular to a high-temperature-resistant core-shell structure flame retardant and its preparation method and application. Background technique [0002] Halogenated flame retardants have excellent flame retardancy, processability and compatibility, good weather resistance, and chemical stability, but they will produce a lot of smoke, corrosive gases, and some toxic substances during thermal decomposition and combustion, seriously endanger human health and pollute the environment. Therefore, halogenated flame retardants are gradually being replaced by halogen-free green flame retardants. Intumescent Flame Retardant (IFR for short) is a kind of flame retardant with carbon, nitrogen and phosphorus as the core components. Because of its halogen-free, low-smoke, low-toxicity and other characteristics, it meets the current requirements for protecting the ecological environment. , is one of the more activ...
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