Phosphorus-contained organic silicon resin fire retardant and preparation method thereof
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A technology of silicone and flame retardant
Inactive Publication Date: 2010-03-17
QINGDAO UNIV OF SCI & TECH +1
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However, since the three elements of the commonly used intumescent flame retardant system come from different compounds, in the process of processing, when various additives are blended with most polymers, there are disadvantages such as poor dispersion, poor compatibi
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Embodiment 1
[0043] (a) A 500ml three-neck flask is equipped with a stirrer, a thermometer, and a spherical condenser, weighs 1.0 moles of pentaerythritol and 3.5 moles of phosphorus oxychloride, stirs and mixes, controls the reaction temperature at 20°C, and absorbs the gas in the reaction with an alkaline solution The product was reacted for 6 hours until no gas was released, and a precipitated substance was obtained from the reaction. Cool, filter, wash with chloroform solvent, remove unreacted substances, and dry under vacuum at 80°C to finally obtain a white solid powder which is chlorinated spirocyclic phosphate. attached figure 1 It is the infrared spectrum of chlorinated spirocyclic phosphate: 1308cm -1 It is the characteristic absorption peak of P=O, 1016cm -1 Stretching vibration absorption for P-O-C
[0044] (b) Equip a 500ml four-necked flask with a stirrer, a thermometer, a spherical condenser and a 100ml constant pressure funnel, add 500mL of deionized water, and prepare t...
Embodiment 2
[0047] (a) Weigh 1.0 moles of polyol and 3.5 moles of phosphorus oxychloride, stir and mix, control the reaction temperature at 20°C, absorb the gas products in the reaction with alkaline solution, react for 6 hours, until no gas is released, and the reaction is precipitated substance. Cool, filter, wash with solvents such as chloroform, remove unreacted substances, and dry in vacuum to finally obtain a white solid powder which is chlorinated spirocyclic phosphate.
[0048] (b) A 500ml four-neck flask is equipped with a stirrer, a thermometer, a spherical condenser and a 100ml constant pressure funnel, and 250mL of deionized water is added to react the monomers aminopropylmethyldimethoxysilane and phenyltrimethoxysilane , dimethyldiethoxysilane, and methyltriethoxysilane were respectively added to the constant pressure funnel, the reaction temperature was controlled at 40°C, and the reaction monomer was added dropwise at an even speed. After the dropwise addition, continued hy...
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Abstract
The invention provides a phosphorus-contained organic silicon resin fire retardant shown as a following formula and a preparation method thereof. The preparation method of the phosphorus-contained organic silicon resin fire retardant comprises the following steps: firstly, adopting polyalcohol and phosphorus oxychloride as raw materials to prepare chlorinated volution phosphoester; then carrying out hydrolytic condensation on amino-containing silane, dialkoxy silane and trialkoxysilane to obtain amino-containing organic silicon resin; finally dissolving the amino-containing organic silicon resin into a methylbenzene solvent, an N,N-dimethyl fomamide solvent or an acetonitrile solvent, and the like, and adding the chlorinated volution phosphoester and an acid-binding agent for synthesis to obtain the phosphorus-containing organic silicon resin fire retardant. The phosphorus-containing organic silicon resin fire retardant can be used as a fire retardant for polyolefin, makrolan, ABS, nylon and PC/ABS, has high efficiency and low toxicity compared with the traditional fire retardant and is an environmental protection type fire retardant for plastics. R1, R2, R3 and R4 are respectively selected from CH3 or C6H5, R5 is selected from CH2 or CH2CH2 or CH2CH2NHCH2CH2, and R6 is selected from the CH3 or C2H5; n is equal to integers of 1 subtracting 50, P is equal to integers of 1 subtracting 50, and q is equal to integers of 1 subtracting 50.
Description
Technical field: [0001] The invention relates to the technical field of flame retardant synthesis, in particular to a phosphorus-containing organosilicon resin used for flame retardancy and a preparation method thereof. Background technique: [0002] Flame retardants widely used in plastics, fibers, coatings, etc. can generally be divided into two categories: halogen-containing and halogen-free flame retardants, among which phosphorus-nitrogen-containing intumescent flame retardants are widely used, The effect is good, and it is in line with the sustainable development strategy of environmental protection. [0003] Intumescent flame retardant systems usually contain three elements: carbon source, acid source and gas source. That is to say, the intumescent flame retardant is composed of three additives containing a certain functional group, which have the advantages of low smoke, non-toxicity, and high resistance to flames. However, since the three elements of the commonly ...
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