CN103496886B - A kind of preparation method of fire-retardant heat insulation matrix material - Google Patents
A kind of preparation method of fire-retardant heat insulation matrix material Download PDFInfo
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- CN103496886B CN103496886B CN201310353820.4A CN201310353820A CN103496886B CN 103496886 B CN103496886 B CN 103496886B CN 201310353820 A CN201310353820 A CN 201310353820A CN 103496886 B CN103496886 B CN 103496886B
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Abstract
The invention discloses a kind of preparation method of fire-retardant heat insulation matrix material, first polycrystalline mullite fibre is laid on clean sheet glass, then by silicon dioxide-poly-ether ether ketone-even dip-coating of triphenyl mixing solutions on polycrystalline mullite fibre, and pass above-mentioned mixing solutions gently with glass stick the mixed solution of ceramic fiber is fully flooded, then will be immersed in anhydrous ethanol solvent by the polycrystalline mullite fibre of silicon dioxide-poly-ether ether ketone-triphenyl mixing solutions dip treating, after 30 ~ 60s, it taken out from anhydrous ethanol solvent and use dry filter paper to remove residual alcohol solvent, finally be placed in baking oven dry, oven drying temperature is 100 ~ 105 DEG C, after 10h, it taken out from baking oven and naturally cool to room temperature, namely this fire-retardant heat insulation matrix material is obtained.Price of the present invention is low, and fire-protection rating is high, not easily the moisture absorption, moisture absorption and water suction, and deformation coefficient is little, and toughness is large, chemical-resistant reagent corrodibility, stability, resistance to elevated temperatures, fire line, eco-environmental prote are strong.
Description
Technical field
The present invention relates to the preparation method of fire-retardant heat insulation matrix material, more particularly, relate to a kind of preparation method building flame-retardant thermal insulation material.
Background technology
Along with China's sustained economic growth, urban-rural integration process constantly advance, buildings maximization, centralization, three-dimensional, structure are becomed privileged, the complicated trend of equipment is progressively formed.But domestic corresponding building thermal insulation material development is more delayed, current material can not meet market demands, body of wall thermal conductivity is high, heat-proof quality is poor, energy saving and fire line poor.
Greatly developing heat insulating material makes it meet structural thermal insulation power conservation requirement, makes great efforts to improve insulating efficiency, reduces production cost, has become the most important thing of industry, and the anti-flaming thermal-insulation performance that lagging material is excellent simultaneously receives publicity day by day.China's wall heat insulation material mainly contains plasterboard, gypsum hollow lath, Thistle board, gas concrete, holllow building block, hollow brick, has developed again multiple lightweight large panel structure material in recent years, as color steel foam battenboard, rock wool and glass clamp central layer etc.But these material prices are high, and fire-protection rating is poor, the easy moisture absorption, moisture absorption and water suction, more difficultly apply in engineering construction.Conventional wall inorganic lagging material has cement expanded perlite, air-mixed concrete pieces, slag, but these inorganic materials exist, and toughness is little, the defect of chemical-resistant reagent corrodibility difference; Body of wall organic insulation material has polystyrene, polyethylene, polyurethane foam, styrofoam, phenol formaldehyde foam etc., these organic insulation materials are lightweight, workability good, good effect of heat insulation, but it exists the shortcoming that deformation coefficient is large, poor stability, resistance to elevated temperatures are poor, fire resistance is poor, eco-environmental prote is poor.Thus, actively researching and developing good toughness, quality is light, physical and chemical performance is stablized, the novel inorganic-organic composite material of fire-retardant heat insulation excellent property, is the Important Action advancing the application of flame-retardant thermal insulation material through engineering approaches.
Polycrystalline mullite fibre is the outer novel Ultralight high-temperature refractory fiber of a kind of Now Domestic, and be the one in whole three dichlorine monoxides and silica-based ceramic fiber, use temperature, at 1500 ~ 1700 DEG C, exceeds vitreous state fiber 200 ~ 400 DEG C.Polycrystalline mullite fibre is a kind of environment-friendly materials, its shrinking percentage is low, high temperature oxidation resisting, physical and chemical performance stable, to environment and body harmless, have the excellent characteristic such as water-fast, antifreeze, fire-retardant, polycrystalline mullite fibre is used as Building class flame-retardant thermal insulation material and is subject to extensive concern simultaneously.Although polycrystalline mullite fibre has excellent fire-retardant heat insulation performance, its fiber is loose, so its tensile strength and flexural strength poor, then limit its application.Silicon-dioxide is a kind of stupalith of high comprehensive performance, its Heat stability is good, and chemical-resistant reagent corrodes.Polyether-ether-ketone is a kind of thermoplastic macromolecule material of excellent combination property, and its resistance toheat is good, stable chemical performance, resistance to conventional soda acid corrode, and its toughness is high, stretch-proof and bending, good mechanical performance.
Summary of the invention
Technical problem to be solved by this invention is, there is provided a kind of price low, fire-protection rating is high, the not easily moisture absorption, moisture absorption and water suction, deformation coefficient is little, and the preparation method of the fire-retardant heat insulation matrix material that toughness is large, chemical-resistant reagent corrodibility, stability, resistance to elevated temperatures, fire line, eco-environmental prote are strong.
The technical scheme that the present invention solves the employing of its technical problem is as described below: a kind of preparation method of fire-retardant heat insulation matrix material, it is characterized in that: first polycrystalline mullite fibre is laid on clean sheet glass, then by silicon dioxide-poly-ether ether ketone-even dip-coating of triphenyl mixing solutions on polycrystalline mullite fibre, and pass described mixing solutions gently with glass stick the mixed solution of ceramic fiber is fully flooded, then will be immersed in anhydrous ethanol solvent by the polycrystalline mullite fibre of silicon dioxide-poly-ether ether ketone-triphenyl mixing solutions dip treating, after 30 ~ 60s, it taken out from anhydrous ethanol solvent and use dry filter paper to remove residual alcohol solvent, finally be placed in baking oven dry, oven drying temperature is 100 ~ 105 DEG C, after 10h, it taken out from baking oven and naturally cool to room temperature, namely this fire-retardant heat insulation matrix material is obtained.
Described silicon dioxide-poly-ether ether ketone-triphenyl mixing solutions is made up of the chemical reagent of following mass ratio relation: N,N-dimethylacetamide: polyether-ether-ketone: triphenyl: polyvinylpyrrolidone: silicon dioxide powder=60: 4 ~ 7: 4: 0.4 ~ 0.6: 4 ~ 7.
The preparation method of described silicon dioxide-poly-ether ether ketone-triphenyl mixing solutions is: take quantitative each reagent first according to the above ratio, then by quantitative N, N-dimethylacetamide solvent is poured in beaker, and by N, N-dimethylacetamide solvent is heated to 80 ~ 90 DEG C, then add polyether-ether-ketone, magnetic agitation makes it fully dissolve; Triphenyl is added again after polyether-ether-ketone dissolves completely, magnetic agitation makes solution fully mix, again polyvinylpyrrolidone is joined afterwards in above-mentioned mixing solutions, magnetic agitation makes polyvinylpyrrolidonepowder powder dissolve, add from polyether-ether-ketone and start to add to polyvinylpyrrolidone and in consoluet whole process, the temperature of mixing solutions remains between 80 ~ 90 DEG C; In mixing solutions, SiO 2 powder is added again after polyvinylpyrrolidonepowder powder is dissolved completely, afterwards mixing solutions is cooled to room temperature, and ultrasonic vibration 10 ~ 15min, SiO 2 powder is fully disperseed in mixing solutions, obtain milky slurries, be silicon dioxide-poly-ether ether ketone-triphenyl mixing solutions.
The median size of described silicon dioxide powder is 1.5 μm.
The present invention adopts dip-coating and dipping technique, silicon dioxide powder and polyether-ether-ketone superpolymer and appropriate phosphorus flame retardant are filled in polycrystalline mullite fibre, make a kind of inorganic-organic composite material, it will have the excellent properties of silicon-dioxide, polyether-ether-ketone and polycrystalline mullite fibre material concurrently, will show excellent insulation and flame retardant properties.
According to above-mentioned the present invention, its beneficial effect is:
1, patent of the present invention has advantage simple, easy and simple to handle, with low cost;
2, the fire-retardant excellent thermal insulation performance of fire-retardant heat insulation matrix material prepared by the present invention is applied;
3, the fire-retardant heat insulation matrix material that prepared by application the present invention has good hardness and toughness.
Embodiment
Below in conjunction with embodiment, the present invention is further described:
A kind of preparation method of fire-retardant heat insulation matrix material, first the polycrystalline mullite fibre of 100mm × 50mm × 20mm is laid on clean sheet glass, then by silicon dioxide-poly-ether ether ketone-even dip-coating of triphenyl mixing solutions on polycrystalline mullite fibre, and pass above-mentioned mixing solutions gently with glass stick the mixed solution of ceramic fiber is fully flooded, then will be immersed in anhydrous ethanol solvent by the polycrystalline mullite fibre of silicon dioxide-poly-ether ether ketone-triphenyl mixing solutions dip treating, after 30 ~ 60s, it taken out from anhydrous ethanol solvent and use dry filter paper to remove residual alcohol solvent, finally be placed in baking oven dry, oven drying temperature is 100 ~ 105 DEG C, after 10h, it taken out from baking oven and naturally cool to room temperature, namely this fire-retardant heat insulation matrix material is obtained.
Described silicon dioxide-poly-ether ether ketone-triphenyl mixing solutions is made up of the chemical reagent of following mass ratio relation: N,N-dimethylacetamide: polyether-ether-ketone: triphenyl: polyvinylpyrrolidone: silicon dioxide powder=60:4 ~ 7:4:0.4 ~ 0.6:4 ~ 7.The median size of described silicon dioxide powder is 1.5 μm.
The preparation method of described silicon dioxide-poly-ether ether ketone-triphenyl mixing solutions is as the following example (taking quantitative each reagent according to the above ratio):
Embodiment one
Poured in beaker by the N,N-dimethylacetamide solvent of 120g, and by N,N-dimethylacetamide solvothermal to 80 ~ 90 DEG C, then add the polyether-ether-ketone of 10g, magnetic agitation makes it fully dissolve; 8g triphenyl is added again after polyether-ether-ketone dissolves completely, magnetic agitation makes solution fully mix, again the polyvinylpyrrolidone of 0.8g is joined in above-mentioned mixing solutions afterwards, magnetic agitation makes polyvinylpyrrolidonepowder powder dissolve, add from polyether-ether-ketone and start to add to polyvinylpyrrolidone and in consoluet whole process, the temperature of mixing solutions remains between 80 ~ 90 DEG C; In mixing solutions, 8g SiO 2 powder is added again after polyvinylpyrrolidonepowder powder is dissolved completely, afterwards mixing solutions is cooled to room temperature, and ultrasonic vibration 10min, SiO 2 powder is fully disperseed in mixing solutions, obtain milky slurries, be silicon dioxide-poly-ether ether ketone-triphenyl mixing solutions.
Embodiment two
Poured in beaker by the N,N-dimethylacetamide solvent of 120g, and by N,N-dimethylacetamide solvothermal to 80 ~ 90 DEG C, then add the polyether-ether-ketone of 12g, magnetic agitation makes it fully dissolve; 8g triphenyl is added again after polyether-ether-ketone dissolves completely, magnetic agitation makes solution fully mix, again the polyvinylpyrrolidone of 0.8g is joined in above-mentioned mixing solutions afterwards, magnetic agitation makes polyvinylpyrrolidonepowder powder dissolve, add from polyether-ether-ketone and start to add to polyvinylpyrrolidone and in consoluet whole process, the temperature of mixing solutions remains between 80 ~ 90 DEG C; In mixing solutions, 10g SiO 2 powder is added again after polyvinylpyrrolidonepowder powder is dissolved completely, afterwards mixing solutions is cooled to room temperature, and ultrasonic vibration 10min, SiO 2 powder is fully disperseed in mixing solutions, obtain milky slurries, be silicon dioxide-poly-ether ether ketone-triphenyl mixing solutions.
Embodiment three
Poured in beaker by the N,N-dimethylacetamide solvent of 120g, and by N,N-dimethylacetamide solvothermal to 80 ~ 90 DEG C, then add the polyether-ether-ketone of 14g, magnetic agitation makes it fully dissolve; 6g triphenyl is added again after polyether-ether-ketone dissolves completely, magnetic agitation makes solution fully mix, again the polyvinylpyrrolidone of 1.0g is joined in above-mentioned mixing solutions afterwards, magnetic agitation makes polyvinylpyrrolidonepowder powder dissolve, add from polyether-ether-ketone and start to add to polyvinylpyrrolidone and in consoluet whole process, the temperature of mixing solutions remains between 80 ~ 90 DEG C; In mixing solutions, 10g SiO 2 powder is added again after polyvinylpyrrolidonepowder powder is dissolved completely, afterwards mixing solutions is cooled to room temperature, and ultrasonic vibration 15min, SiO 2 powder is fully disperseed in mixing solutions, obtain milky slurries, be silicon dioxide-poly-ether ether ketone-triphenyl mixing solutions.
Embodiment 4
Poured in beaker by the N,N-dimethylacetamide solvent of 120g, and by N,N-dimethylacetamide solvothermal to 80 ~ 90 DEG C, then add the polyether-ether-ketone of 14g, magnetic agitation makes it fully dissolve; 8g triphenyl is added again after polyether-ether-ketone dissolves completely, magnetic agitation makes solution fully mix, again the polyvinylpyrrolidone of 1.2g is joined in above-mentioned mixing solutions afterwards, magnetic agitation makes polyvinylpyrrolidonepowder powder dissolve, add from polyether-ether-ketone and start to add to polyvinylpyrrolidone and in consoluet whole process, the temperature of mixing solutions remains between 80 ~ 90 DEG C; In mixing solutions, 13g SiO 2 powder is added again after polyvinylpyrrolidonepowder powder is dissolved completely, afterwards mixing solutions is cooled to room temperature, and ultrasonic vibration 15min, SiO 2 powder is fully disperseed in mixing solutions, obtain milky slurries, be silicon dioxide-poly-ether ether ketone-triphenyl mixing solutions.
Although the present invention describes with reference to above-mentioned embodiment particularly; but those of ordinary skill in the art very clearly can recognize that above embodiment is only for illustration of the present invention completely; wherein can make various changes and revise and not depart from the present invention in a broad sense; so not as limitation of the invention; as long as in spirit of the present invention, to the change of above-described embodiment all by fall into application claims protection domain within.
Claims (2)
1. a preparation method for fire-retardant heat insulation matrix material, is characterized in that:
First polycrystalline mullite fibre is laid on clean sheet glass, then by silicon dioxide-poly-ether ether ketone-even dip-coating of triphenyl mixing solutions on polycrystalline mullite fibre, and pass described mixing solutions gently with glass stick the mixed solution of ceramic fiber is fully flooded, then will be immersed in anhydrous ethanol solvent by the polycrystalline mullite fibre of silicon dioxide-poly-ether ether ketone-triphenyl mixing solutions dip treating, after 30 ~ 60s, it taken out from anhydrous ethanol solvent and use dry filter paper to remove residual alcohol solvent, finally be placed in baking oven dry, oven drying temperature is 100 ~ 105 DEG C, after 10h, it taken out from baking oven and naturally cool to room temperature, namely this fire-retardant heat insulation matrix material is obtained,
Described silicon dioxide-poly-ether ether ketone-triphenyl mixing solutions is made up of the chemical reagent of following mass ratio relation: N, N-N,N-DIMETHYLACETAMIDE: polyether-ether-ketone: triphenyl: polyvinylpyrrolidone: silicon dioxide powder=60: 4 ~ 7: 4: 0.4 ~ 0.6: 4 ~ 7
The preparation method of described silicon dioxide-poly-ether ether ketone-triphenyl mixing solutions is: take quantitative each reagent first according to the above ratio, then by quantitative N, N-dimethylacetamide solvent is poured in beaker, and by N, N-dimethylacetamide solvent is heated to 80 ~ 90 DEG C, then add polyether-ether-ketone, magnetic agitation makes it fully dissolve; Triphenyl is added again after polyether-ether-ketone dissolves completely, magnetic agitation makes solution fully mix, again polyvinylpyrrolidone is joined afterwards in above-mentioned mixing solutions, magnetic agitation makes polyvinylpyrrolidonepowder powder dissolve, add from polyether-ether-ketone and start to add to polyvinylpyrrolidone and in consoluet whole process, the temperature of mixing solutions remains between 80 ~ 90 DEG C; In mixing solutions, SiO 2 powder is added again after polyvinylpyrrolidonepowder powder is dissolved completely, afterwards mixing solutions is cooled to room temperature, and ultrasonic vibration 10 ~ 15min, SiO 2 powder is fully disperseed in mixing solutions, obtain milky slurries, be silicon dioxide-poly-ether ether ketone-triphenyl mixing solutions.
2. the preparation method of a kind of fire-retardant heat insulation matrix material according to claim 1, is characterized in that, the median size of described silicon dioxide powder is 1.5 μm.
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Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
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CN101353567A (en) * | 2007-07-24 | 2009-01-28 | 成都思摩纳米技术有限公司 | Heat insulation flame-retardant material |
CN101489656A (en) * | 2006-05-26 | 2009-07-22 | 宝柏氏公司 | Hot gas filtration fabrics with silica and flame resistant fibers |
CN101626894A (en) * | 2007-01-08 | 2010-01-13 | 尤尼弗瑞克斯I有限责任公司 | Fire-barrier film laminate |
CN102312404A (en) * | 2010-07-06 | 2012-01-11 | 上海杰事杰新材料(集团)股份有限公司 | Application of thermoplastic resin composite materials in preparing road reinforcing plate |
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Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN101489656A (en) * | 2006-05-26 | 2009-07-22 | 宝柏氏公司 | Hot gas filtration fabrics with silica and flame resistant fibers |
CN101626894A (en) * | 2007-01-08 | 2010-01-13 | 尤尼弗瑞克斯I有限责任公司 | Fire-barrier film laminate |
CN101353567A (en) * | 2007-07-24 | 2009-01-28 | 成都思摩纳米技术有限公司 | Heat insulation flame-retardant material |
CN102312404A (en) * | 2010-07-06 | 2012-01-11 | 上海杰事杰新材料(集团)股份有限公司 | Application of thermoplastic resin composite materials in preparing road reinforcing plate |
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