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Phosphoric acid ester flame retardant for unsaturated resin
2017-12-2 11:56:36
Phosphoric acid ester flame retardant for unsaturated resin
Based on polyvinyl alcohol and phosphoric acid as raw materials, the phosphate ester flame retardant used for unsaturated resin was synthesized, and the synthesis process was optimized: m (H3PO4) /m (PVA) =2. 0, catalyst CO (NH2) 21%, 100 C, 120min. Infrared spectroscopy (FT-IR), nuclear magnetic resonance (NMR) and elemental analysis were used to characterize the structure of the unsaturated resin flame retardant.
The thermal properties of it were analyzed by TGA-DSC. The results show that the synthetic route of the unsaturated resin with phosphate ester flame retardant is simple and the flame retardancy is excellent.
Polymer materials are widely used, but the flammability of many organic polymer materials will cause fire hazards. Therefore, all countries in the world are working to develop a variety of flame retardants and flame retardant materials. Phosphorus flame retardant has the characteristics of high flame retardancy, low smoke, low toxicity and non corrosive gas, and its flame retardant effect is related to the phosphorus content of the flame retardant.
Phosphorus flame retardants, especially organophosphorus flame retardants, play an important role in all kinds of flame retardants. The small molecule phosphorus containing flame retardant has the disadvantages of high volatility, easy migration, poor heat resistance and poor mechanical properties of materials, which affects the flame retardance effect and limits its application. Most organic polymers containing phosphorus flame retardants have many advantages such as low smoke, low toxicity, good thermal stability, good flame retardancy, good compatibility with polymer substrates, migration resistance, volatilization resistance and durable flame retardancy. They have become the research focus of flame retardants.
PVA is very conducive to the intramolecular dehydration to produce olefins and aromatic rings at high temperature. Therefore, PVA is a good carbon forming agent in intumescent flame retardant. In this paper, PVA and phosphoric acid as raw material and urea as catalyst, synthesis of unsaturated resin based phosphate flame retardant (PVA-POH), the reaction conditions are studied, through infrared spectroscopy (FT-IR), nuclear magnetic resonance (NMR) and elemental analysis. Its structure, analysis of the thermal performance of TGA-DSC.
Reagents: polyvinyl alcohol (PVA) 20-99 (industrial pure), phosphoric acid, urea, anhydrous ethanol (all analytically pure), osmosis agent JFC
The synthesis of flame retardant PVA-POH: add 5gPVA 250mL three mouth bottle, add 20mL distilled water wetting stirring 15min, then add 10~30mL85% of phosphoric acid, stirring at room temperature after 30min, slowly heated to PVA completely dissolved into a colorless and transparent solution, then adding a certain amount of urea as catalyst, stirring, heating to proper temperature reaction time get, white or pale yellow transparent solution; adding 50mL ethanol precipitation, dissolution and precipitation repeated 3 times, decompression after filtration, vacuum oven drying at 60 DEG 24h, white or pale yellow product PVA-POH.
Tris(2-chloroisopropyl)Phosphate(TCPP)
Cas No:13674 -84-5
HS Code HS: 29199000
The most important indicator of product:
colorless transparent liquid, moisture ≤ 0.1, Acid value ≤ 0.1, Chroma ≤ 50, the phosphorus content: 9.4 ± 0.5
Raw materials: phosphorus oxychloride and epichlorohydrin.
Belong to several categories of dangerous goods:
Currently Tris(2-chloroisopropyl)Phosphate TCPP general cargo exports are not dangerous.
The product is used for the soft / hard polyurethane foam, with thermal and hydrolytic stability good, especially suitable for ASTME84 (Level 11) foam, with low viscosity unsaturated polyester resin in low temperature application and phenolic plastics at. This product is also used to grab the foam sealant and sheet production. For polyvinyl chloride, polystyrene, phenolic resin, acrylic resin and rubber, coating, flame retardant, also used for soft and hard polyurethane foam, epoxy resin, polystyrene, cellulose acetate, ethyl cellulose tree and phenolic plastics, polyvinyl acetate and gun type foam sealant production. Particularly recommended for rigid polyurethane foam has excellent thermal and hydrolytic stability is particularly suitable for ASTM84 (II), compound for polyurethane foam and unsaturated resin and phenolic plastics.
PVA-POH texture characterization: infrared spectroscopy (FT-IR): NicoletFT-IR6700 type infrared spectrometer, KBr pellet; nuclear magnetic resonance (NMR): VarianunityInova-400 NMR test 1H-, 31P-, 13C-NMR spectrum, DMSO-d6 as solvent, the internal standard was four methyl silane (TMS); element analysis (EA): CarloErba1106CHN element analyzer (Italy) C, H, O determination of content; phosphorus content with vanadium ammonium molybdate colorimetric method (GB/T6437-2002) determination.
Flame-retardant finishing process: two immersion two rolling (flame retardant PVA-POH300g/L, urea 100g/L, phosphoric acid 15g/L, penetrant JFC10g/L, rolling rate 70%~80%) to pre drying (90 degrees, 5min) to baking (165 C, 3min) to soap wash, water wash and drying.
Thermal analysis (TGA-DSC): using the synchronous thermal analyzer STA449CJupiter (Germany NETZSCH), the nitrogen flow rate is 45mL/min, and the 5~7mg sample is called to the aluminum crucible, and the temperature rises from 10 to 40 degrees to 590 degrees.
With the increase of the amount of phosphoric acid, the phosphorus content increased obviously, but when m (H3PO4) /m (PVA) >2. At 0, the degree of increase slowed down; >2. After 25, the yield decreased, probably because the higher the amount of phosphoric acid, the more intramolecular dehydration at the time of reaction. And the higher the amount of phosphoric acid, the color of the flame retardant gradually changed from white to yellowish, so its application range was limited. Select m (H3PO4) /m (PVA) =2. 0 is better.
With the increase of reaction temperature, the yield and phosphorus content increased first and then decreased, and the color of the products gradually deepened. The yield and phosphorus content were higher at 100 DEG, 105 DEG C yield and phosphorus content reached the maximum, and then continue to heat the reaction product appears black, dehydration obviously, phosphorus content and yield were significantly decreased. In consideration of energy, the optimum reaction temperature is 100.
With the prolongation of reaction time, the yield and phosphorus content increased. The yield of 120min was higher and the color of flame retardant was white. After 125min, the yield decreased. It may be that the reaction time is too long, resulting in dehydration and carbonization of products, resulting in the color of products. Consider the color of the flame retardant and choose 120min.
Copyright: Zhang Jia Gang YaRui Chemical co.,Ltd
http://www.yaruichem.com
Based on polyvinyl alcohol and phosphoric acid as raw materials, the phosphate ester flame retardant used for unsaturated resin was synthesized, and the synthesis process was optimized: m (H3PO4) /m (PVA) =2. 0, catalyst CO (NH2) 21%, 100 C, 120min. Infrared spectroscopy (FT-IR), nuclear magnetic resonance (NMR) and elemental analysis were used to characterize the structure of the unsaturated resin flame retardant.
The thermal properties of it were analyzed by TGA-DSC. The results show that the synthetic route of the unsaturated resin with phosphate ester flame retardant is simple and the flame retardancy is excellent.
Polymer materials are widely used, but the flammability of many organic polymer materials will cause fire hazards. Therefore, all countries in the world are working to develop a variety of flame retardants and flame retardant materials. Phosphorus flame retardant has the characteristics of high flame retardancy, low smoke, low toxicity and non corrosive gas, and its flame retardant effect is related to the phosphorus content of the flame retardant.
Phosphorus flame retardants, especially organophosphorus flame retardants, play an important role in all kinds of flame retardants. The small molecule phosphorus containing flame retardant has the disadvantages of high volatility, easy migration, poor heat resistance and poor mechanical properties of materials, which affects the flame retardance effect and limits its application. Most organic polymers containing phosphorus flame retardants have many advantages such as low smoke, low toxicity, good thermal stability, good flame retardancy, good compatibility with polymer substrates, migration resistance, volatilization resistance and durable flame retardancy. They have become the research focus of flame retardants.
PVA is very conducive to the intramolecular dehydration to produce olefins and aromatic rings at high temperature. Therefore, PVA is a good carbon forming agent in intumescent flame retardant. In this paper, PVA and phosphoric acid as raw material and urea as catalyst, synthesis of unsaturated resin based phosphate flame retardant (PVA-POH), the reaction conditions are studied, through infrared spectroscopy (FT-IR), nuclear magnetic resonance (NMR) and elemental analysis. Its structure, analysis of the thermal performance of TGA-DSC.
Reagents: polyvinyl alcohol (PVA) 20-99 (industrial pure), phosphoric acid, urea, anhydrous ethanol (all analytically pure), osmosis agent JFC
The synthesis of flame retardant PVA-POH: add 5gPVA 250mL three mouth bottle, add 20mL distilled water wetting stirring 15min, then add 10~30mL85% of phosphoric acid, stirring at room temperature after 30min, slowly heated to PVA completely dissolved into a colorless and transparent solution, then adding a certain amount of urea as catalyst, stirring, heating to proper temperature reaction time get, white or pale yellow transparent solution; adding 50mL ethanol precipitation, dissolution and precipitation repeated 3 times, decompression after filtration, vacuum oven drying at 60 DEG 24h, white or pale yellow product PVA-POH.
Tris(2-chloroisopropyl)Phosphate(TCPP)
Cas No:13674 -84-5
HS Code HS: 29199000
The most important indicator of product:
colorless transparent liquid, moisture ≤ 0.1, Acid value ≤ 0.1, Chroma ≤ 50, the phosphorus content: 9.4 ± 0.5
Raw materials: phosphorus oxychloride and epichlorohydrin.
Belong to several categories of dangerous goods:
Currently Tris(2-chloroisopropyl)Phosphate TCPP general cargo exports are not dangerous.
The product is used for the soft / hard polyurethane foam, with thermal and hydrolytic stability good, especially suitable for ASTME84 (Level 11) foam, with low viscosity unsaturated polyester resin in low temperature application and phenolic plastics at. This product is also used to grab the foam sealant and sheet production. For polyvinyl chloride, polystyrene, phenolic resin, acrylic resin and rubber, coating, flame retardant, also used for soft and hard polyurethane foam, epoxy resin, polystyrene, cellulose acetate, ethyl cellulose tree and phenolic plastics, polyvinyl acetate and gun type foam sealant production. Particularly recommended for rigid polyurethane foam has excellent thermal and hydrolytic stability is particularly suitable for ASTM84 (II), compound for polyurethane foam and unsaturated resin and phenolic plastics.
PVA-POH texture characterization: infrared spectroscopy (FT-IR): NicoletFT-IR6700 type infrared spectrometer, KBr pellet; nuclear magnetic resonance (NMR): VarianunityInova-400 NMR test 1H-, 31P-, 13C-NMR spectrum, DMSO-d6 as solvent, the internal standard was four methyl silane (TMS); element analysis (EA): CarloErba1106CHN element analyzer (Italy) C, H, O determination of content; phosphorus content with vanadium ammonium molybdate colorimetric method (GB/T6437-2002) determination.
Flame-retardant finishing process: two immersion two rolling (flame retardant PVA-POH300g/L, urea 100g/L, phosphoric acid 15g/L, penetrant JFC10g/L, rolling rate 70%~80%) to pre drying (90 degrees, 5min) to baking (165 C, 3min) to soap wash, water wash and drying.
Thermal analysis (TGA-DSC): using the synchronous thermal analyzer STA449CJupiter (Germany NETZSCH), the nitrogen flow rate is 45mL/min, and the 5~7mg sample is called to the aluminum crucible, and the temperature rises from 10 to 40 degrees to 590 degrees.
With the increase of the amount of phosphoric acid, the phosphorus content increased obviously, but when m (H3PO4) /m (PVA) >2. At 0, the degree of increase slowed down; >2. After 25, the yield decreased, probably because the higher the amount of phosphoric acid, the more intramolecular dehydration at the time of reaction. And the higher the amount of phosphoric acid, the color of the flame retardant gradually changed from white to yellowish, so its application range was limited. Select m (H3PO4) /m (PVA) =2. 0 is better.
With the increase of reaction temperature, the yield and phosphorus content increased first and then decreased, and the color of the products gradually deepened. The yield and phosphorus content were higher at 100 DEG, 105 DEG C yield and phosphorus content reached the maximum, and then continue to heat the reaction product appears black, dehydration obviously, phosphorus content and yield were significantly decreased. In consideration of energy, the optimum reaction temperature is 100.
With the prolongation of reaction time, the yield and phosphorus content increased. The yield of 120min was higher and the color of flame retardant was white. After 125min, the yield decreased. It may be that the reaction time is too long, resulting in dehydration and carbonization of products, resulting in the color of products. Consider the color of the flame retardant and choose 120min.
Copyright: Zhang Jia Gang YaRui Chemical co.,Ltd
http://www.yaruichem.com
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