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Phosphorus containing flame retardant for epoxy resin
2017-12-3 15:48:18
Phosphorus containing flame retardant for epoxy resin
The synthesis of novel aromatic aromatic epoxy resin containing phosphorus flame retardant polyphenylphosphonic acid (9, 10- two hydrogen -9- -10- -10- phosphonyl phenylene ester) and its effect on the flame retardancy of epoxy resin (ER) and unsaturated polyester resin (USPE) were studied.
The phosphorous flame retardant used for epoxy resin is obtained by melting polycondensation of 2- (6- oxygen -6 oxygen phosphonyl phenanthrene) 1, 4- hydroquinone and phosphonyl two chlorine. The phosphorus content of 13.8% poly phenyl phosphate (9 10-, two -9- -10- hydrogen oxa phosphaphenanthrene phosphonomethoxy) phenyl ester added to epoxy resin, unsaturated resin, the results show that the epoxy resin used for flame retardant epoxy resin, unsaturated resin has good flame retardant properties, content of only 2% the phosphorus content of only 0.28% when the oxygen index can reach 28 LOI, flame retardant UL-94 can reach VO level.
In recent decades, with the development of science and technology, plastic, rubber, synthetic fiber and polymer materials in aerospace engineering, transportation, electronic appliances and daily necessities and other fields has been widely used, but most of the polymers are flammable, combustible, and some also produce a lot of smoke and toxic gases, causing harm to the environment the huge loss caused by social wealth, pose a huge threat to the safety of people's life.
In the fire incident, a large proportion of the fire was caused by the ignition of polymer materials. Therefore, the development of flame retardants for polymer materials, especially the environmentally friendly halogen free flame retardants, is a hot spot of research on the flame retardancy of polymer materials in various countries.
After entering 1990s, flame retardant technology has experienced 1 a new stage of development, in addition to the flame retardant flame propagation speed, meet the basic requirements of low smoke, low toxicity, high efficiency, but also needs to satisfy the introduction, less content of flame retardant polymer materials will not lead to the original performance requirements such as excessive deterioration.
Therefore, in recent years, high efficiency, low smoke, low toxicity, dustless or less dust constitute the key research topics in the field of flame retardants, and also the main direction of the development of flame retardants in the world.
We synthesize 1 kinds of high phosphorus halogen-free flame retardants, and this new type of flame retardant epoxy resin, added to the eight flame retardancy of unsaturated fat and are discussed in this paper.
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.
The main raw materials: 9 10-, two -9 -10 hydrogen oxa phosphaphenanthrene (DOPO) and Phenylphosphonic chloride two, industrial products, before use after purification; pure analysis, benzoquinone, are chemical reagent factory products; epoxy resin E-44 light yellow liquid, 0.41 ~ 0.47mol/100g epoxy value, softening point to 12 20 DEG C; unsaturated polyester 191, Changzhou 253 building materials factory, light yellow transparent liquid, the acid value of KOH:28 ~ 36mg/g, the viscosity of 0.25 ~ 0.45Pa s.
The synthesis of flame retardants. The method is provided to synthesize ODOPB. The synthesis of PDPPP is followed by the conditions of the previous synthesis of PSPPP. In the 250mL reaction bottle with nitrogen import and export and agitator, the phosphonyl chloride 0.19mol, ODOPB 0.185mol and the catalyst are added.
Through nitrogen, heating up heating, maintaining the temperature of 160 C reaction 1.5h, and then increasing the temperature to 220 degrees C, and continue to react to 2H. The residual HCl gas in the system was removed from the vacuum system at the later stage. The obtained products are light yellow, and the mass of molecular weight is 3000~8900, and the melting point is 195~204.
The flame retardant synthesized by POPPP was analyzed by FT-IR170SX infrared spectrometer and KBr press. The content of C, O and H was determined by Heraeus element analyzer. The content of P was treated by Schoniger combustion bottle method and detected by inductively coupled plasma atomic emission spectrometry (ICP-AES). The Finnigan-4570 type low resolution GC/MS was used for mass spectrometric analysis. The 1H-NMR spectra of the samples were measured by Bruker AMX-300 NMR.
Preparation of flame-retardant sample, preparation of epoxy resin (ER) E44 flame retardant sample: PDPPP and epoxy resin were added to 500mL cup proportionally under magnetic stirring and heated to 0.5h at 40 C until flame retardants were completely dissolved in epoxy resin. When polyamide 651 is added as a curing agent, 2h is heated at 100 C, and then 48h is placed at room temperature. The obtained solid is cut to get the test sample.
Preparation of unsaturated polyester resin (USPE) 191 flame retardant sample: flame retardant and unsaturated resin should be added to 500mL with magnetic stirring device under nitrogen protection. Increase the temperature to 60 C and heat 1H. Until the flame retardant is completely dissolved, then benzoyl peroxide is added. 4h was treated at 110 C, and then 48h was placed at room temperature. The obtained solid was cut to get the test sample.
The flame retardancy test, the oxygen index (LOI) and the vertical combustion test (UL-94) of the flame retardant samples were tested by the JF-3 type oxygen index instrument and the CZF-2 vertical combustion apparatus according to the standard procedure.
Copyright: Zhang Jia Gang YaRui Chemical co.,Ltd
http://www.yaruichem.com
The synthesis of novel aromatic aromatic epoxy resin containing phosphorus flame retardant polyphenylphosphonic acid (9, 10- two hydrogen -9- -10- -10- phosphonyl phenylene ester) and its effect on the flame retardancy of epoxy resin (ER) and unsaturated polyester resin (USPE) were studied.
The phosphorous flame retardant used for epoxy resin is obtained by melting polycondensation of 2- (6- oxygen -6 oxygen phosphonyl phenanthrene) 1, 4- hydroquinone and phosphonyl two chlorine. The phosphorus content of 13.8% poly phenyl phosphate (9 10-, two -9- -10- hydrogen oxa phosphaphenanthrene phosphonomethoxy) phenyl ester added to epoxy resin, unsaturated resin, the results show that the epoxy resin used for flame retardant epoxy resin, unsaturated resin has good flame retardant properties, content of only 2% the phosphorus content of only 0.28% when the oxygen index can reach 28 LOI, flame retardant UL-94 can reach VO level.
In recent decades, with the development of science and technology, plastic, rubber, synthetic fiber and polymer materials in aerospace engineering, transportation, electronic appliances and daily necessities and other fields has been widely used, but most of the polymers are flammable, combustible, and some also produce a lot of smoke and toxic gases, causing harm to the environment the huge loss caused by social wealth, pose a huge threat to the safety of people's life.
In the fire incident, a large proportion of the fire was caused by the ignition of polymer materials. Therefore, the development of flame retardants for polymer materials, especially the environmentally friendly halogen free flame retardants, is a hot spot of research on the flame retardancy of polymer materials in various countries.
After entering 1990s, flame retardant technology has experienced 1 a new stage of development, in addition to the flame retardant flame propagation speed, meet the basic requirements of low smoke, low toxicity, high efficiency, but also needs to satisfy the introduction, less content of flame retardant polymer materials will not lead to the original performance requirements such as excessive deterioration.
Therefore, in recent years, high efficiency, low smoke, low toxicity, dustless or less dust constitute the key research topics in the field of flame retardants, and also the main direction of the development of flame retardants in the world.
We synthesize 1 kinds of high phosphorus halogen-free flame retardants, and this new type of flame retardant epoxy resin, added to the eight flame retardancy of unsaturated fat and are discussed in this paper.
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.
The main raw materials: 9 10-, two -9 -10 hydrogen oxa phosphaphenanthrene (DOPO) and Phenylphosphonic chloride two, industrial products, before use after purification; pure analysis, benzoquinone, are chemical reagent factory products; epoxy resin E-44 light yellow liquid, 0.41 ~ 0.47mol/100g epoxy value, softening point to 12 20 DEG C; unsaturated polyester 191, Changzhou 253 building materials factory, light yellow transparent liquid, the acid value of KOH:28 ~ 36mg/g, the viscosity of 0.25 ~ 0.45Pa s.
The synthesis of flame retardants. The method is provided to synthesize ODOPB. The synthesis of PDPPP is followed by the conditions of the previous synthesis of PSPPP. In the 250mL reaction bottle with nitrogen import and export and agitator, the phosphonyl chloride 0.19mol, ODOPB 0.185mol and the catalyst are added.
Through nitrogen, heating up heating, maintaining the temperature of 160 C reaction 1.5h, and then increasing the temperature to 220 degrees C, and continue to react to 2H. The residual HCl gas in the system was removed from the vacuum system at the later stage. The obtained products are light yellow, and the mass of molecular weight is 3000~8900, and the melting point is 195~204.
The flame retardant synthesized by POPPP was analyzed by FT-IR170SX infrared spectrometer and KBr press. The content of C, O and H was determined by Heraeus element analyzer. The content of P was treated by Schoniger combustion bottle method and detected by inductively coupled plasma atomic emission spectrometry (ICP-AES). The Finnigan-4570 type low resolution GC/MS was used for mass spectrometric analysis. The 1H-NMR spectra of the samples were measured by Bruker AMX-300 NMR.
Preparation of flame-retardant sample, preparation of epoxy resin (ER) E44 flame retardant sample: PDPPP and epoxy resin were added to 500mL cup proportionally under magnetic stirring and heated to 0.5h at 40 C until flame retardants were completely dissolved in epoxy resin. When polyamide 651 is added as a curing agent, 2h is heated at 100 C, and then 48h is placed at room temperature. The obtained solid is cut to get the test sample.
Preparation of unsaturated polyester resin (USPE) 191 flame retardant sample: flame retardant and unsaturated resin should be added to 500mL with magnetic stirring device under nitrogen protection. Increase the temperature to 60 C and heat 1H. Until the flame retardant is completely dissolved, then benzoyl peroxide is added. 4h was treated at 110 C, and then 48h was placed at room temperature. The obtained solid was cut to get the test sample.
The flame retardancy test, the oxygen index (LOI) and the vertical combustion test (UL-94) of the flame retardant samples were tested by the JF-3 type oxygen index instrument and the CZF-2 vertical combustion apparatus according to the standard procedure.
Copyright: Zhang Jia Gang YaRui Chemical co.,Ltd
http://www.yaruichem.com
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