反相悬浮聚合法制备膨胀型阻燃剂及阻燃丁苯橡胶的性能研究
发布时间：2018-11-19 20:09
【摘要】：本文以研究化学膨胀阻燃SBR为目标,首先采用自由基引发体系,引发丙烯酸钠和丙烯酰胺共聚,将经典化学膨胀阻燃(IFR)体系三组分(聚磷酸APP、季戊四醇PET、三聚氰胺MEL)进行原位包裹,研究三组分之间阻燃效果最佳时的质量匹配,研究发现:MEL的添加量为膨胀阻燃剂的3wt%,APP:PER质量比在4～5.67之间时剩炭率最高,扫描电镜(SEM)结果发现剩炭率较高的膨胀型阻燃剂的泡沫炭层泡孔较均匀,泡孔壁较厚,隔热、隔质效果好。 为了提高SBR/IFR体系的综合力学及阻燃性能,采用反相悬浮聚合法制备IFR微粉,同时讨论了反相悬浮聚合体系稳定性的影响因素,确定了稳定聚合的聚合条件:98%Span-80+2%TX-10复配乳化剂乳化反相悬浮聚合体系的油相析出量明显要少于其他单一乳化改体系时油相的析出量;在乳化剂用量为单体质量的10%时,整个聚合体系表现出良好的稳定性;当搅拌速率增大到1000r/min时,搅拌速率对于整个聚合体系的影响趋于平缓,1.5h之后剪切应力对单体液滴的尺寸影响不大,故乳化时间定为1.5h;阻燃性能研究确定IFR添加量为30份时为最佳。 最后通过热分析动力学、SEM和TG-FTIR技术讨论了IFR阻燃SBR的阻燃机理。SEM测试表明:反相悬浮聚合法制备的阻燃剂颗粒尺寸大小主要集中在0.5μm附近,且阻燃剂颗粒表面光滑形态呈现出规则的球体,SBR/IFR(30wt%)燃烧后试样表面炭层结构致密,炭层内部并有尺寸大小均匀的蜂窝状的炭层小室,小室在炭层上覆盖均匀,几乎为闭合结构;SBR/IFR体系热降解过程的热分解动力学分析显示:N2和空气气氛下SBR/IFR体系热降解过程反应级数均接近于理论值1,热降解反应主要受核增长与生长机理控制,其中空气气氛下还受部分气体产物在气相边界层的外扩散机理控制,由于炭层在氧气的存在体系氧化成大量的CO2气体逸出时受到边界向外扩散速率的影响。
[Abstract]:In this paper, the chemical intumescent flame retardant (SBR) was studied. Firstly, the copolymerization of sodium acrylate and acrylamide was initiated by the free radical initiator system. The three components of the classical chemical intumescent flame retardant (IFR) system (APP, pentaerythritol polyphosphate PET,) were prepared. Melamine MEL was encapsulated in situ to study the mass matching when the flame retardant effect was best among the three components. The results showed that the highest residual carbon rate was obtained when the mass ratio of MEL to per was 45.67 when the content of MEL was 3wt of the intumescent flame retardant. Scanning electron microscope (SEM) results showed that the foam carbon layer with high residual carbon content had more uniform foam pores, thicker foam pore wall, better insulation and better insulation effect. In order to improve the comprehensive mechanical and flame retardant properties of SBR/IFR system, IFR powder was prepared by inverse suspension polymerization. The factors influencing the stability of inverse suspension polymerization system were discussed. The polymerization conditions of stable polymerization were determined as follows: the amount of oil phase precipitation of 98%Span-80 2%TX-10 emulsifier emulsion inverse suspension polymerization system was obviously lower than that of other single emulsification modification system; When the amount of emulsifier is the mass of monomer, the whole polymerization system shows good stability. When the stirring rate is increased to 1000r/min, the effect of stirring rate on the whole polymerization system tends to be gentle, and the shear stress has little effect on the size of the monomer droplet after 1.5 h, so the emulsifying time is 1.5 h. The flame retardancy of IFR was determined to be the best when the content of IFR was 30 phr. Finally, the flame retardant mechanism of IFR flame-retardant SBR was discussed by thermal analysis kinetics, SEM and TG-FTIR techniques. SEM test showed that the particle size of flame retardant prepared by reverse suspension polymerization was mainly around 0.5 渭 m. The smooth surface of flame retardant particles showed a regular sphere. After SBR/IFR (30 wt%) combustion, the carbon layer on the surface of the sample was compact, and the carbon layer had a honeycomb chamber inside the carbon layer, and the chamber was evenly covered on the carbon layer. Almost closed structure; The kinetic analysis of thermal degradation of SBR/IFR system shows that the reaction order of SBR/IFR system in N2 and air atmospheres is close to the theoretical value of 1, and the thermal degradation reaction is mainly controlled by nuclear growth and growth mechanism. The diffusion mechanism of some gas products in the gas phase boundary layer is also controlled in the air atmosphere. Because the carbon layer is oxidized to a large amount of CO2 gas in the presence of oxygen system, it is affected by the boundary diffusion rate.
【学位授予单位】：青岛科技大学
【学位级别】：硕士
【学位授予年份】：2011
【分类号】：TQ333.1
本文编号：2343304
[Abstract]:In this paper, the chemical intumescent flame retardant (SBR) was studied. Firstly, the copolymerization of sodium acrylate and acrylamide was initiated by the free radical initiator system. The three components of the classical chemical intumescent flame retardant (IFR) system (APP, pentaerythritol polyphosphate PET,) were prepared. Melamine MEL was encapsulated in situ to study the mass matching when the flame retardant effect was best among the three components. The results showed that the highest residual carbon rate was obtained when the mass ratio of MEL to per was 45.67 when the content of MEL was 3wt of the intumescent flame retardant. Scanning electron microscope (SEM) results showed that the foam carbon layer with high residual carbon content had more uniform foam pores, thicker foam pore wall, better insulation and better insulation effect. In order to improve the comprehensive mechanical and flame retardant properties of SBR/IFR system, IFR powder was prepared by inverse suspension polymerization. The factors influencing the stability of inverse suspension polymerization system were discussed. The polymerization conditions of stable polymerization were determined as follows: the amount of oil phase precipitation of 98%Span-80 2%TX-10 emulsifier emulsion inverse suspension polymerization system was obviously lower than that of other single emulsification modification system; When the amount of emulsifier is the mass of monomer, the whole polymerization system shows good stability. When the stirring rate is increased to 1000r/min, the effect of stirring rate on the whole polymerization system tends to be gentle, and the shear stress has little effect on the size of the monomer droplet after 1.5 h, so the emulsifying time is 1.5 h. The flame retardancy of IFR was determined to be the best when the content of IFR was 30 phr. Finally, the flame retardant mechanism of IFR flame-retardant SBR was discussed by thermal analysis kinetics, SEM and TG-FTIR techniques. SEM test showed that the particle size of flame retardant prepared by reverse suspension polymerization was mainly around 0.5 渭 m. The smooth surface of flame retardant particles showed a regular sphere. After SBR/IFR (30 wt%) combustion, the carbon layer on the surface of the sample was compact, and the carbon layer had a honeycomb chamber inside the carbon layer, and the chamber was evenly covered on the carbon layer. Almost closed structure; The kinetic analysis of thermal degradation of SBR/IFR system shows that the reaction order of SBR/IFR system in N2 and air atmospheres is close to the theoretical value of 1, and the thermal degradation reaction is mainly controlled by nuclear growth and growth mechanism. The diffusion mechanism of some gas products in the gas phase boundary layer is also controlled in the air atmosphere. Because the carbon layer is oxidized to a large amount of CO2 gas in the presence of oxygen system, it is affected by the boundary diffusion rate.
【学位授予单位】：青岛科技大学
【学位级别】：硕士
【学位授予年份】：2011
【分类号】：TQ333.1
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