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反相懸浮聚合法制備膨脹型阻燃劑及阻燃丁苯橡膠的性能研究

發(fā)布時(shí)間:2018-11-19 20:09
【摘要】:本文以研究化學(xué)膨脹阻燃SBR為目標(biāo),首先采用自由基引發(fā)體系,引發(fā)丙烯酸鈉和丙烯酰胺共聚,將經(jīng)典化學(xué)膨脹阻燃(IFR)體系三組分(聚磷酸APP、季戊四醇PET、三聚氰胺MEL)進(jìn)行原位包裹,研究三組分之間阻燃效果最佳時(shí)的質(zhì)量匹配,研究發(fā)現(xiàn):MEL的添加量為膨脹阻燃劑的3wt%,APP:PER質(zhì)量比在4~5.67之間時(shí)剩炭率最高,掃描電鏡(SEM)結(jié)果發(fā)現(xiàn)剩炭率較高的膨脹型阻燃劑的泡沫炭層泡孔較均勻,泡孔壁較厚,隔熱、隔質(zhì)效果好。 為了提高SBR/IFR體系的綜合力學(xué)及阻燃性能,采用反相懸浮聚合法制備IFR微粉,同時(shí)討論了反相懸浮聚合體系穩(wěn)定性的影響因素,確定了穩(wěn)定聚合的聚合條件:98%Span-80+2%TX-10復(fù)配乳化劑乳化反相懸浮聚合體系的油相析出量明顯要少于其他單一乳化改體系時(shí)油相的析出量;在乳化劑用量為單體質(zhì)量的10%時(shí),整個(gè)聚合體系表現(xiàn)出良好的穩(wěn)定性;當(dāng)攪拌速率增大到1000r/min時(shí),攪拌速率對(duì)于整個(gè)聚合體系的影響趨于平緩,1.5h之后剪切應(yīng)力對(duì)單體液滴的尺寸影響不大,故乳化時(shí)間定為1.5h;阻燃性能研究確定IFR添加量為30份時(shí)為最佳。 最后通過(guò)熱分析動(dòng)力學(xué)、SEM和TG-FTIR技術(shù)討論了IFR阻燃SBR的阻燃機(jī)理。SEM測(cè)試表明:反相懸浮聚合法制備的阻燃劑顆粒尺寸大小主要集中在0.5μm附近,且阻燃劑顆粒表面光滑形態(tài)呈現(xiàn)出規(guī)則的球體,SBR/IFR(30wt%)燃燒后試樣表面炭層結(jié)構(gòu)致密,炭層內(nèi)部并有尺寸大小均勻的蜂窩狀的炭層小室,小室在炭層上覆蓋均勻,幾乎為閉合結(jié)構(gòu);SBR/IFR體系熱降解過(guò)程的熱分解動(dòng)力學(xué)分析顯示:N2和空氣氣氛下SBR/IFR體系熱降解過(guò)程反應(yīng)級(jí)數(shù)均接近于理論值1,熱降解反應(yīng)主要受核增長(zhǎng)與生長(zhǎng)機(jī)理控制,其中空氣氣氛下還受部分氣體產(chǎn)物在氣相邊界層的外擴(kuò)散機(jī)理控制,由于炭層在氧氣的存在體系氧化成大量的CO2氣體逸出時(shí)受到邊界向外擴(kuò)散速率的影響。
[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.
【學(xué)位授予單位】:青島科技大學(xué)
【學(xué)位級(jí)別】:碩士
【學(xué)位授予年份】:2011
【分類(lèi)號(hào)】:TQ333.1

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