本文選題：硅橡膠 + 次磷酸鋁��； 參考：《青島科技大學(xué)》2015年碩士論文

【摘要】：硅橡膠作為發(fā)展速度最快的合成材料之一,由于其優(yōu)異的熱穩(wěn)定性、低溫韌性以及絕緣性被廣泛應(yīng)用于各個(gè)領(lǐng)域,尤其是在電子電氣產(chǎn)品方面。然而,硅橡膠易燃的特點(diǎn)極大限制了其在某些領(lǐng)域的應(yīng)用。所以有必要對(duì)硅橡膠添加阻燃劑以改善其阻燃性能。次磷酸鹽類化合物作為一種環(huán)境友好型的無(wú)鹵阻燃劑正迅速發(fā)展。其功能不同于其他無(wú)機(jī)材料和鹵代化合物阻燃劑,而是通過(guò)催化形成致密的炭化層,保護(hù)內(nèi)部材料不被進(jìn)一步燃燒,同時(shí)抑制了有毒氣體的釋放。但是,次磷酸鹽仍然存在阻燃效率不高的問(wèn)題,采用協(xié)同阻燃技術(shù)有望進(jìn)一步提高其阻燃效率。為此,本文采用次磷酸鋁(AHP)為阻燃劑,可膨脹石墨(EG)、空心玻璃微球(HGM)、鐵紅(Fe203)、鐵黃(FeOOH)和二茂鐵(Fer)作為協(xié)效劑,通過(guò)混煉的方法制備阻燃硅橡膠復(fù)合材料,并使用錐形量熱儀(CCT)、熱重分析儀(TGA)和紅外光譜儀(FT-IR)對(duì)復(fù)合材料的燃燒性、熱穩(wěn)定性和揮發(fā)產(chǎn)物進(jìn)行了研究。主要包括以下內(nèi)容：(1)通過(guò)CCT、TGA和FT-IR對(duì)EG協(xié)效AHP阻燃SR復(fù)合材料及燃燒特性進(jìn)行研究。CCT結(jié)果表明,AHP可以增強(qiáng)SR材料的阻燃性,EG對(duì)SR/AHP復(fù)合材料有顯著的協(xié)效阻燃作用。20wt%的AHP使SR復(fù)合材料的PHRR由530kW/m2下降到320kW/m2,殘?zhí)柯蕪?5%提高到33%。4wt%的EG使SR/AHP復(fù)合材料的PHRR下降到192kW/m2,比純SR樣品降低了64%,且殘?zhí)柯侍岣叩?8%。炭渣照片顯示,AHP使炭層致密,表面完整,EG使SR/AHP復(fù)合材料的炭渣膨脹,且炭層更為致密。TGA結(jié)果表明,AHP的添加增強(qiáng)了SR復(fù)合材料的高溫區(qū)熱穩(wěn)定性,EG的添加對(duì)SR/AHP復(fù)合材料的熱穩(wěn)定性有促進(jìn)作用。20wt%的AHP使SR復(fù)合材料的初始分解溫度由390℃降低到339℃,最終殘?zhí)苛繌?2.3%提升到52.3%,復(fù)合材料的熱降解階段由一個(gè)增加到兩個(gè)。4wt%的EG使SR/AHP復(fù)合材料的60%質(zhì)量損失溫度從480℃提高到523℃,殘?zhí)柯蕪?2.3%提高到57.6%。揮發(fā)產(chǎn)物的FT-IR結(jié)果顯示,EG和AHP使SR復(fù)合材料在3000-2800,2400-2300和1300-750cm-1處的吸收強(qiáng)度降低。說(shuō)明EG和AHP可抑制SR復(fù)合材料在燃燒過(guò)程中可燃性氣體及二氧化碳的釋放。(2)通過(guò)CCT、TGA和FT-IR對(duì)HGM協(xié)效AHP阻燃SR復(fù)合材料及燃燒特性進(jìn)行研究。CCT結(jié)果表明,HGM對(duì)SR/AHP復(fù)合材料有良好的協(xié)效阻燃作用。4wt%的HGM使SR/AHP復(fù)合材料的PHRR從318kW/m2降低到224kW/m2,1 wt%的HGM使SR/AHP復(fù)合材料的殘?zhí)柯蕪?3%提高到40%。炭渣照片顯示,HGM使SR/AHP復(fù)合材料的炭渣膨脹,且炭層更為致密。TGA結(jié)果表明,HGM對(duì)SR/AHP復(fù)合材料的熱穩(wěn)定性有促進(jìn)作用。4wt%的HGM使SR/AHP復(fù)合材料的初始分解溫度由338℃C提高到350℃,0.5wt%的HGM使SR/AHP復(fù)合材料的殘?zhí)柯蕪?2.6%提高到55.1%。揮發(fā)產(chǎn)物的FT-IR結(jié)果表明,HGM使SR復(fù)合材料在3000-2800,2400-2300和1300-750cm-1處的吸收強(qiáng)度降低。說(shuō)明HGM可抑制SR/AHP復(fù)合材料在燃燒過(guò)程中可燃性氣體及二氧化碳的釋放。(3)通過(guò)CCT、TGA和FT-IR分別對(duì)Fe2O3、FeOOH和Fer協(xié)效AHP阻燃SR復(fù)合材料及燃燒特性進(jìn)行研究。CCT結(jié)果表明,3. FeOOH和Fer均對(duì)SR/AHP復(fù)合材料有協(xié)效阻燃效果。4wt%的Fe2O3使SR/AHP復(fù)合材料的PHRR由318kW/m2降低到183kW/m2,殘?zhí)柯蕪?3%提高到50%；4wt%的FeOOH使SR/AHP復(fù)合材料的PHRR由318kW/m2下降到198kW/m2,殘?zhí)柯蕪?3%提高到47%;0.5wt%的Fer可使SR/AHP復(fù)合材料的PHRR由318kW/m2下降到172kW/m2,當(dāng)Fer的含量達(dá)到4wt%時(shí),SR/AHP復(fù)合材料的殘?zhí)柯视?1%提升到56%。通過(guò)對(duì)比,三種鐵系化合物中Fer對(duì)SR/AHP具有較好的協(xié)效阻燃作用。TGA結(jié)果顯示,4wt%的Fe2O3使SR/AHP復(fù)合材料的初始分解溫度由330℃降低到322℃,其殘?zhí)苛繉?duì)比SR/AHP復(fù)合材料也有所下降,由52.4%下降到46.7%；4wt%的FeOOH使SR/AHP復(fù)合材料的初始分解溫度上升到363℃,最終殘?zhí)柯氏陆档?1.4%：4wt%的Fer沒(méi)有對(duì)SR/AHP復(fù)合材料的初始分解溫度造成影響,但其殘?zhí)柯氏陆盗?.9個(gè)百分點(diǎn)。以上結(jié)果與Mass結(jié)果相矛盾,這是樣品的規(guī)模效應(yīng)造成的,由于TGA取樣質(zhì)量過(guò)小,協(xié)效劑的含量增多并沒(méi)有對(duì)復(fù)合材料的熱穩(wěn)定性顯現(xiàn)改善效果。揮發(fā)產(chǎn)物的FT-IR結(jié)果表明,三種鐵系化合物均可使SR/AHP復(fù)合材料在3000-2800,2400-2300和1300-750cm-1處的吸收強(qiáng)度降低,其中Fer的效果最為明顯。說(shuō)明Fer比Fe203和FeOOH對(duì)于抑制SR/AHP復(fù)合材料在燃燒過(guò)程中釋放可燃性氣體及二氧化碳的效果更好。
[Abstract]:As one of the fastest growing synthetic materials, silicone rubber is widely used in various fields because of its excellent thermal stability, low temperature toughness and insulation, especially in electronic and electrical products. However, the flammability of silicone rubber restricts its application in some fields. Therefore, it is necessary to add flame retardants to silicone rubber. In order to improve its flame retardancy, the hypophosphite is developing rapidly as an environmentally friendly halogen free flame retardant. Its function is different from other inorganic materials and halogenated flame retardants, but by catalyzing the formation of compact carbonization layer, protecting the internal materials from further combustion and inhibiting the release of toxic gases. It is a problem that hypophosphite still has low flame retardancy efficiency, and it is expected to further improve its flame retardancy efficiency by using synergistic flame retardancy technology. Therefore, this paper uses aluminum hypophosphite (AHP) as flame retardant, expansible graphite (EG), hollow glass microsphere (HGM), iron red (Fe203), iron yellow (FeOOH) and two ferrocene (Fer) as synergist, by mixing method The flame retardant, thermal stability and volatilization products of the composites were studied by conical calorimeter (CCT), thermogravimetric analyzer (TGA) and infrared spectrometer (FT-IR). The main contents were as follows: (1) the.CCT result table was studied by CCT, TGA and FT-IR for EG co effective AHP flame retardant SR Composites and combustion characteristics. It is clear that AHP can enhance the flame retardancy of the SR material. EG has a significant synergistic effect on the SR/AHP composite with a synergistic flame retarding effect of.20wt%, which reduces the PHRR of the SR composite from 530kW/m2 to 320kW/m2. The carbon residue rate from 25% to 33%.4wt% makes the composite material decrease to 64%, and the carbon residue rate is increased to the carbon residue. The photo shows that AHP makes the carbon layer dense and the surface is complete. EG makes the carbon slag of SR/AHP composites expand and the carbon layer is more compact.TGA. The addition of AHP enhances the thermal stability of the high temperature zone of the SR composite, and the addition of EG promotes the thermal stability of the SR/AHP composite by.20wt% AHP to the initial decomposition temperature of the SR composite material by 39. The final carbon residue was reduced from 0 to 339, and the final carbon residue was increased from 22.3% to 52.3%. The thermal degradation phase of the composite was increased from one to two.4wt% EG to increase the 60% mass loss temperature of SR/AHP composites from 480 to 523, and the carbon residue rate from 52.3% to 57.6%. volatilization product FT-IR fruit. EG and AHP made SR composites in 3000-28002400 The absorption strength of -2300 and 1300-750cm-1 decreases. It shows that EG and AHP can inhibit the release of combustible gas and carbon dioxide in the combustion process of SR composites. (2) the study of HGM co effective AHP flame retardant SR composites and combustion properties by CCT, TGA and FT-IR The HGM of wt% made the PHRR of SR/AHP composite decreased from 318kW/m2 to 224kW/m2,1 wt% HGM, and the carbon residue rate of SR/AHP composite material was increased from 33% to the 40%. carbon slag, and the carbon slag in the SR/AHP composite was expanded and the carbon layer was more compact. The initial decomposition temperature of P composites was increased from 338 C to 350, and HGM of 0.5wt% increased the residual carbon rate of SR/AHP composites from 52.6% to 55.1%. volatilization products. The results showed that HGM reduced the absorption strength of SR composite at 3000-28002400-2300 and 1300-750cm-1. The release of combustible gases and carbon dioxide. (3) the experimental results of Fe2O3, FeOOH and Fer synergistic AHP flame retardant SR composites and combustion properties were studied by CCT, TGA and FT-IR respectively. The rate of 4wt% increased from 33% to 50%; the PHRR of the SR/AHP composite decreased from 318kW/m2 to 198kW/m2, the residual carbon rate increased from 33% to 47%, and Fer of 0.5wt% reduced the PHRR from 318kW/m2 to 172kW/m2. When the content of the composite was reached, the carbon residue rate of the composite was raised from 31% to three ferric systems. The results of a better synergistic flame retardant effect of Fer on SR/AHP showed that the initial decomposition temperature of 4wt% composites decreased from 330 to 322, and the residual carbon content of SR/AHP composites decreased from 52.4% to 46.7%, and 4wt% FeOOH made the initial decomposition temperature of SR/AHP composites up to 363. The loss of the final carbon residue to 51.4%:4wt% Fer did not affect the initial decomposition temperature of the SR/AHP composite, but the carbon residue decreased by 5.9 percentage points. The above results contradict the results of the Mass. This is the result of the scale effect of the sample. As the mass of the sample is too small, the synergist increases and does not heat the composite. The FT-IR results of the volatile products show that the three kinds of iron system compounds can reduce the absorption strength of the SR/AHP composites at 3000-28002400-2300 and 1300-750cm-1, and the effect of Fer is most obvious. It shows that Fer is more effective than Fe203 and FeOOH to release the combustible gas in the combustion process. Carbon dioxide has a better effect.
【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】：2015
【分類號(hào)】：TB33

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