大豆油基聚氨酯的改性及其纳米复合材料的制备与表征
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摘要
随着环境保护和石油资源枯竭两大难题越来越被重视,研究以可再生资源为原料制备环境友好的聚合物越来越成为关注的焦点。本文采用具有生物可降解和生物相容性的大豆油基多元醇作为聚氨酯(PU)的软段,并在PU基体中引入了丙烯酸酯、羟基官能化的碳纳米管(CNT)以及表面改性的凹凸棒土(ATT),制备了聚氨酯丙烯酸酯、PU/CNT和PU/ATT纳米复合材料,研究了结构与性能的关系,对拓展PU应用领域有重要的理论和实用意义。另外,本文还尝试使用辐射接枝法来对氧化石墨和石墨烯有机化改性,以提高其在聚合物中的分散性。
1.采用甲醇、乙二醇和1,2-丙二醇为开环试剂,环氧大豆油开环得到三种多元醇,先和异佛尔酮二异氰酸酯(IPDI)预聚得到PU预聚体,再和丙烯酸羟乙酯(HEA)经过热聚合制备聚氨酯丙烯酸酯(PUA)树脂。引入丙烯酸酯后,可以显著提高聚氨酯的交联密度、玻璃化转变温度、阻尼性能、热稳定性和拉伸强度,且随着多元醇的羟基值的增大而增大。值得注意的是样品PUA248的拉伸强度高达40MPa以及杨氏模量为724MPa,可以作为硬塑料使用。该大豆油基聚氨酯丙烯酸酯树脂可以作为绿色、价廉以及可生物降解材料用于绝缘材料领域。
2.采用三种不同直径的羟基官能化CNT增强大豆油基PU,目的在于研究其结构与PU性能的关系。结果表明,直径较大的CNT相比直径较小的CNT而言,分散性要好一些,直径较小的CNT容易形成不可逆的团聚。对于制备优异性能的CNT基纳米复合材料,共价官能化处理是一种最为有效的方法,用来提高负载转移效率,然而我们的实验结果表明, CNT的分散性是更为重要的影响因素。PU/CNT纳米复合材料的拉伸强度和杨氏模量随着CNT直径的增大不断提高。相比纯PU而言,随着CNT的直径不断增大,热电导率分别提高了77%、63%和80%。PU/CNT纳米复合材料的玻璃化转变温度同样也随着CNT的直径增大而增大,另外,加入少量的CNT(1wt%)到PU基体中,可以明显地提高其热稳定性。
3.通过酸活化或硅烷偶联剂(KH560和KH570)的表面改性得到了三种改性凹凸棒土,表面处理不影响ATT的晶体结构,经过硅烷偶联剂改性后,硅烷偶联剂包裹在ATT表面。采用不同的凹凸棒土(ATT、acid-ATT、KH560-ATT和KH570-ATT)增强大豆油基PU。结果表明,PU纳米复合材料的储存模量、玻璃化转变温度、拉伸强度和杨氏模量随着ATT的含量增加而不断提高。其中acid-ATT具有最好的增强效应,当填充12wt%的acid-ATT时,PU纳米复合材料的Tg提高了16.8℃,拉伸强度提高了443%,杨氏模量提高了8倍。另外,KH560-ATT和KH570-ATT的加入可以显著提高PU的热稳定性,PU纳米复合材料的热稳定性随着KH560-ATT或KH57O-ATT含量增加而不断提高。
4.通过γ-射线辐照聚合法,聚丙烯酸、聚丙烯酰胺和聚苯乙烯成功接枝到氧化石墨(GO)表面,得到复合物GO-g-PAA、GO-g-PAM和GO-g-PS。复合物GO-g-PAA和GO-g-PAM,热电导率分别为0.44和0.75W／m·K。另外,通过溶剂热法还原GO-g-PS得到聚苯乙烯／石墨烯复合物(G-g-PS),复合物中聚苯乙烯的接枝量高达81.3%,复合物具有优异的热稳定性,起始降解温度可以达到381.5℃。该复合物可以作为纳米填料,制备高性能聚合物纳米复合材料。
With the problem of environmental protection and petroleum-based resources exhaustion have been paid increasing attention, the study on preparation environment friendly polymer derived from renewable resources has become the focus of attention. In the present paper, biodegradable and biocompatible soy-based polyol was used as soft segment of polyurethane (PU). Polyurethane acrylates were prepared by acrylation of polyurethane. Hydroxyl-fuctionalized carbon nanotubes (CNT) and surface modified attapulgite (ATT) were used as fillers to prepared PU/CNT and PU/ATT nanocomposites. The structure-property relationships were studied. It has very important theoretical and practical significance to broaden the apply field of polyurethane materials. Moreover, graphite oxide (GO) and graphene were organic modified via radiation-induced graft polymerization to improve the dispersion in polymer matrix.
1. Three polyols based on ESO were prepared by oxirane ring opening with methanol, glycol, and1,2-propanediol. Polyurethane acrylates (PUAs) were prepared by the reaction of these polyols with isophorone diisocyanate (IPDI) and hydroxyethylacrylate (HEA) by a thermal polymerization process. The acrylated reaction between PU and HEA could significantly increase the crosslinking density, glass transition temperature, damping properties, thermal stability and mechanical properties of PUs. Furthermore, those properties of PUs and PUAs increased with the increasing of OH number. It should be noted that the PUA248appeared as a rigid plastic with the tensile strength higher than40MPa and the Young's modulus of724MPa. The soy-based PUAs could be employed for green, inexpensive, biodegradable materials in insulating material field.
2. Three different diameters of hydroxyl-functionalized CNTs were used to reinforce the soy-based PU matrix. The aim was to find structure-property relationships within neat PU and PU/CNT nanocomposites. The results revealed that the larger diameter CNTs more easily dispersed in the PU matrix than the smaller diameter ones, which easily formed irreversible agglomerates. Covalent functionalizing of CNTs is the most effective method to improve load transfer efficiency. However, our experiment demonstrated that CNT dispersion in the polymer matrix was a more important factor in the production of superior CNT-based nanocomposites. The tensile strength and Young's modulus of PU nanocomposites enhanced with the increase of CNT diameter. As compared with neat PU, with the increase of CNT diameter, the thermal conductivity of PU nanocomposites was improved by77,63and80%, respectively. The glass transition temperature of PU nanocomposites also increased with the increase of CNT diameters. Furthermore, adding small amounts (1wt%) of CNTs to the PU matrix significantly improved its thermal stability.
3. The different ATTs were obtained by acid-activated or silane coupling agents (KH560and KH570) modification. Surface treatment of ATTs did not change its crystal structure. The ATT fibers were coated with silane coupling agents after surface modification. Four types of ATT (neat ATT, acid-ATT, KH560-ATT and KH570-ATT) were used to reinforce the soy-based PU matrix. The storage moduli, glass transition temperature, tensile strength and Young's modulus of PUs significantly increased with the increase of ATT contents. The acid-ATT has the best reinforce effect with12wt% acid-ATT loading,16.8℃improvement in glass transition temperature,443%increment in tensile strength,8-fold increase in Young's modulus of PU nanocomposites were obtained. Furthermore, with the incorporation of KH560and KH570modified ATT, the thermal stability of PU nanocomposites was significantly improved with the increase of ATT content.
4. Poly(acrylic acid)(PAA), poly(acrylamide)(PAM) and polystyrene (PS) successfully grafted GO via y-ray radiation-induced graft polymerization. The result hybrids were named as GO-g-PAA, GO-g-PAM and GO-g-PS, respectively. The thermal conductivities of GO-g-PAA and GO-g-PAM were0.44and0.75W/m-K, respectively. Moreover, GO-g-PS was reduced by solvothermal method to prepare PS/graphene hybrid. The hybrid has higher than81.3%grafted PS and excellent thermal stability with initial decomposition temperature of381.5℃. It could be used as nanofiller to prepare superior polymer nanocomposites.
1.采用甲醇、乙二醇和1,2-丙二醇为开环试剂,环氧大豆油开环得到三种多元醇,先和异佛尔酮二异氰酸酯(IPDI)预聚得到PU预聚体,再和丙烯酸羟乙酯(HEA)经过热聚合制备聚氨酯丙烯酸酯(PUA)树脂。引入丙烯酸酯后,可以显著提高聚氨酯的交联密度、玻璃化转变温度、阻尼性能、热稳定性和拉伸强度,且随着多元醇的羟基值的增大而增大。值得注意的是样品PUA248的拉伸强度高达40MPa以及杨氏模量为724MPa,可以作为硬塑料使用。该大豆油基聚氨酯丙烯酸酯树脂可以作为绿色、价廉以及可生物降解材料用于绝缘材料领域。
2.采用三种不同直径的羟基官能化CNT增强大豆油基PU,目的在于研究其结构与PU性能的关系。结果表明,直径较大的CNT相比直径较小的CNT而言,分散性要好一些,直径较小的CNT容易形成不可逆的团聚。对于制备优异性能的CNT基纳米复合材料,共价官能化处理是一种最为有效的方法,用来提高负载转移效率,然而我们的实验结果表明, CNT的分散性是更为重要的影响因素。PU/CNT纳米复合材料的拉伸强度和杨氏模量随着CNT直径的增大不断提高。相比纯PU而言,随着CNT的直径不断增大,热电导率分别提高了77%、63%和80%。PU/CNT纳米复合材料的玻璃化转变温度同样也随着CNT的直径增大而增大,另外,加入少量的CNT(1wt%)到PU基体中,可以明显地提高其热稳定性。
3.通过酸活化或硅烷偶联剂(KH560和KH570)的表面改性得到了三种改性凹凸棒土,表面处理不影响ATT的晶体结构,经过硅烷偶联剂改性后,硅烷偶联剂包裹在ATT表面。采用不同的凹凸棒土(ATT、acid-ATT、KH560-ATT和KH570-ATT)增强大豆油基PU。结果表明,PU纳米复合材料的储存模量、玻璃化转变温度、拉伸强度和杨氏模量随着ATT的含量增加而不断提高。其中acid-ATT具有最好的增强效应,当填充12wt%的acid-ATT时,PU纳米复合材料的Tg提高了16.8℃,拉伸强度提高了443%,杨氏模量提高了8倍。另外,KH560-ATT和KH570-ATT的加入可以显著提高PU的热稳定性,PU纳米复合材料的热稳定性随着KH560-ATT或KH57O-ATT含量增加而不断提高。
4.通过γ-射线辐照聚合法,聚丙烯酸、聚丙烯酰胺和聚苯乙烯成功接枝到氧化石墨(GO)表面,得到复合物GO-g-PAA、GO-g-PAM和GO-g-PS。复合物GO-g-PAA和GO-g-PAM,热电导率分别为0.44和0.75W／m·K。另外,通过溶剂热法还原GO-g-PS得到聚苯乙烯／石墨烯复合物(G-g-PS),复合物中聚苯乙烯的接枝量高达81.3%,复合物具有优异的热稳定性,起始降解温度可以达到381.5℃。该复合物可以作为纳米填料,制备高性能聚合物纳米复合材料。
With the problem of environmental protection and petroleum-based resources exhaustion have been paid increasing attention, the study on preparation environment friendly polymer derived from renewable resources has become the focus of attention. In the present paper, biodegradable and biocompatible soy-based polyol was used as soft segment of polyurethane (PU). Polyurethane acrylates were prepared by acrylation of polyurethane. Hydroxyl-fuctionalized carbon nanotubes (CNT) and surface modified attapulgite (ATT) were used as fillers to prepared PU/CNT and PU/ATT nanocomposites. The structure-property relationships were studied. It has very important theoretical and practical significance to broaden the apply field of polyurethane materials. Moreover, graphite oxide (GO) and graphene were organic modified via radiation-induced graft polymerization to improve the dispersion in polymer matrix.
1. Three polyols based on ESO were prepared by oxirane ring opening with methanol, glycol, and1,2-propanediol. Polyurethane acrylates (PUAs) were prepared by the reaction of these polyols with isophorone diisocyanate (IPDI) and hydroxyethylacrylate (HEA) by a thermal polymerization process. The acrylated reaction between PU and HEA could significantly increase the crosslinking density, glass transition temperature, damping properties, thermal stability and mechanical properties of PUs. Furthermore, those properties of PUs and PUAs increased with the increasing of OH number. It should be noted that the PUA248appeared as a rigid plastic with the tensile strength higher than40MPa and the Young's modulus of724MPa. The soy-based PUAs could be employed for green, inexpensive, biodegradable materials in insulating material field.
2. Three different diameters of hydroxyl-functionalized CNTs were used to reinforce the soy-based PU matrix. The aim was to find structure-property relationships within neat PU and PU/CNT nanocomposites. The results revealed that the larger diameter CNTs more easily dispersed in the PU matrix than the smaller diameter ones, which easily formed irreversible agglomerates. Covalent functionalizing of CNTs is the most effective method to improve load transfer efficiency. However, our experiment demonstrated that CNT dispersion in the polymer matrix was a more important factor in the production of superior CNT-based nanocomposites. The tensile strength and Young's modulus of PU nanocomposites enhanced with the increase of CNT diameter. As compared with neat PU, with the increase of CNT diameter, the thermal conductivity of PU nanocomposites was improved by77,63and80%, respectively. The glass transition temperature of PU nanocomposites also increased with the increase of CNT diameters. Furthermore, adding small amounts (1wt%) of CNTs to the PU matrix significantly improved its thermal stability.
3. The different ATTs were obtained by acid-activated or silane coupling agents (KH560and KH570) modification. Surface treatment of ATTs did not change its crystal structure. The ATT fibers were coated with silane coupling agents after surface modification. Four types of ATT (neat ATT, acid-ATT, KH560-ATT and KH570-ATT) were used to reinforce the soy-based PU matrix. The storage moduli, glass transition temperature, tensile strength and Young's modulus of PUs significantly increased with the increase of ATT contents. The acid-ATT has the best reinforce effect with12wt% acid-ATT loading,16.8℃improvement in glass transition temperature,443%increment in tensile strength,8-fold increase in Young's modulus of PU nanocomposites were obtained. Furthermore, with the incorporation of KH560and KH570modified ATT, the thermal stability of PU nanocomposites was significantly improved with the increase of ATT content.
4. Poly(acrylic acid)(PAA), poly(acrylamide)(PAM) and polystyrene (PS) successfully grafted GO via y-ray radiation-induced graft polymerization. The result hybrids were named as GO-g-PAA, GO-g-PAM and GO-g-PS, respectively. The thermal conductivities of GO-g-PAA and GO-g-PAM were0.44and0.75W/m-K, respectively. Moreover, GO-g-PS was reduced by solvothermal method to prepare PS/graphene hybrid. The hybrid has higher than81.3%grafted PS and excellent thermal stability with initial decomposition temperature of381.5℃. It could be used as nanofiller to prepare superior polymer nanocomposites.
引文
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