ABS树脂高性能化制备技术及其中间体的新应用研究
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摘要
ABS树脂是由丙烯腈、丁二烯和苯乙烯三种单体共聚组成的一种橡胶增韧热塑性材料,其微观结构为聚丁二烯(PB)橡胶粒子分散相均匀地分散在苯乙烯-丙烯腈树脂(SAN)连续相之中。ABS树脂在我国虽早已实现了大规模工业化生产,但是,随着科学技术的快速发展和材料工业的不断进步,人们对ABS树脂的高性能化和低成本化的技术需求不断加强,因此,研究开发高性能ABS树脂的新技术和新应用具有十分重要的意义。
本文对ABS树脂的技术概况、双峰分布ABS的技术进展、板材级ABS树脂的技术特点、ABS树脂抗氧化的技术需求和基于ABS中间体的球形聚合物刷的制备方法与应用概况进行了总结。主要研究工作包括：(1)采用双种子乳液接枝聚合技术制备了双峰分布ABS树脂,并与单峰分布ABS树脂进行了性能比较；(2)采用三种工艺路线制备了高抗冲、高熔体粘度板材级ABS树脂,研究了接枝率、接枝链长度和橡胶相含量等对ABS树脂冲击强度、拉伸强度、熔融指数和微观形态结构等的影响；(3)采用受阻酚类抗氧剂Irganox1076和Irganox245分别与硫酯类抗氧剂DLTP复配,研究了抗氧剂在ABS树脂中的稳定作用和协同效应；(4)以ABS中间体聚丁二烯(PB)乳胶粒子为核制备了球形聚电解质刷,并以其为纳米反应器制得Ni、Co、Ag纳米贵金属催化剂,采用对硝基苯酚还原成对氨基苯酚的模型反应研究了其催化活性。主要研究结果如卜：
(1)所制备的双峰分布ABS树脂(HL-ABS)展示出比单峰分布ABS树脂(L-ABS)更加优异的性能,并在超大粒径聚丁二烯胶乳(H-PBL,575nm)比例为10.0%时性能达到最佳：当保持相同橡胶含量时,HL-ABS具有比L-ABS更高的冲击强度和几乎相当的拉伸强度；保持相同的冲击强度,HL-ABS比L-ABS具有更高的拉伸强度,且需要橡胶含量更少；采用两种不同粒径的橡胶粒子作为橡胶相,打破了L-ABS固有的韧性和刚性的平衡性限制；大小两种橡胶粒子的协同效应是双峰分布ABS树脂HL-ABS拥有比L-ABS更好性能的本质原因。
(2)采用双峰分布ABS粉料(HL-PB-g-SAN)与SAN-32共混的工艺路线(以H-PBL和320nm大粒径PBL (L-PBL)的混合胶乳为基础胶乳,合成双峰分布ABS接枝粉料,然后与高腈SAN-32树脂熔融共混),当PB含量为18.5%时,冲击强度、拉伸强度、断裂伸长率和熔体粘度等四项指标可完全满足板材级ABS树脂性能指标要求,所制备的板材级ABS树脂加工性能良好,并成功应用于冰箱内胆的生产
(3)抗氧剂Irganox245和DLTP复配后产生强协同效应,可高效地阻止ABS树脂的热氧老化,而抗氧剂Irganox1076和DLTP复配后的抗氧化效果和Irganox1076单独使用时的效果相当,只产生比较弱的协同作用,其稳定作用介于高效抗氧剂和低效抗氧剂之间。
(4)以PB胶乳为核成功制得球形聚丙烯酸刷(PB-PAA),其粒径较PB胶乳核明显增大,且粒径分布窄；PB-PAA刷的厚度随丙烯酸的用量增加而增大,并且随环境中pH值的增大而增大并在pH值为7以后达到最大值；其厚度还随盐浓度增加而变小并且在超过一定盐浓度后发生团聚；PB-PAA刷的接枝密度可以通过改进后的Daoud-Cotton模型进行估算；以球形PB-PAA刷为载体和纳米反应器所制备的Ni、Co、Ag三种纳米金属催化剂均具有较高的催化活性,催化效率均随着贵金属纳米粒子负载量和反应温度的增加而增大。
ABS resin is a rubber-toughened thermoplastic material which was polymerized by three kinds of monomers:acrylonitrile (AN), styrene (ST) and butadiene (BD). The typical micro structure of ABS resin was shown as which rubbery polybutadiene (PB) particles were uniformly dispersed into the continuous phase of poly (ST-co-AN)(SAN). With the rapid development of science and material industry, the requirement for production of higher performance and lower cost of ABS resin is increased continuously even though massive industrialization production of ABS resin has been achieved in China. Therefore, the research and development of high performance ABS resin made great sense.
In this thesis, the technological survey of ABS resin, the technological progress of ABS resin with bimodal distribution of rubber particles, the technological features of panel grade ABS resin, and the technological requirements of ABS resin in preventing thermal-oxidative aging, as well as the preparation and application of spherical polyelectrolyte brushes based on ABS intermediate were summarized. The main research works were:(1) ABS resins with bimodal distribution of rubber particles were prepared by bi-seeded emulsion grafting copolymerization, and their performance was compared with those with unimodal distribution of rubber particles.(2) Panel grade ABS resin with high impact resistance and high melt viscosity was prepared by three process routes. The effects of grafting ratio, grafting chain length and rubber phase content on impact strength, tensile strength, melt index and micromorphology of ABS resin were investigated.(3) Hindered phenol antioxidants, Irganox1076and Irganox245, were combined with thioester antioxidant DLTP, respectively. The stabilization and synergistic effect of the antioxidant on ABS resin were investigated.(4) Spherical polyelectrolyte brushes were synthesized by using ABS intermediate polybutadiene (PB) colloidal particles as core. With the brush as a nanoreactor, nanoparticles of Ni, Co and Ag were obtained and being used as catalysts to catalyze the model reduction reaction of p-nitrophenol into p-aminopheno.
The main results were showed as follows:
(1) The bimodal distribution ABS resin (HL-ABS) displayed better performance than unimodal distribution one (L-ABS). HL-ABS achieved the best performance at large-sized PB colloidal particles (H-PBL,575nm) ratio of10.0%. Keeping the same rubber content, HL-ABS had higher impact strength than L-ABS and almost the same tensile strength. Keeping the same impact strength, HL-ABS had higher tensile strength with less rubber content compared to L-ABS. The L-ABS intrinsic equilibrium restriction of toughness and rigidity was overcome by using two different size rubber particles for the rubbery phase, and the synergistic effect of the large and the small rubber particles was the essential reason why bimodal distribution ABS resin HL-ABS displays higher performance than L-ABS.
(2) Panel grade ABS resins were prepared successfully by the process route (Treating mixed rubber particles of H-PBL and320nm large-sized PBL (L-PBL) as basic rubber particles, blending ABS grafting powder with bimodal distribution of rubber particles (HL-PB-g-SAN) with SAN-32). When PB content was18.5%, all the performance including impact strength, tensile strength, breaking elongation and melt index could match the property requirements of panel grade ABS resin, and the resulted panel grade ABS resin product was applied successfully to refrigerator internal bladder with favorable processing performance.
(3) The combination of Irganox245and DLTP showed much better stabilization effect than the individual components due to the strong synergistic effect. Only weak synergism could be observed in the combination of Irganox1076and DLTP. Irganox1076and Irgnox1076/DLTP exhibited similar behaviors between antioxidants with the highest and lowest efficiencies.
(4) The particle size of the synthesized spherical polyelectrolyte brushes (PB-PAA brush) with PB as core was obviously larger than that of its core, and the particle size distribution of PB-PAA brush was narrow. The PB-PAA brush thickness could be controlled by adjusting the amount of acrylic acid (AA), and it varied regularly with pH and salt concentration in solution. Emulsion concentration, grafting density, polymer chain length and so on had obviously influence on the stability of PB-PAA brush. Catalysts of Ni, Co and Ag nanoparticles which prepared and loaded in spherical PB-PAA nano-reactors possessed relatively high catalytic activity, and their catalytic efficiency increased with the rise of capacity of metal nanoparticles and the temperature.
本文对ABS树脂的技术概况、双峰分布ABS的技术进展、板材级ABS树脂的技术特点、ABS树脂抗氧化的技术需求和基于ABS中间体的球形聚合物刷的制备方法与应用概况进行了总结。主要研究工作包括：(1)采用双种子乳液接枝聚合技术制备了双峰分布ABS树脂,并与单峰分布ABS树脂进行了性能比较；(2)采用三种工艺路线制备了高抗冲、高熔体粘度板材级ABS树脂,研究了接枝率、接枝链长度和橡胶相含量等对ABS树脂冲击强度、拉伸强度、熔融指数和微观形态结构等的影响；(3)采用受阻酚类抗氧剂Irganox1076和Irganox245分别与硫酯类抗氧剂DLTP复配,研究了抗氧剂在ABS树脂中的稳定作用和协同效应；(4)以ABS中间体聚丁二烯(PB)乳胶粒子为核制备了球形聚电解质刷,并以其为纳米反应器制得Ni、Co、Ag纳米贵金属催化剂,采用对硝基苯酚还原成对氨基苯酚的模型反应研究了其催化活性。主要研究结果如卜：
(1)所制备的双峰分布ABS树脂(HL-ABS)展示出比单峰分布ABS树脂(L-ABS)更加优异的性能,并在超大粒径聚丁二烯胶乳(H-PBL,575nm)比例为10.0%时性能达到最佳：当保持相同橡胶含量时,HL-ABS具有比L-ABS更高的冲击强度和几乎相当的拉伸强度；保持相同的冲击强度,HL-ABS比L-ABS具有更高的拉伸强度,且需要橡胶含量更少；采用两种不同粒径的橡胶粒子作为橡胶相,打破了L-ABS固有的韧性和刚性的平衡性限制；大小两种橡胶粒子的协同效应是双峰分布ABS树脂HL-ABS拥有比L-ABS更好性能的本质原因。
(2)采用双峰分布ABS粉料(HL-PB-g-SAN)与SAN-32共混的工艺路线(以H-PBL和320nm大粒径PBL (L-PBL)的混合胶乳为基础胶乳,合成双峰分布ABS接枝粉料,然后与高腈SAN-32树脂熔融共混),当PB含量为18.5%时,冲击强度、拉伸强度、断裂伸长率和熔体粘度等四项指标可完全满足板材级ABS树脂性能指标要求,所制备的板材级ABS树脂加工性能良好,并成功应用于冰箱内胆的生产
(3)抗氧剂Irganox245和DLTP复配后产生强协同效应,可高效地阻止ABS树脂的热氧老化,而抗氧剂Irganox1076和DLTP复配后的抗氧化效果和Irganox1076单独使用时的效果相当,只产生比较弱的协同作用,其稳定作用介于高效抗氧剂和低效抗氧剂之间。
(4)以PB胶乳为核成功制得球形聚丙烯酸刷(PB-PAA),其粒径较PB胶乳核明显增大,且粒径分布窄；PB-PAA刷的厚度随丙烯酸的用量增加而增大,并且随环境中pH值的增大而增大并在pH值为7以后达到最大值；其厚度还随盐浓度增加而变小并且在超过一定盐浓度后发生团聚；PB-PAA刷的接枝密度可以通过改进后的Daoud-Cotton模型进行估算；以球形PB-PAA刷为载体和纳米反应器所制备的Ni、Co、Ag三种纳米金属催化剂均具有较高的催化活性,催化效率均随着贵金属纳米粒子负载量和反应温度的增加而增大。
ABS resin is a rubber-toughened thermoplastic material which was polymerized by three kinds of monomers:acrylonitrile (AN), styrene (ST) and butadiene (BD). The typical micro structure of ABS resin was shown as which rubbery polybutadiene (PB) particles were uniformly dispersed into the continuous phase of poly (ST-co-AN)(SAN). With the rapid development of science and material industry, the requirement for production of higher performance and lower cost of ABS resin is increased continuously even though massive industrialization production of ABS resin has been achieved in China. Therefore, the research and development of high performance ABS resin made great sense.
In this thesis, the technological survey of ABS resin, the technological progress of ABS resin with bimodal distribution of rubber particles, the technological features of panel grade ABS resin, and the technological requirements of ABS resin in preventing thermal-oxidative aging, as well as the preparation and application of spherical polyelectrolyte brushes based on ABS intermediate were summarized. The main research works were:(1) ABS resins with bimodal distribution of rubber particles were prepared by bi-seeded emulsion grafting copolymerization, and their performance was compared with those with unimodal distribution of rubber particles.(2) Panel grade ABS resin with high impact resistance and high melt viscosity was prepared by three process routes. The effects of grafting ratio, grafting chain length and rubber phase content on impact strength, tensile strength, melt index and micromorphology of ABS resin were investigated.(3) Hindered phenol antioxidants, Irganox1076and Irganox245, were combined with thioester antioxidant DLTP, respectively. The stabilization and synergistic effect of the antioxidant on ABS resin were investigated.(4) Spherical polyelectrolyte brushes were synthesized by using ABS intermediate polybutadiene (PB) colloidal particles as core. With the brush as a nanoreactor, nanoparticles of Ni, Co and Ag were obtained and being used as catalysts to catalyze the model reduction reaction of p-nitrophenol into p-aminopheno.
The main results were showed as follows:
(1) The bimodal distribution ABS resin (HL-ABS) displayed better performance than unimodal distribution one (L-ABS). HL-ABS achieved the best performance at large-sized PB colloidal particles (H-PBL,575nm) ratio of10.0%. Keeping the same rubber content, HL-ABS had higher impact strength than L-ABS and almost the same tensile strength. Keeping the same impact strength, HL-ABS had higher tensile strength with less rubber content compared to L-ABS. The L-ABS intrinsic equilibrium restriction of toughness and rigidity was overcome by using two different size rubber particles for the rubbery phase, and the synergistic effect of the large and the small rubber particles was the essential reason why bimodal distribution ABS resin HL-ABS displays higher performance than L-ABS.
(2) Panel grade ABS resins were prepared successfully by the process route (Treating mixed rubber particles of H-PBL and320nm large-sized PBL (L-PBL) as basic rubber particles, blending ABS grafting powder with bimodal distribution of rubber particles (HL-PB-g-SAN) with SAN-32). When PB content was18.5%, all the performance including impact strength, tensile strength, breaking elongation and melt index could match the property requirements of panel grade ABS resin, and the resulted panel grade ABS resin product was applied successfully to refrigerator internal bladder with favorable processing performance.
(3) The combination of Irganox245and DLTP showed much better stabilization effect than the individual components due to the strong synergistic effect. Only weak synergism could be observed in the combination of Irganox1076and DLTP. Irganox1076and Irgnox1076/DLTP exhibited similar behaviors between antioxidants with the highest and lowest efficiencies.
(4) The particle size of the synthesized spherical polyelectrolyte brushes (PB-PAA brush) with PB as core was obviously larger than that of its core, and the particle size distribution of PB-PAA brush was narrow. The PB-PAA brush thickness could be controlled by adjusting the amount of acrylic acid (AA), and it varied regularly with pH and salt concentration in solution. Emulsion concentration, grafting density, polymer chain length and so on had obviously influence on the stability of PB-PAA brush. Catalysts of Ni, Co and Ag nanoparticles which prepared and loaded in spherical PB-PAA nano-reactors possessed relatively high catalytic activity, and their catalytic efficiency increased with the rise of capacity of metal nanoparticles and the temperature.
引文
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