石墨/可发性聚苯乙烯的合成工艺及性能研究
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摘要
随着我国节能减排策略的深入,作为保温材料的可发性聚苯乙烯(EPS)板材备受人们的关注。保温材料EPS具有低导热系数、有一定的强度和韧性、可规模化成型、工艺成熟以及施工便利等优点。为了进一步降低导热系数,德国巴斯夫公司经过10年的不懈努力和研发,首先推出了石墨/可发性聚苯乙烯(Graphite/Expandable Polystyrene,G-EPS)复合材料,并在2010年推向市场,但其合成工艺技术保密,以此控制低导热系数G-EPS市场。因此,如何利用现有EPS的大生产工艺来制备出低导热系数的G-EPS是本论文的主要研究内容。
第二章主要采用苯乙烯单体溶胀法,实现了线性低密聚乙烯(LLDPE)与苯乙烯单体的悬浮共聚合的工艺。阐述了LLDPE对PS的增韧改性机理,对不同配比的LLDPE与苯乙烯单体进行比较实验,确定了LLDPE与苯乙烯不同配比的最佳工艺条件,获得了分散性好、粒度分布均匀的增韧聚苯乙烯粒子(PS)。通过IR、SEM、DSC表征,考察了LLDPE加入量对聚合过程的接枝效率、成球率、粒子的形貌、平均粒径、粒度分布和共聚物玻璃化转变温度等性质的影响。
第三章主要是寻找一种便利的石墨改性工艺,使得改性石墨在苯乙烯单体中有良好分散性。本章通过石墨在苯乙烯单体中的沉降实验,详细讨论了石墨的种类和粒径的影响;对石墨改性工艺中溶剂的选择进行了讨论,并对改性前后石墨在水中、单体、水和单体混合液中的分散稳定性进行表征,结果表明改性后的石墨和苯乙烯有良好的相容性。通过改变改性石墨不同加入顺序,用扫描电镜(SEM)分析了合成工艺中加入顺序对石墨在苯乙烯中分散性的影响。此外对石墨改性工艺中的设备进行了设计并投入了工业化生产,实现了年产800吨改性石墨的大生产工艺,从而为合成G-EPS提供基础和保证。
第四章是在改性石墨的基础上,研究了一步法制备石墨/可发性聚苯乙烯(Graphite/Expandable Polystyrene,G-EPS)复合粒子的中试工艺,制备了黑色度均匀的G-EPS。本章详细讨论了水油比对G-EPS聚合反应体系粘度的影响;石墨添加量对G-EPS的粒径分布、分子量的变化进行了讨论;并研究了引发剂浓度对G-EPS的分子量和反应周期的影响;利用扫描电镜(SEM)对G-EPS原粒、泡粒进行了形貌分析;对G-EPS泡沫的导热系数和阻燃性能进行了测定,并对G-EPS具有低导热系数和高阻燃性从机理上进行了初步探讨。
第五章研究了一步法制备石墨/可发性聚苯乙烯(Graphite/Expandable Polystyrene,G-EPS)复合粒子的工业化大生产工艺。主要解决了以下几方面的问题:优化了工业化生产试验的工艺参数及工艺流程;优化了工业化生产设备的选型和设计,实现了年产9万吨G-EPS的大生产工艺;将工业化生产的产品送到国家权威部门作性能测试,并在保温材料生产厂家做各种性能检验;综合分析了工业化生产G-EPS的经济效益。
本论文主要研究了石墨改性的工业化大生产工艺和石墨/可发性聚苯乙烯复合材料合成的中试和大生产工艺,并对产品的性能进行系统的研究。打破了德国巴斯夫和韩国锦湖等公司对低导热系数G-EPS市场的垄断地位,拥有了国内自主研发的技术,填补了国内G-EPS生产技术的空白。
Along with our country energy-saving and emission-reduction strategy deeply, expandable polystyrene (EPS) board as thermal insulation material has some advantages, attracted much people's attention. Thermal insulation materials EPS has a low thermal conductivity coefficient, a certain strength and toughness, forming easily, mature technology and so on. In order to further reduce the thermal conductivity, after 10 years hard work, BASF of Germany firstly pushed out Graphite/Expandable Polystyrene (G-EPS) composite material to the market in 2010, but the process of synthesis is still confidential, in order to control the market of the low thermal conductivity of G-EPS. Therefore, how to use existing production process of EPS to prepare a low coefficient of thermal conductivity of G-EPS is the main research content of this paper.
The second chapter realizes the suspension polymerization of linear low density polyethylene (LLDPE) and styrene monomer using styrene monomer swelling method. The toughening modification mechanism adout LLDPE to PS is expatiated. The optimum process conditions for different ratios of LLDPE and styrene monomer were compared and identified. The polystyrene particles (PS) with symmetrical particle size distribution are obtained.The effect of LLDPE quantity added on the grafting polymerization efficiency ,the ball ratio,particle morphology, average particle size, particle size distribution and the copolymer glass transition temperature properties has been studied by IR, SEM and DSC.
In the third chapter, the main purpose is to find a convenient graphite modified process, which can make the modified graphite disperse well in styrene monomer. The effect of graphite type and particle size is discussed in detail by the sedimentation experiment of the graphite in styrene monomer, and the solvent of modifying graphite are selected. In addition, the dispersing stability of modified graphite in water, monomer and the mixture of monomer and water were characterized. The results show that the modified graphite and styrene has good compatibility. The effect of adding order of modified graphite on its dispersion in styrene are examined by SEM. Furthermore, the equipment of modifying graphite process was designed and put into industrial production. A modified graphite production process of annual output 800 tons is set up, which can provide a basis and guarantee for the synthesis of G-EPS.
In the fourth chapter, based on the modified graphite, one-step preparation process of graphite/polystyrene is studied, and composite particles with the black uniform G-EPS are prepared. In this chapter the effect of the water-oil ratio of G-EPS polymerization reaction system on viscosity and graphite addition quantity on the G-EPS particle size distribution are discusseed detailedly. The effects of initiator concentration on the molecular weight of G-EPS and reaction cycle changes are also discussed. The morphology of G-EPS original and foam tablets are analized using the scanning electron microscope (SEM) .Thermal conductivity and flame resistant properties determined, and the mechanism of G-EPS with low thermal conductivity and high flame retardant from are discussed.
In the fifth chapter, the one-step preparation manufacturing process of composite graphite/expandable polystyrene (G-EPS) particles is investigated. The main problems solved in this chapter are as follows: Process parameters, production process as well as equipment in industrial production are optimized, a production process of G-EPS with annual output of 90,000 tons is achieved, and performances of the industrial products are tested by both national authorities and manufacturers of insulation materials. Moreover, the economic benefits of industrial production of G-EPS are analysed integratively.
The studies are focused on different processes, such as the manufacturing process of modified graphite, the pilot process and the manufacturing process of composite graphite/expandable polystyrene (G-EPS). Performances of the industrial products are evaluated systematically. Fourthermore, the production technology of G-EPS is self-developed, which filled the void of domestic industry. As a result of this breakthrough, the monopoly position of BASF and South Korea Kumho Group in low thermal conductive G-EPS market is broken.
第二章主要采用苯乙烯单体溶胀法,实现了线性低密聚乙烯(LLDPE)与苯乙烯单体的悬浮共聚合的工艺。阐述了LLDPE对PS的增韧改性机理,对不同配比的LLDPE与苯乙烯单体进行比较实验,确定了LLDPE与苯乙烯不同配比的最佳工艺条件,获得了分散性好、粒度分布均匀的增韧聚苯乙烯粒子(PS)。通过IR、SEM、DSC表征,考察了LLDPE加入量对聚合过程的接枝效率、成球率、粒子的形貌、平均粒径、粒度分布和共聚物玻璃化转变温度等性质的影响。
第三章主要是寻找一种便利的石墨改性工艺,使得改性石墨在苯乙烯单体中有良好分散性。本章通过石墨在苯乙烯单体中的沉降实验,详细讨论了石墨的种类和粒径的影响;对石墨改性工艺中溶剂的选择进行了讨论,并对改性前后石墨在水中、单体、水和单体混合液中的分散稳定性进行表征,结果表明改性后的石墨和苯乙烯有良好的相容性。通过改变改性石墨不同加入顺序,用扫描电镜(SEM)分析了合成工艺中加入顺序对石墨在苯乙烯中分散性的影响。此外对石墨改性工艺中的设备进行了设计并投入了工业化生产,实现了年产800吨改性石墨的大生产工艺,从而为合成G-EPS提供基础和保证。
第四章是在改性石墨的基础上,研究了一步法制备石墨/可发性聚苯乙烯(Graphite/Expandable Polystyrene,G-EPS)复合粒子的中试工艺,制备了黑色度均匀的G-EPS。本章详细讨论了水油比对G-EPS聚合反应体系粘度的影响;石墨添加量对G-EPS的粒径分布、分子量的变化进行了讨论;并研究了引发剂浓度对G-EPS的分子量和反应周期的影响;利用扫描电镜(SEM)对G-EPS原粒、泡粒进行了形貌分析;对G-EPS泡沫的导热系数和阻燃性能进行了测定,并对G-EPS具有低导热系数和高阻燃性从机理上进行了初步探讨。
第五章研究了一步法制备石墨/可发性聚苯乙烯(Graphite/Expandable Polystyrene,G-EPS)复合粒子的工业化大生产工艺。主要解决了以下几方面的问题:优化了工业化生产试验的工艺参数及工艺流程;优化了工业化生产设备的选型和设计,实现了年产9万吨G-EPS的大生产工艺;将工业化生产的产品送到国家权威部门作性能测试,并在保温材料生产厂家做各种性能检验;综合分析了工业化生产G-EPS的经济效益。
本论文主要研究了石墨改性的工业化大生产工艺和石墨/可发性聚苯乙烯复合材料合成的中试和大生产工艺,并对产品的性能进行系统的研究。打破了德国巴斯夫和韩国锦湖等公司对低导热系数G-EPS市场的垄断地位,拥有了国内自主研发的技术,填补了国内G-EPS生产技术的空白。
Along with our country energy-saving and emission-reduction strategy deeply, expandable polystyrene (EPS) board as thermal insulation material has some advantages, attracted much people's attention. Thermal insulation materials EPS has a low thermal conductivity coefficient, a certain strength and toughness, forming easily, mature technology and so on. In order to further reduce the thermal conductivity, after 10 years hard work, BASF of Germany firstly pushed out Graphite/Expandable Polystyrene (G-EPS) composite material to the market in 2010, but the process of synthesis is still confidential, in order to control the market of the low thermal conductivity of G-EPS. Therefore, how to use existing production process of EPS to prepare a low coefficient of thermal conductivity of G-EPS is the main research content of this paper.
The second chapter realizes the suspension polymerization of linear low density polyethylene (LLDPE) and styrene monomer using styrene monomer swelling method. The toughening modification mechanism adout LLDPE to PS is expatiated. The optimum process conditions for different ratios of LLDPE and styrene monomer were compared and identified. The polystyrene particles (PS) with symmetrical particle size distribution are obtained.The effect of LLDPE quantity added on the grafting polymerization efficiency ,the ball ratio,particle morphology, average particle size, particle size distribution and the copolymer glass transition temperature properties has been studied by IR, SEM and DSC.
In the third chapter, the main purpose is to find a convenient graphite modified process, which can make the modified graphite disperse well in styrene monomer. The effect of graphite type and particle size is discussed in detail by the sedimentation experiment of the graphite in styrene monomer, and the solvent of modifying graphite are selected. In addition, the dispersing stability of modified graphite in water, monomer and the mixture of monomer and water were characterized. The results show that the modified graphite and styrene has good compatibility. The effect of adding order of modified graphite on its dispersion in styrene are examined by SEM. Furthermore, the equipment of modifying graphite process was designed and put into industrial production. A modified graphite production process of annual output 800 tons is set up, which can provide a basis and guarantee for the synthesis of G-EPS.
In the fourth chapter, based on the modified graphite, one-step preparation process of graphite/polystyrene is studied, and composite particles with the black uniform G-EPS are prepared. In this chapter the effect of the water-oil ratio of G-EPS polymerization reaction system on viscosity and graphite addition quantity on the G-EPS particle size distribution are discusseed detailedly. The effects of initiator concentration on the molecular weight of G-EPS and reaction cycle changes are also discussed. The morphology of G-EPS original and foam tablets are analized using the scanning electron microscope (SEM) .Thermal conductivity and flame resistant properties determined, and the mechanism of G-EPS with low thermal conductivity and high flame retardant from are discussed.
In the fifth chapter, the one-step preparation manufacturing process of composite graphite/expandable polystyrene (G-EPS) particles is investigated. The main problems solved in this chapter are as follows: Process parameters, production process as well as equipment in industrial production are optimized, a production process of G-EPS with annual output of 90,000 tons is achieved, and performances of the industrial products are tested by both national authorities and manufacturers of insulation materials. Moreover, the economic benefits of industrial production of G-EPS are analysed integratively.
The studies are focused on different processes, such as the manufacturing process of modified graphite, the pilot process and the manufacturing process of composite graphite/expandable polystyrene (G-EPS). Performances of the industrial products are evaluated systematically. Fourthermore, the production technology of G-EPS is self-developed, which filled the void of domestic industry. As a result of this breakthrough, the monopoly position of BASF and South Korea Kumho Group in low thermal conductive G-EPS market is broken.
引文
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