双环戊二烯-苯乙烯共聚加氢石油树脂的研究

制备了双环戊二烯-苯乙烯共聚加氢石油树脂,考察了苯乙烯含量、聚合温度、聚合时间等条件对共聚树脂性质的影响,并探究了聚合机理。研究结果表明:通过选择合适的催化剂,实现了双环戊二烯-苯乙烯共聚树脂的选择性加氢,得到软化点为98℃、加德纳色号接近0号、蜡雾点为87℃、浊点为36℃的双环戊二烯-苯乙烯共聚加氢石油树脂。     

苯乙烯改性间戊二烯石油树脂的工艺研究

间戊二烯树脂有许多的优点,但也存在软化点低、蜡雾点高的缺点,限制了其在很多领域里的应用。通过改性可以改善树脂的诸多缺点,在间戊二烯中添加苯乙烯及单烯烃复合改性,可使软化点控制在89-96℃,蜡雾点≤105℃。提高石油树脂的极性,降低石油树脂的色度,改善间戊二烯树脂相容性,使得间戊二烯树脂在热熔胶及热熔压敏胶等领域有所应用。     

液体石油树脂的研发与生产

以异戊烯、α-甲基苯乙烯、α-蒎烯等为主要原料,通过傅克反应合成了高品质的液体石油树脂。考察了反应温度、反应时间、原料配比等对液体石油树脂的影响。确定了聚合最佳工艺条件:m(异戊烯)∶m(α-蒎烯)∶m(抽余C₅)∶m(α-甲基苯乙烯)=360∶72∶96∶72,进料阶段反应温度40℃,反应时间70 min,保温阶段反应温度50℃,反应时间80 min,成品树脂色度(YI)≤35,软化点0～15℃,相对分子质量为600～700。     

浅色低分子量改性碳五石油树脂的生产工艺研究

在实验室考察了碳五直链单烯烃、苯乙烯、α-甲基苯乙烯三种单烯烃对C5石油树脂的改性。采用阳离子聚合工艺以间戊二烯为原料合成了C5石油树脂,对三种改性剂用量对树脂性能的影响进行了分析。结果表明,碳五直链单烯烃作为良好的改性剂可制得色泽较浅的碳五树脂,提高石油树脂的极性,降低石油树脂的色度,改善间戊二烯树脂相容性,所得改性C5石油树脂具有良好的色相、软化点以及优异的相容性能。     

浅色芳烃石油树脂合成工艺的研究

以裂解C9馏分和C9馏分精馏切割后所得的苯乙烯为原料,通过脱色处理,用BF3催化聚合,合成了浅色C9芳烃石油树脂。当脱色苯乙烯和脱色C9原料质量比为3∶1,反应温度为10℃,反应时间为15 h,催化剂用量为2%时,树脂综合性能最好,色度为4号,软化点为105.9℃,且收率为33.5%。     

碳五馏分对碳五石油树脂物理性质的影响

以从碳五(C_(5))馏分中分离出的主要组分间戊二烯、异戊二烯和异戊烯为原料,烷烃和不活泼烯烃为溶剂,无水三氯化铝为催化剂,合成C_(5)石油树脂。研究3种组分用量对C_(5)石油树脂软化点和色度的影响,获得物理性质优异的C_(5)石油树脂的适宜原料用量:间戊二烯24%~32%,异戊二烯≤10%,异戊烯6%~12%。     

苯乙烯、α-甲基苯乙烯改性C5石油树脂的研究

以苯乙烯、α-甲基苯乙烯为改性剂,采用阳离子聚合工艺合成了C5石油树脂,对聚合体系、改性剂等因素进行了分析.结果表明,无水AlCl3是引发C5-苯乙烯共聚体系的理想催化剂;苯乙烯与其余可聚单体的质量比在0.4-0.8,或α-甲基苯乙烯与其余可聚单体的质量比在1.0左右时,所得改性C5石油树脂具有良好的色相、软化点以及优...     

催化加氢合成浅色度C5石油树脂

通过对C5石油树脂的催化加氢,合成了浅色度C5石油树脂,制备并筛选了催化剂,采用固定床反应器对C5石油树脂进行了加氢工艺研究,采用BET、SEM和DTA-TG对催化剂进行了表征,用IR对C5石油树脂加氢前后的结构进行了分析。研究结果表明,Ni基多金属催化剂C5JH-3在原料浓度为20%、温度为220~240℃、压力3.5MPa、空速0.5h-1、氢油比600∶1的条件下对C5石油树脂加氢,可制得软化点高的浅色度树脂。     

裂解C5合成石油树脂研究

介绍了利用乙烯装置裂解C5馏份合成石油树脂的方法，对石油树脂的合成工艺进行了研究。利用自制催化剂A-1，反应温度40℃，苯作溶剂，聚合时间3h时，树脂收率＞50％，软化点85℃以上。     

BF3-AlCl3在C5石油树脂中的应用

裂解乙烯C5馏分含有大量线性不饱和分子和质量分数超过16%的环戊二烯,用BF3做催化剂可以得到浅色石油树脂,但当环戊二烯含量高时一般需先除去,得到的树脂软化点不是很高。本文以乙烯装置副产Ｃ5馏分为原料,考察了BF3与AlCl3质量比、催化剂用量、反应温度对Ｃ5石油树脂软化点及收率的影响。实验结果表明,三氟化硼和无水三氯化铝最佳质量比为7∶3,催化剂总用量占原料总质量的2%,在反应温度为40 ℃,反应时间为4 h时,可得到收率为56.6%（质量分数）,色度为6～7,软化点为101 ℃的浅色C5石油树脂,其直接可用于油墨、橡胶等中。     

石油树脂对热熔胶、压敏胶粘接性能的影响

介绍了石油树脂的分类、增粘树脂的结构特点,国内外热熔胶、压敏胶用石油树脂发展,热熔胶对石油树脂的性能要求;论述了石油树脂与聚合物之间的相客性、石油树脂的软化点、熔融粘度等对热熔胶粘接性能的影响,展望了石油树脂的生产和发展方向.     

双环戊二烯石油树脂高压釜加氢工艺研究

作者主要研究了双环戊二烯石油树脂高压釜加氢工艺。原料为色度(Gardner)10#,软化点130℃,采用BASF催化剂,考察了加氢过程中各种工艺参数的影响,确定了最佳工艺条件:石油树脂质量分数25%~33%,反应温度200~260℃,反应压力(4.0~6.0)MPa,加氢反应时间6~8h,制备出色相低的DCPD加氢石油树脂。     

间戊二烯C5石油树脂的生产应用研究

∶针对间戊二烯石油树脂合成反应,采用了一种DPE/AlCl3均相复合催化体系,实验结果表明,与传统的AlCl3催化剂相比,采用了这种均相复合催化体系可提高间戊二烯石油树脂的收率和软化点,同时可提高树脂的相对分子质量和降低相对分子质量分布,配比为1∶1.5的DPE/AlCl3复合催化体系为较佳的选择。此时制备的间戊二烯树脂平均收率比AlCl3催化剂时的平均收率高出2.8%;DPE/AlCl3复合催化体系得到的间戊二烯树脂软化点明显高于AlCl3引发制备的树脂软化点,平均高出9.8℃。而且此时DPE/AlCl3复合催化体系合成的间戊二烯树脂的相对分子质量高于AlCl3引发制备的树脂,相对分子质量分布低于AlCl3引发制备的树脂。     

C_9热聚石油树脂的研究

以裂解C9中双环戊二烯含量较多的馏分为原料,与裂解C9切出的轻组分按一定比例混合,在一定温度和压力下通过热聚合得到热聚石油树脂。研究了反应温度、反应时间及不同原料配比对树脂性能的影响,确定了适宜的聚合温度、压力、反应时间等工艺条件,制得软化点大于130℃,色度7以下的高品质石油树脂。     

Morphology and Viscoelastic Behavior of Styrene-Diene Block Copolymers in Pressure Sensitive Adhesives

Linear (SDS) and radial (SD)_x block copolymers of styrene (S) and dienes (D=butadiene or isoprene), varying in composition and molecular weight, were formulated as pressure sensitive adhesives. The morphology of these compositions was determined by electron microscopy of ultra-thin sections and dynamic viscoelastic measurements were made at 35 Hz between -90° and + 140°C or higher. Pressure sensitive tack and holding power were determined and interpreted in terms of morphological and rheological properties.

A high degree of tack resulted only when the tackifying resin was compatible with the polydiene segments of the block polymer and incompatible with the polystyrene segments, provided also that the polydiene-tackifier phase was the continuum with the polystyrene phase forming spherical domains. All effective tackifying resins raised the glass transition temperature (T_g) of the rubbery phase, but plasticized the polymer at temperatures well above T_g Polystyrene domain connectivity was found to lead to diminished tack in block polymers containing more than 30% styrene, a result of decreased creep compliance on the time scale of the bonding process and failure to achieve full contact with the substrate. For adhesives not limited by contact, tack increased with the loss modulus of the adhesive on the time scale of the debonding process. Holding power (shear resistance) increased with polymer styrene content and molecular weight, the polystyrene domain structure effectively inhibiting viscous flow at temperatures sufficiently below T_g of the styrene blocks.     

Seepage Characteristics of Emulsion with Phase Transition Behaviors

Petroleum resins have excellent thermal tolerance and selective plugging capability. As the environment temperature exceeds their softening point, petroleum resins transform from a solid into a viscous Newton fluid, accompanied by the transformation of the system from particle dispersoid to emulsion. The presence of phase transition decides that the seepage regularity and plugging characteristics of petroleum resins are different from either particle dispersoid or emulsion. Herein, rheological measurements and physical model flooding experiments were performed to investigate the injection and plugging performance of petroleum resins. A correlation chart of the injection pressure, formation permeability, and the ratio of resin particle size to pore diameter is established. The dispersoid is demonstrated to present good injectivity when the ratio of the resin particle size to the pore-throat diameter of the porous media is lower than 0.35. Moreover, when the environment temperature is lower than or around the petroleum resin softening point, the injection performance of the dispersoid is not affected by temperature. Comparably, while the environment temperature is 30 °C higher than the resin softening point, the injection pressure increases due to phase transition. As indicated by the plugging experiment, the presented petroleum resin dispersoid plugging agent manifests excellent performance even in the case that the permeability of water-channeling paths is up to 20 μm², reaching a water plugging efficiency of over 85%. For water-channeling fractures with widths of 0.05–0.5 mm, the plugging pressure gradient can exceed 5 MPa m⁻¹. As suggested by combined analysis of injection and plugging performance, the disperse system should be optimized in accordance with the formation condition during field practice. Specifically, the ratio of the resin particle size to the formation pore diameter should be kept lower than 0.35, while the softening point of the petroleum resin should be 10–20 °C lower than the formation temperature.     

C_5石油树脂加氢改质的研究

使用抚顺市正川化工厂提供的C5石油树脂,采用含钯质量分数是2.0%,其他金属质量分数是2.0%的实验室自制的加氢催化剂,在GSH型磁力搅拌反应釜中进行间歇加氢反应,最优的工艺条件为:反应温度为280℃、反应压力为4.0 MPa、反应时间为4 h。此时可以得到色度降低3个单位,氢化率为98.5%的加氢C5石油树脂,而其软化点降低仅为8.5℃。可以制得色度在1以下,软化点为91.5℃的无色、无味、稳定性很好的加氢C5石油树脂。     

双环戊二烯石油树脂的合成研究

以双环戊二烯(DCPD)为原料,采用热聚合方法得到粗DCPD石油树脂,然后采用固定床反应装置对粗DCPD石油树脂进行加氢研究,以得到热稳定性优良的加氢石油树脂。确定了热聚合最佳工艺条件:m(双环戊二烯)∶m(环己烷)=1∶1,反应温度为270～275℃,反应时间6～8h,粗品色度(Gardner)10#～12#,软化点为130℃;采用钯催化剂考察了加氢过程中各种工艺参数的影响,最佳工艺条件为∶w(DCPD石油树脂)=20%～25%,反应温度280～290℃,反应压力(5.0～6.0)MPa,空速0.5h-1,V(氢)∶V(油)=300∶1,得到的DCPD加氢石油树脂色度(Gardner)1#,软化点125℃。     

间戊二烯C5石油树脂加氢改质工艺研究

采用含钯质量分数1.0%,其他金属质量分数1.0%的自制催化剂对抚顺市正川化工厂生产间戊二烯C5石油树脂,在高压釜中进行间歇加氢,最佳工艺条件为:反应温度270℃,反应压力3.0 MPa,反应时间4 h。此时制备的加氢间戊二烯树脂色度可以降低5个单位以上,加氢的氢化率可达98.3%,而其软化点降低仅为9.4℃。可以制得色度在1以下、软化点为92.6℃的无色、无味、稳定性很好的加氢间戊二烯石油树脂。