溶剂法制备碳纳米管结合胶及其微观结构的研究

利用溶剂法制备碳纳米管结合胶,确定了制备高质量碳纳米管结合胶的实验参数：橡胶／甲苯溶液的质量浓度为0．020g／mL,橡胶与碳纳米管的质量比为4：1,反应时间为7h。用扫描探针显微镜对天然橡胶、碳纳米管及其结合胶的微观形貌进行研究,得到了碳纳米管结合胶的清晰结构。碳纳米管结合胶的结构为天然橡胶分子在定向紧密排列的碳纳米管的两侧沿着纳米管的表面与碳纳米管结合形成环状的闭合结构,随着纳米管管径的增大,结合胶的结构趋向于炭黑结合胶的结构。     

结合胶的制备及微观形貌研究

利用溶剂法、炭黑(DZ13)制备结合胶,结果表明:当橡胶和炭黑的质量比为2∶1、炭黑粒径一定时,橡胶/甲苯溶液的质量浓度为0.02g/mL,反应时间为10h时制得的结合胶量最大;相对分子质量高的橡胶制得的结合胶质量分数更高。用扫描探针显微镜(SPM)对天然橡胶、丁苯橡胶(SBS)、炭黑以及SBS结合胶的微观形貌进行研究。结果表明,将SBS和炭黑混合物溶解后进行分离,对分离物观察能看到结合胶的微观形貌。     

混炼工艺对SBR/BR/白炭黑胶料性能的影响

研究混炼工艺对丁苯橡胶（SBR）/顺丁橡胶（BR）/白炭黑胶料物理性能和结合胶含量的影响。对于一次投胶混炼法,橡胶对白炭黑的润湿效果好,胶料的拉伸强度和结合胶含量大于分段投胶混炼法胶料。对于分段投胶混炼法,用贫相橡胶控制结合胶时,胶料的拉伸强度和结合胶含量较大;结合胶含量受生胶种类和并用比以及混炼工艺的共同影响;2种生胶的用量越接近,越容易形成结合胶,形成结合胶的白炭黑表面越大;混炼工艺引起的混炼场差异影响结合胶的生成。     

瞬时增加橡胶结合胶含量的方法及制备的橡胶制品

正授权公告号:CN 104292523B授权公告日:2016年2月17日专利权人:怡维怡橡胶研究院有限公司发明人:王玉海、张琳、刘震等本发明涉及瞬时增大橡胶结合胶含量的方法及橡胶制品的制备。增大橡胶结合胶含量的方法如下:将橡胶与炭黑混炼,制成炭黑母胶,或将橡胶、炭黑和偶联剂混炼,制成炭黑母胶;用电子束对炭黑母胶进行辐照,然后将辐照后的炭黑母胶与补强填充剂、防老剂、硫化剂和油混炼,制成混     

全配方湿法连续混炼工艺的研究

针对炭黑与橡胶混炼难度大以及传统干法混炼工艺繁琐、产生粉尘污染等问题,研究全配方（补强填料包括炭黑和白炭黑）湿法连续混炼工艺。结果表明：全配方湿法连续混炼工艺分为4个阶段,分别为补强填料和小料水分散体的制备、炭黑母胶的制备、白炭黑母胶的制备、连续混炼;全配方湿法连续混炼工艺从初期补强填料和小料水分散体的研磨到后期的连续混炼均促进了炭黑在橡胶基体中的分散,使硫化胶的物理性能和动态力学性能比传统干法混炼工艺硫化胶明显提高,同时避免了干法混炼工艺的粉尘飞扬的问题,可实现胶料的清洁化、连续化生产。     

加工配方及工艺对溶聚丁苯橡胶/白炭黑复合材料性能的影响

采用不同加工工艺及配方,制备了溶聚丁苯橡胶(SSBR)/白炭黑复合材料,考察了硅烷偶联剂、白炭黑、橡胶加工工艺及配方对复合材料性能的影响。结果表明,排胶温度和时间对SSBR/白炭黑复合材料的动态力学性能及白炭黑分散性影响显著。升高排胶温度和延长混炼时间均能提高SSBR/白炭黑复合材料的抗湿滑性能、降低滚动阻力,但过高的排胶温度和过长的混炼时间易引起橡胶基体降解。SSBR/白炭黑复合材料的最佳排胶温度为160℃,混炼时间为7 min。随着混合填料中炭黑用量的增加,混炼胶的门尼黏度无明显变化,硫化胶的力学性能增强、抗湿滑性能下降、滚动阻力增加。     

SSM法和传统炼胶工艺生产的胎面胶料性能对比

随着胎面胶配方中白炭黑的大量应用,采用传统法炼胶工艺进行大用量白炭黑混炼是比较困难的,生产出的终炼胶炭黑、白炭黑分散度较差。SSM法炼胶工艺可以提高胶料的机械剪切效率,使炭黑、白炭黑和各种配合剂分散更均匀,有效地避免胶料混炼过程中产生的炭黑、白炭黑凝胶,以及由此引发的胶料黏度下降、压延和挤出等后序加工不便等问题;减少橡胶分子链不可逆化学裂解的发生,增加可逆机械剪切分子链的数量;提高炭黑的补强作用,提升轮胎硫化后的物理性能。     

硫酸法制备饲料级磷酸氢钙无脱氟工艺研究

用硫酸浸取磷矿,通过改变工艺参数和实验条件,在不添加除氟剂的条件下,制备了低氟含量的饲料级磷酸氢钙。探讨了反应温度、反应时间、加酸量、静置时间、中和终点pH,搅拌转速等因素对产品中氟含量的影响。结果表明,在磷矿粉用量40 g的情况下,优化的工艺条件为：反应温度80℃,浓硫酸20 mL,反应时间3 h,静置时间2.5 h,中和终点pH 6.0,搅拌转速400 r/min。在此条件下制备出的磷酸氢钙中氟的质量分数至0.07%,低于0.18%的行业标准。     

串联式连续混炼设备用于炭黑配方胶料低温混炼的实验研究

本文根据低温混炼原理,将自主研发设计的串联式连续混炼机用于炭黑配方胶料的低温混炼,不仅实现了块状橡胶的连续混炼、保证了基体胶和配合剂配比的准确性,同时保证了混炼温度低于135℃,保留了橡胶大分子链的完整性,经实验验证:与密炼机高温混炼相比,串联式连续混炼设备采用低温法制备的炭黑配方胶料分散度高、综合物理机械性能好。同时,通过实验探究了串联式连续混炼设备中下游连续混炼机转子转速对于混炼胶质量的影响,结果表明:当连续混炼机转子转速为30rpm时,所制备的胶料性能最好。     

改性木质素绿色化学湿法混炼对橡胶与橡胶助剂性能的提升

从秸秆中清洁分离木质素,并对木质素进行甲基化改性和相容性改性,研究改性木质素绿色化学湿法混炼对橡胶与橡胶助剂性能的影响。结果表明：用改性木质素以绿色湿法混炼工艺制备的生物橡胶可提高轮胎胶料的粘合性能、耐磨性能和耐老化性能;用改性木质素以绿色湿法混炼工艺制备的生物基炭黑母胶、生物基白炭黑母胶、生物基碳纳米管母胶可提高轮胎胶料的性能;木质素改性氧化锌和癸酸钴可分别等量替代未改性氧化锌和癸酸钴用于轮胎胶料中,可以减量增效和降低成本。本技术有利于提升国产NR性能并实现秸秆高值化利用。     

橡塑合金改性沥青制备工艺关键参数研究

为了合理、有效地利用废旧橡胶粉和废旧塑料并改善两者与沥青的相容性,采用精密开炼机预先将两种废旧材料熔融共混,制备成橡塑（质量）比分别为5∶5（Ⅰ型）、6∶4（Ⅱ型）、和7∶3（Ⅲ型）3种橡塑合金改性剂。按照正交试验方案对伦特70^#基质沥青进行改性,制备橡塑合金改性沥青,以橡塑合金改性沥青的48 h离析软化点、25 ℃针入度、软化点和5 ℃延度为指标,筛选橡塑合金改性沥青的最佳复配方案,并通过灰色关联度分析法和极差分析法确定制备工艺最佳的关键参数。最后通过扫描电子显微镜、布氏旋转黏度试验、BBR试验和DSR试验对橡塑合金改性沥青的结构形态、流变性能、低温抗裂性能和抗疲劳性能进行了分析。结果表明：最佳复配方案为外掺20 %（相较于基质沥青质量）橡塑比为7∶3（Ⅲ型）的橡塑合金、2 %增溶剂（糠醛抽出油）和9 %稳定剂（硫磺）,制备的橡塑合金改性沥青储存稳定性和高温稳定性良好,推荐制备工艺的最佳关键参数为剪切温度180 ℃、剪切速率3 500 r/min、剪切时间1.5 h和发育时间0.5 h;橡塑合金改性剂与沥青的相容性好,制备的橡塑合金改性沥青具有较低的温度敏感性,较好的低温抗裂性和抗疲劳性能。     

丙烯酸丁酯原位改性白炭黑/天然橡胶复合材料的研究

丙烯酸丁酯单体(BA)在适量的引发剂作用下与白炭黑(WC)表面和橡胶分子上同时发生接枝反应,采用乳液共沉法制备改性白炭黑填充型天然橡胶复合材料(NR/WC/BA).实验结果表明复合材料有良好的加工流动性、力学性能和耐老化性能.     

异戊烷溶剂体系合成稀土异戊橡胶聚合工艺的研究

进行了异戊烷溶剂体系合成稀土异戊橡胶聚合工艺的研究。考察了催化剂用量、温度、单体质量浓度和时间对异戊二烯（IP）聚合反应和聚合物结构的影响,确定了异戊烷溶剂体系聚合工艺条件：每克IP催化剂用量（1．5～2．0）×10-8mol,聚合温度50℃,p（IP）=10g／dL,聚合时间3h。制备的异戊烷溶剂体系的稀土畀戊橡胶产品质量与己烷溶剂体系的相当,达到了国外同类产品水平。     

Preparation of carbon black/natural rubber latex masterbatch in bead form

Carbon black/natural rubber latex masterbatch in the form of spherical beads was prepared according to the acid-precipitation method. High-loading carbon black (40 phr) was incorporated in natural rubber with the aid of a nonionic surfactant (Nonidet P40). Shearing the beads in an internal mixer provided good integration of carbon black in the rubber matrix and hence the high bound rubber content. Results confirmed the contribution of chemical interaction to the bound rubber content. By an oxidation process, the size of modified carbon black was reduced, whereas the large agglomeration took place in the case of partially graphitized carbon black. © 2001 John Wiley & Sons, Inc. J Appl Polym Sci 82: 489–498, 2001     

Effect of bound rubber on characteristics of highly filled styrene–butadiene rubber compounds with different types of carbon black

Viscosity and cure time of a filled rubber compound having an accelerated sulfur cure system are affected by types and contents of the rubber and the filler as well as of the curatives. Bound rubber content is used as level of the reinforcement. Influence of bound rubber on viscosity and cure time of a rubber compound was studied using highly filled styrene–butadiene rubber compounds with carbon black having different structures. The bound rubber content increases with increase of the carbon black content and also increases as the carbon black structure is developed. The Mooney viscosity increases linearly with increase of the bound rubber content irrespective of the carbon black structure when the primary particle size of carbon black is nearly the same. The Mooney scorch time decreases linearly with increase of the bound rubber content irrespective of the carbon black structure. © 2004 Wiley Periodicals, Inc. J Appl Polym Sci 93: 1001–1006, 2004     

Structure and properties of hollow carbon black and filled rubber nanocomposites

Abstract

Hollow carbon black (HCB) is introduced in this work. It has a special hollow structure, high specific surface area, high structure and high electric conductivity. Hollow carbon black is used to fill styrene–butadiene rubber (SBR). The bound rubber test results show that the bound rubber of SBR/HCB can be measured when the HCB content reaches 25 phr because a strong filler network is formed, which indicates good electric conductivity of SBR/HCB. In comparison, the bound rubber of SBR/N330 can not be measured even when the N330 content is 40 phr. The mechanical measurements show that HCB has very good reinforcing effect on SBR especially when the filler content is low. The electric conductivity and thermal conductivity increase with the increase in filler content. At the same filler content, the properties of SBR/HCB nanocomposites are better than those of SBR/N330 nanocomposites, which suggests that HCB has good application potential.     

HTV硅橡胶生胶挥发分的快速测定

为了缩短测试甲基乙烯基硅橡胶生胶挥发分的时间,将常压恒温干燥箱烘烤改为真空干燥烘箱烘烤。考察了称样量、烘箱温度、烘烤时间、真空度对测试结果的影响,并与传统的电热恒温干燥箱法测试数据进行对照;验证了此法的精密度、再现性和稳定性。结果表明,较佳测试条件是:取样量为2.0~2.5 g、相对真空度(表压)为-0.09 MPa、烘箱温度150℃、恒温时间40 min,在此条件下测试的甲基乙烯基硅橡胶生胶挥发分数据与采用常规检测方法测得的数据比较吻合,精密度、再现性较好,且测试时间比常规检测方法缩短2 h。     

The effects of filler content on cure and mechanical properties of dichlorocarbene modified styrene butadiene rubber/carbon black composites

A study has been carried out on the curing characteristics and mechanical properties of carbon black filled dichlorocarbene modified styrene butadiene rubber (DCSBR). Processing characteristics such as optimum cure time and maximum torque increases with increasing of the concentration of carbon black in DCSBR whereas scorch time decreases. The mechanical properties and resistance of the vulcanizate towards thermal, flame and oil resistance have been carried out. Variation of bound rubber content of carbon black filled DCSBR and the influence of the extracting temperature on the bound rubber content was investigated and its activation energy was calculated from the Arrhenius plot. The reinforcing nature of the filler was assessed from stress strain and swelling data. The enhancement in mechanical properties was supported by data on the increased content of crosslink density in these samples obtained from swelling and stress strain analysis. The results of the studies indicate that carbon black can be used as a good reinforcing filler for DCSBR.