热缩聚法制备包覆沥青的基础研究

包覆沥青对提高锂离子电池负极材料的性能起到重要作用。以乙烯渣油沥青为原料,通过常压热缩聚法制备包覆沥青。考察了反应温度、反应时间对包覆沥青的基础指标(软化点、甲苯不溶物、喹啉不溶物和结焦值)和光学显微结构的影响。研究结果表明：以N₂作为保护气体,当热缩聚反应温度为390℃,反应时间为4 h的条件下,制备出了软化点为200℃,甲苯不溶物为35.47%,喹啉不溶物为1.11%,结焦值为67%的各向同性沥青。通过FTIR和TGA分析可知,乙烯渣油沥青和高软化点各向同性沥青的芳香性指数(Iar)分别为0.526 6和0.5377,在700℃热解残余质量分别为20.22%和50.79%。表明乙烯渣油沥青通过热缩聚处理后得到的高软化点各向同性沥青具有较高的芳香性和良好的热稳定性,是一种优质的包覆沥青。     

利用煤系软沥青制备包覆沥青的研究

随着锂离子电池的高速发展,石墨负极电化学性能的提高至关重要.对天然石墨的包覆改性可有效改善石墨负极电化学性能.煤系软沥青来源广泛、价格低廉,是制备包覆沥青的优质原料.介绍了一种以煤系软沥青为原料制备包覆沥青的方法并对试验过程中的影响因素进行讨论研究,制备出的包覆沥青可有效改善石墨负极的电化学性能,提供了一种制备包覆沥青...     

聚苯乙烯接枝包覆硫黄微胶囊的制备与表征

以合成硫黄为芯材、聚苯乙烯(PS)为壳材,采用原位接枝改性聚合方法制备PS接枝包覆硫黄微胶囊,分析不同苯乙烯/硫黄颗粒配比对硫黄微胶囊形貌的影响,表征接枝状况和热稳定性。结果表明,当硫黄颗粒用量不变、苯乙烯用量为1.5 mL时,硫黄微胶囊的表面形貌规整,分散性较好,热稳定性提高。     

超临界条件下辽河稠油高软化点沥青颗粒的制备

在梯级分离实验装置上,以正戊烷为溶剂,在压力为4.0～7.0 MPa、温度为155～170℃的条件下,讨论压力、温度变化对辽河稠油减渣脱油沥青收率、脱油沥青颗粒分布的影响.压力增加,脱油沥青的收率减小;温度升高,脱油沥青的收率增大.随着压力的增加,50、40、30目颗粒的质量分数均减小,大于50目颗粒的质量分数增大.随着温度的升高,50、40、30目沥青颗粒的质量分数均增大,大于50目沥青颗粒的质量分数减小.在所得的颗粒中大于50、50、40、30目脱油沥青颗粒的质量分数依次减小,其中大于50目小颗粒的质量分数大于67%.得到了沥青收率与沥青颗粒分布的关系.随着沥青收率的增加,大于50目小沥青颗粒的质量分数减小,50目与小于50日较大沥青颗粒的质量分数增大.大于50目沥青颗粒质量分数与沥青收率的定量关系为:Y=114.9502-1.7118X,R=0.9585.扫描电镜(SEM)的分析结果表明:造粒得到的沥青颗粒为多孔性颗粒,由团聚形成的不规则较大颗粒和破碎得到的不规则小颗粒组成.     

沥青裂缝自修复微胶囊的制备与表征

为了提高沥青路面自修复性能,采用原位聚合法制备包裹沥青再生剂的脲醛树脂微胶囊,利用四因素三水平正交试验,研究了最佳芯壁比、终点pH、温度与乳化剂浓度对包裹沥青再生剂的脲醛树脂微胶囊形貌、粒径与包覆率的影响;对完整试样和断裂愈合后的试样分别进行延度试验,探究普通基质沥青和添加自修复微胶囊沥青的自修复能力。极差数值分析结果表明：pH和温度对微胶囊制备影响程度更大,制备微胶囊的最佳工艺是甲醛与脲的摩尔比为4：5,芯壁比为6：5,终点pH为4,反应最终温度为70℃,十二烷基苯磺酸钠的质量分数为0.5%,此条件下制备的微胶囊表面形貌致密,平均粒径为21.14μm,包覆率达到85%。在愈合试验中,微胶囊最优质量掺量为0.3%,此时愈合率为38.67%。     

石油沥青合成低软化点、高残炭沥青树脂

两种石油沥青在低温下合成沥青树脂，考察了工艺参数和原料组成对沥青树脂性能的影响。结果表明，大庆石油沥青反应活性适中、含胶质—沥青质较少，可以合成具有软化点(SP)为80～112C、残炭(CY)为59．13％、β树脂(TI～PS)含量为21．19％、喹啉不溶物(QI)值为1．32％、灰分为0．02％的优质沥青树脂，该沥青树脂已能够满足作为浸渍剂的要求。     

净化煤沥青的制备及其性质表征

采用溶剂絮凝法和离心分离法对煤焦油进行净化处理，以净化煤焦油为原料制备了净化煤沥青，比较了净化沥青和未净化沥青的结构性质差异，并研究了两类煤沥青的炭化行为特征。     

改性煤沥青热转化中间相结构性质与表征

采用实验室自制石英管式炉,以中温煤焦油沥青（CTP01）、改性沥青（CTP02）进行热缩聚反应。通过红外光谱（FT-IR）、拉曼（Raman）、X射线衍射法（XRD）、热重（TG/DTG）以及偏光显微镜对CTP01和CTP02在热转化过程中生成的中间相沥青进行了表征分析。结果表明：在反应温度430℃、恒温时间7 h制得中间相沥青,CTP02内部具有排列规整、取向性更好的芳香片层分子,热聚合后明显相对分子质量变大,芳环上的取代基明显增强,稠环芳烃含量增加;CTP01制得中间相沥青光学各向异性含量较低,很难形成稳定的区域型结构,主要以中小区域镶嵌型为主,而CTP02制得中间相沥青光学各向异性含量较高,易形成广域型结构。     

沥青包覆石墨用作锂离子电池负极材料的研究

锂离子电池因其质量轻，能量密度高等优良性能，是近几年来电化学界研究的热点。但锂离子电池用石墨作负极还存在一些问题，需要对石墨改性处理。本文介绍了石墨的一种改性方法：沥青包覆石墨法，可有效降低石墨的比表面积，从而大幅度提高了石墨负极材料的首次可逆容量和库仑效率，改善电池的循环性能等。     

浅色高软化点马来松香季戊四醇酯的制备

以精制松香、马来酸酐和季戊四醇为原料,制备浅色高软化点马来松香季戊四醇酯。重点讨论了不同还原剂、催化剂、减色剂、原料配比及反应时间等因素对产品性能的影响。研究表明最佳合成条件为：马来酸酐、还原剂SHHP、催化剂R-1、减色剂M-6的用量分别为精制松香质量的13%、0.3‰、3‰、3‰,精制松香和马来酸酐加成反应60 min,马来松香和季戊四醇酯化反应150 min,所得产品颜色为加纳色号3号,酸值为9.8 mg/g,软化点为159 ℃。     

沥青软化点对炮泥性能的影响

以矾土、碳化硅、黏土、沥青、焦炭为原料,焦油为结合剂制备了炮泥试样,并研究了沥青软化点(75~145℃)对炮泥可塑性和强度的影响。结果表明:炮泥试样的可塑性不随沥青软化点的增大而呈现有规律的变化,沥青对炮泥可塑性的影响主要由沥青的组成决定;200℃烘干后试样的强度也不随沥青软化点的变化而呈现有规律的变化;但1000、1450℃烧后试样的强度随沥青软化点的升高呈增大趋势;综合考虑,制备炮泥用沥青的软化点以120~160℃为宜。     

Structural characterization of N-containing activated carbon fibers prepared from a low softening point petroleum pitch and a melamine resin

The incorporation of heteroatoms like N in activated carbons is of interest to modify the surface chemistry of the materials and, then, to improve their behavior as catalyst or catalyst support. In this work, N-containing activated carbon fibers have been prepared using a petroleum pitch with a low softening point and an N-containing resin. The novelty of the preparation method is that it involves the steps used in the synthesis of activated carbon fibers, i.e. spinning, stabilization, carbonization and activation. The materials have been characterized with techniques such as XPS and UPS, which allows us to follow the changes in both the chemical state of N species and the valence band structure of the carbon samples during the preparation steps.     

Stabilisation of low softening point petroleum pitch fibres by HNO3

This paper deals with the stabilisation of low softening point pitch fibres obtained from petroleum pitches using HNO₃ as oxidising agent. This method presents some advantages compared with conventional methods: pitches with low softening point (SP) can be used to prepare carbon fibres (CF), the stabilisation time has been reduced, the CF yields are similar to those obtained after general methods of stabilisation, and the initial treatments to increase SP when low SP pitches are used to prepare CF, are avoided. The parent pitches were characterised by different techniques such as diffuse reflectance infrared Fourier transform spectroscopy (DRIFTS), elemental analysis and solvent extraction with toluene and quinoline. The interaction between HNO₃ and the pitch fibres, as well as the changes occurring during the heat treatment, have been followed by DRIFTS.     

一种高效红外吸收和能量转换涂层的制备与表征

采用固相高温烧结法制备一种可以高效吸收和热能转换的红外功能涂层用填料,借助扫描电镜(SEM)和X射线衍射(XRD)对涂层填料的形貌、结构进行表征,系统分析涂层材料的物化性能,并对其在燃气传热过程中的实际节能效果进行验证.结果表明:合成的Fe-Mn-Cu体系红外填料具有较高的发射率,用其制备的红外涂层具有较强的耐酸碱性能、较好的附着能力以及较高的耐冲击强度.红外辐射与吸收的匹配程度对燃气的使用效率有重要影响,在金属Al表面涂覆后,使用普通燃气燃烧器可使燃气使用效率提高10.3%,而与红外燃烧器搭配使用时,燃气使用效率提高21.7%.     

Preparation and characterization of spinnable pitch for general-purpose carbon fiber from refined pitch

Four types of spinnable pitches (MP-N-A, MP-A, MP-A-H, and MP-A-N) for general-purpose carbon fiber have been prepared under certain conditions with the refined pitch as the raw materials. Fourier transform infrared spectrum and solid-state nuclear magnetic resonance spectra combined with curve-fitting analysis have been used to characterize the average molecular structure (I_ar, CH₃/CH₂, S_AR, and S_HFG) of spinnable pitches. Thermogravimetric analyses and polarizing microscope have been used to observe the thermal stability and the microstructure of spinnable pitches, respectively. The X-ray diffraction combined with curve-fitting analysis have showed that, the stacking heights (L_c) of these four kinds of spinnable pitches were 2.21, 1.78, 1.79, and 1.76 nm, respectively. The parallel layers (N) of each spinnable pitch were 7.30, 6.02, 6.06, and 5.97. What is more, the numbers of aromatic ring in each layer (n) were 17.03, 11.61, 11.75, and 11.41. Finally, the scanning electron microscopy has been used to characterize the surface morphology of carbon fibers which obtained by each spinnable pitches. © 2019 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2019 , 136, 47880.     

球状高温沥青生产工艺研究

对影响球状高温沥青质量和产量的各种因素 (如温度、压力、流量等 )进行了研究。开发的球状高温沥青生产工艺合理、投资少 ,产品质量稳定 ,产量和成品率高     

T1ρ study of pitch softening

Proton rotating frame spin-lattice relaxation time (T_1ρ) measurements have been made in 10 samples of pitch from room temperature to 673 K to obtain information about the mechanisms of pitch softening. The T_1ρ minimum of pitch was found to occur at approximately the same temperature as the softening point. This result suggests that the softening phenomenon of pitch can be detected at the molecular level by T_1ρ measurements. Laboratory frame spin-lattice relaxation time (T₁) measurements were also made on pitches to obtain information about the molecular motion of pitch in the high frequency ranges.     

水性近红外吸收涂层的制备及性能表征

以自制WPU(水性聚氨酯)和稀土氧化物Sm_2O_3为原料,采用玻璃棒刮涂法制得了具有近红外吸收特性和良好力学性能的绿色环保型WPU/Sm_2O_3复合涂层,系统研究了固化温度、Sm_2O_3添加量及交联剂对涂层性能的影响规律。研究结果表明:Sm_2O_3添加量对涂层性能影响明显,而固化温度只对涂层的力学性能有所影响;当固化温度为100℃,w(Sm_2O_3)=40%时,涂层对1.06μm近红外光的反射率可低至54.8%。水性交联剂的添加可明显提高涂层的硬度;当w(交联剂)=3%时,涂层的硬度、附着力和抗冲击强度分别可达到3H、1级和50 kJ/m~2,涂层对1.06μm近红外光的反射率略有增加,但仍具有较低的近红外反射率(55.7%)。     

Preparation and characterization of novel waterborne antifouling coating

In this article, a waterborne antifouling coating was prepared using novel synthesized silicone-acrylate emulsion and 2,3-epoxy-2-methyl-1,4-naphthoquinone. The silicone-acrylate emulsion was synthesized using polymerizable co-emulsifiers (4-propyl-1-(1-propenyl) sulfosuccinate (M-10S) and allyl octylphenyl polyoxyethylene glycol ether (AE-200)), and characterized by Fourier transform infrared spectroscopy, differential scanning calorimetry, and transmission electron microscopy micrograph. The particles in the emulsion are all spherical with an average particle size of 66.5?nm. The adhesion of the coating film reaches 1 grade and its impact resistance is over 50?cm?kg. The antifouling activity of the coating film is excellent when the concentration of ME is 6.77?wt%.