植物油基丙烯酸油酸甲酯的合成和表征

以植物油基环氧油酸甲酯(EMO)为原料,舍成功能性高分子单体丙烯酸油酸甲酯(AMO).通过红外光谱和核磁共振图谱研究表明,AMO分子中具有明显的丙烯酸基的特征吸收峰.通过差示扫描量热仪测试分析,AMO的玻璃化转变温度(Tg)为-82℃.研究了不同反应时间和催化剂对反应的影响,表明N,N二甲基甲苄胺比三苯基膦更适合EMO催化加成AMO.将AMO和甲基丙烯酸甲酯单体聚合,可以制备出低粘、可剥离压敏胶.     

微波辐射乳液聚合制备聚氰基丙烯酸正丁酯磁性微球

通过化学共沉淀法制备Fe3O4纳米粒子,再用油酸钠和十二烷基磺酸钠(SDS)对Fe3O4进行改性,制得稳定的水基磁流体。在自制的磁流体存在下,以氰基丙烯酸正丁酯(BCA)为单体,用微波辐射乳液聚合的方法制备了Fe3O4/聚氰基丙烯酸正丁酯磁性微球。并用X射线衍射仪(XRD),透射电子显微镜(TEM),傅立叶红外光谱仪(FT-IR),振动样品磁强计(VSM)对制备的磁性高分子微球的结构形貌和磁性能进行表征测试。结果表明,在适当的pH值条件下,得到了粒径为150 nm~200 nm,饱和磁化强度为20.23 emμ/g,粒径均一的聚氰基丙烯酸正丁酯磁性微球。     

丙烯酸-2-丙烯酰胺基-2-甲基丙磺酸-滤渣高吸水性树脂的制备

以N,N-亚甲基双丙烯酰胺为交联剂,过硫酸钾-亚硫酸氢钠为引发剂,丙烯酸(AA)和2-丙烯酰胺基-2-甲基丙磺酸(AMPS)为单体,采用水溶液聚合法合成了丙烯酸-2-丙烯酰胺基-2-甲基丙磺酸-滤渣高吸水性树脂.考察了交联剂、引发剂、单体的质量比、AA中和度、反应温度、滤渣含量对树脂吸水率的影响.经正交实验制得的高吸水性树脂在24h内吸水达到饱和,吸蒸馏水1397g/g,自来水330g/g,0.225moL/L NaCl溶液79g/g.该树脂具有一定的耐盐性.     

ATRP法合成聚羧酸类高效减水剂

以对苯乙烯基磺酸钠和丙烯酸钠嵌段共聚物(PSStNa-b-PAANa)为大分子引发剂,甲基丙烯酸甲酯为单体,采用原子转移自由基聚合(ATRP)方法,制备对苯乙烯基磺酸钠、丙烯酸钠和甲基丙烯酸甲酯三嵌段共聚物(PSStNa-b-PAANa-b-PMMA),并通过酯交换方法在聚合物分子上接枝聚乙二醇单甲醚(MPEG)以得到...     

粒状聚(丙烯酸-丙烯酸钠)钙基复合膨润土的制备与吸附性能

用悬浮乳液法以膨润土为主要原料,丙烯酸为聚合单体,司班80(Span 80)作为分散剂,环己烷为分散介质,过硫酸钾为引发剂,N,N-亚甲基双丙烯酰胺为交联剂制备了粒状聚(丙烯酸-丙烯酸钠)钙基复合膨润土吸附剂。以丙烯酸(钠)单体溶出量和Cd2+吸附量为目标函数,对粒状复合膨润土制备进行单因素优化实验,确定适宜合成条件为聚合温度70℃、聚合时间3 h、有机相环己烷与司班80(Span 80)体积比52.5∶2.5、油水比100∶15,其中水相为膨润土、丙烯酸、氢氧化钠与水的混合物。通过X射线衍射、红外光谱和扫描电镜对产品进行表征分析,对共聚反应机理进行了讨论。结果表明:粒状复合膨润土制备过程中,丙烯酸和丙烯酸钠插层进入到膨润土层间,在层间发生了聚合反应,并且没有破坏原土的基本结构。复合膨润土对Pb2+、Cd2+、F-吸附性能优于钙基膨润土。     

淀粉基吸水树脂的制备与性能分析

以淀粉、丙烯酸(AA)和丙烯酰胺(AM)为原料,采用过硫酸铵[(NH_4)_2S_2O_8]作为引发剂,利用N,N-亚甲基双丙烯酰胺(NMBA)进行交联,采用水溶液聚合法制备了AA-AM共聚淀粉吸水树脂。考察了丙烯酸溶液pH、丙烯酸单体用量、引发剂及交联剂用量、反应体系温度与时间对合成树脂性能的影响。通过性能测试和分析得出优化合成条件为:丙烯酸溶液pH=5.5,丙烯酸单体与葡萄糖剩基(AGU)摩尔比为7∶1,过硫酸铵用量为0.35mmol,交联剂用量为0.08571mmol,反应时间为65℃,反应温度为3h。在优化工艺下合成的树脂吸收蒸馏水、0.9%NaCl溶液量分别达到798.6g/g和95.7g/g。采用红外光谱(FT-IR)和热重分析(TG)对合成的树脂进行了表征与分析评价。     

聚偏氟乙烯接枝3-苯基丙烯酸的改性研究

以过氧化对苯二甲酰(BPO)为引发剂,3-苯基丙烯酸为单体,在N,N-二甲基甲酰胺溶液中引发接枝聚合,制得接枝3-苯基丙烯酸的聚偏氟乙烯.通过红外测试、差示扫描量热仪以及热失重分析表明3-苯基丙烯酸(CA)接枝到PVDF骨架上.通过接触角测试,发现改性后的聚偏氟乙烯(PVDF-g-P(CA))的接触角由88°降低到54...     

含氟聚丙烯酸酯功能材料的制备与性能研究

以十二烷基硫酸钠(SDS)和聚乙二醇-400(PEG-400)为乳化剂,采用半连续乳液聚合法制备了丙烯酸六氟丁酯(HFBA)-丙烯酸丁酯(BA)-甲基丙烯酸甲酯(MMA)共聚物乳液,考察了丙烯酸丁酯与甲基丙烯酸甲酯摩尔比对乳液所成薄膜力学性能及耐水性的影响,并优化了丙烯酸六氟丁酯的用量。结果表明,薄膜的抗张强度随BA与MMA摩尔比的减小而增大,耐水性增强,但断裂伸长率降低;薄膜的耐水性随着氟单体用量的增大而增强。SEM-EDS显示含氟组分易向薄膜-空气界面迁移;接触角测定结果表明加入氟单体后薄膜表面与水的接触角增大。     

聚(苯乙烯-丙烯酸)磁性高分子微球的制备及性能

以苯乙烯为单体、丙烯酸为功能基单体、N,N′-亚甲基双丙烯酰胺为交联剂,加入自制的纳米Fe3O4磁流体,采用分散聚合的方法制备出聚(苯乙烯-丙烯酸)磁性高分子微球。采用XRD、FT-IR、SEM、752N型分光光度计和化学滴定法,对所制得的磁性高分子微球进行了表征及性能分析,研究了交联剂N,N′-亚甲基双丙烯酰胺的加入对其性能的影响。结果表明,所制磁性微球粒径在0.7μm~2 m之间,单分散性好;交联剂对微球性能有着明显的影响,随着交联剂的增加,微球粒径变小、粒径分布变宽、表面羧基含量增加、耐酸碱性增强,最佳含量应为单体用量的4%。     

GMA改性超支化聚合物的合成及在光致抗蚀剂中的应用

通过巯基链转移支化聚合法,以4-乙烯基苄硫醇(VBT)为支化单体,丙烯酸正丁酯(BA)、苯乙烯(St)、丙烯酸(AA)为共聚单体,偶氮二异丁腈(AIBN)为引发剂,丙二醇甲醚醋酸酯(PMA)为溶剂,合成了HBPs。利用甲基丙烯酸缩水甘油酯(GMA)环氧基与HBP羧基的反应,向HBP中引入双键制备了具有碱溶性和光固化特性的G-HBP。采用FT-IR、1H-NMR、DSC、凝胶色谱(GPC)-激光光散射(LS)-示差黏度(DV)三检测仪表征了聚合物的结构及性能,验证了其超支化结构;将合成的G-HBP用作负性光致抗蚀剂的主体树脂,测试了光致抗蚀剂显影成像过程参数。结果表明,显影时间为40 s,去膜时间为30 s,感度级数为7级。抗蚀剂性能优异,分辨率可达到40μm。     

Nickel-cobalt nanoparticles supported on single-walled carbon nanotubes and their catalytic hydrogenation activity

Single-walled carbon nanotubes were synthesized from graphite using the arc discharge technique. A nickel/yttrium/graphite mixture was used as the catalyst. After purification by sonication in a Triton X-100 solution, nickel-cobalt metal nanoparticles were deposited on the surface of the single-walled carbon nanotubes. The resulting material and/or the nanotubes themselves were characterized by physisorption, Raman spectroscopy, high-resolution transition electron microscopy and X-ray diffraction. Raman spectroscopy indicates that the nanotubes, prepared by the arc discharge technique, are semi-conducting with a diameter centering at 1.4 nm. The average nickel-cobalt particle size is estimated to be in the region of 8 nm. The catalytic activity of the material was examined for the hydrogenation of unsaturated fatty acid methyl esters obtained from avocado oil. The carbon nanotube supported nickel-cobalt particles effectively hydrogenate polyunsaturated methyl linoleate to monounsaturated methyl oleate. In contrast to a conventional nickel on kieselghur catalyst, further hydrogenation of methyl oleate to undesired methyl stearate was not observed.     

Synthesis and growth mechanism of iron oxide nanowhiskers

Iron oxide nanowhiskers with dimensions of approximately 2 × 20 nm were successfully synthesized by selectively heating an iron oleate complex. Such nanostructures resulted from the difference in the ligand coordination microenvironments of the Fe(III) oleate complex, according to our electronic structure calculations and thermogravimetric analysis. A ligand-directed growth mechanism was subsequently proposed to rationalize the growth process. The formation of the nanowhiskers provides a unique example of shape-controlled nanostructures, offering additional insights into nanoparticle synthesis.     

油酸亚锡的合成及其摩擦磨损性能

有机酸的锡盐一般具有低毒,甚至没有毒性,且无腐蚀等特点,因而有望作为润滑油添加剂得到应用,但它们的合成一般均采用含氯的无机锡盐作为原料,因而产品中往往因为含有氯离子而导致对摩擦副的腐蚀.本文以油酸和氧化亚锡为原料合成了油溶性的油酸亚锡,并利用红外光谱和原子发射光谱对其结构进行了表征.用四球摩擦磨损试验机考察了油酸亚锡在26号白油中的摩擦学性能,对其与硫系和磷系添加剂的复配效果进行了考察.结果表明,油酸亚锡作为润滑油添加剂具有良好的抗磨、减摩性能和一定的承载能力;油酸亚锡与磷酸三甲苯酚酯和硫化异丁烯添加剂有良好的协同作用.磨斑的表面分析表明,油酸亚锡添加剂在摩擦表面形成了含锡的化学反应膜.     

A new approach for preparation of oil-soluble bimetallic dispersed catalyst from layered ammonium nickel molybdate

A new route via the coating of layered ammonium nickel molybdate with oleic acid was developed to prepare an oil-soluble bimetallic dispersed catalyst for the hydrocracking reaction of heavy oil. The layered ammonium nickel molybdate, termed Ni-LTM precursor, was synthesized by precipitation, and the NiMo oleate complex was prepared with the oleic acid serving as an organic ligand. The prepared materials were characterized with X-ray diffraction, Fourier transform infrared spectroscopy and X-ray photoelectron spectroscopy. It was found that the oleic acid is chemisorbed as a carboxylate onto the Ni-LTM nanoparticles, specifically on Ni-O bond. Also, the catalytic activities were compared between the NiMo oleate complex and other ordinary monometallic dispersed catalysts. The NiMo oleate complex showed excellent catalytic activity, demonstrating its potential to be applied as a novel dispersed catalyst.     

Ag_2S纳米粒子的合成与表征

以油酸钠为表面活性剂、硝酸银和硫脲为反应物,在甲苯-水两相界面处合成了Ag_2S纳米粒子。采用紫外-可见吸收光谱(UV-Vis)、透射电子显微镜(TEM)和广角X射线衍射(WAXD)等方法对Ag_2S纳米粒子的光学性质、形貌及晶体结构进行了表征。结果表明,通过改变甲苯-水两相界面反应体系的条件,可以得到粒子尺寸窄分布的Ag_2S纳米粒子;WAXD测定表明所合成的Ag_2S纳米粒子具有单斜结构。     

Study of the properties of polymers obtained from vegetable oil derivatives by light scattering techniques

Polymers from oleic acid (principal fatty acid of the olive oil) and methyl oleate were studied by static (SLS) and dynamic (DLS) light scattering in acetone solution. The oleic acid (OA) and methyl oleate (MO) were first epoxidized using a performic acid generated in situ. The epoxidized oleic acid (EOA) and methyl oleate (EMO) were reacted with cis-1,2-cyclohexanedicarboxylic anhydride (CH) as cure agent, triethylamine (TEA) as initiator and small amount of 1,4-butanediol diglycidyl ether (BDGE). According to light scattering results the EMO products without BDGE present low M_W, however the EOA ones are characterized by aggregation and M_W approximately 1.98 × 10⁵ g/mol. The aggregation is evidenced by the presence of two modes in DLS experiments. The dimension of the single particle is approximately R_h = 5 nm and for the aggregates R_h increases until 169 nm. The samples with addition of BDGE in the reaction mixtures for both derivatives (EMO and EOA) result to macromolecular products with M_W higher than 1.71 × 10⁵ g/mol, however no aggregation of this macromolecules is observed. Both products present relatively small dimensions and random coil conformation behavior.     

Synthesis, structure, and properties of large surface area Fe3O4/SiO2 nanocomposites

This paper describes procedures for the template synthesis of magnetically controlled, large surface area Fe₃O₄/SiO₂ nanocomposites using sodium oleate as a template. The structure and magnetic properties of the nanocomposites have been investigated in relation to SiO₂ content and the way in which sodium oleate had been added to the solution. The largest specific surface area (up to 400 m²/g) was reached when the nanocomposites were fabricated using magnetic fluids. The synthesized materials were tested as adsorbents.     

曼尼希碱复配缓蚀剂的酸洗缓蚀性能

为减少曼尼希碱用量并保证其缓蚀效果,以甲醛、苯乙酮和有机胺为原料合成了曼尼希碱主剂,通过正交试验,将其与十二烷基酚聚氧乙烯醚(OP-10)和油酸钠(SO)进行复配,在20%HCl介质中研究了其对Q235碳钢的缓蚀效果并对复配条件进行了优化。采用失重法、电化学方法、大气采样中和滴定法对复配缓蚀剂的性能进行对比分析,并考察不同温度对复配缓蚀剂性能的影响。确定的复配缓蚀剂最佳配方为:0.70%曼尼希碱,0.10%OP-10,0.20%SO。结果表明,经过复配的缓蚀剂缓蚀效果和抑雾效率均比单独添加曼尼希碱有明显的提高,在60℃20%HCl中,曼尼希碱质量分数为0.5%时,Q235钢的腐蚀速率为1.58g/(m2.h),缓蚀率达到99.31%,抑雾率为80.53%;本复配缓蚀剂是以抑制阳极为主的混合型缓蚀剂,具有良好的耐高温性能。     

Esr study of the migration of paramagnetic additives from rigid PVC to pure or mixed fatty esters used as food simulators

The ESR study presented here provides an insight into the behaviour of paramagnetic additives in rigid PVC before, during and after contact with methyl fatty esters and their migration from the plastic material. Before contact, diffusion processes took place in rigid PVC. The mobility of the NO group of the paramagnetic additives is directly linked to the displacement of the whole molecule. Methyl fatty esters plasticize the PVC matrix, increase the mobility of the additive in the material and enhance their migration. The increased lability is due to methyl ester penetration into the polymeric network. Penetration was greatest with short chain esters and probe migration was greater when more penetrating simulators were used. If a fast migration test is required, methyl oleate could be an interesting approach. Results describing the behaviour of binary mixtures as simulators are very complex, probably because they depend to a large extent on the type of paramagnetic additive.     

甲基有机硅树脂的无溶剂合成研究

以甲基三乙氧基硅烷单体和二甲基二乙氧基硅烷单体为原料,采用水解-缩聚的方法合成了甲基有机硅树脂,并研究了无溶剂合成甲基有机硅树脂的条件。结果表明,一定配比,水解温度为70℃,缩聚温度为80～85℃,反应时间为4h,可合成无溶剂体系的甲基有机硅树脂;红外光谱(IR)表明,合成的甲基有机硅树脂在Si-O-Si处有较宽的吸收峰;固化温度为140℃,固化4h,得到无色透明甲基有机硅树脂。