Characterization of polystyrene latexes

Polystyrene latexes were prepared by emulsion polymerization. Styrene was used as monomer, potassium persulfate was the reaction initiator and sodium hydrogen carbonate was used as buffer. Surfactant may or may not be used. Three types of surfactant, ie sodium dodecylbenzene sulfonate (anionic), Triton X‐100 and Vulcastab LW (nonionic), and hexadecyltrimethyl ammonium bromide (cationic), were used. The prepared latexes were characterized according to concentration, density, pH, ionic strength, particle size, particle size distribution and surface charge. For prepared latexes with anionic surfactant, the effects of temperature, initiator concentration, surfactant concentration and amount of monomer on the latex size were investigated. Scanning electron microscopy was used as a tool for latex characterization. The results show that by increasing temperature, initiator and emulsifier concentration, the latex diameter decreases. However, size increases by increasing the amount of monomer. A potentiometric titration technique was employed for determination of surface charge. It was found that for all latexes, surface charge densities are in the same range. © 2000 Society of Chemical Industry     

Concentrated emulsion copolymerization of butyl acrylate and vinyl acetate initiated by a redox initiator at lower temperature

The concentrated emulsion copolymerization of butyl acrylate and vinyl acetate with an ammonium persulfate/sodium hydrogen sulfate mixture as a redox initiator, with a sodium dodecyl sulfate/cetyl alcohol mixture as a compound surfactant, and with poly(vinyl alcohol) as a liquid film reinforcer was carried out at lower temperature. In less than 3 h, the polymerization conversion was greater than 95%. The effects of the surfactant, the initiator, the volume fraction of the monomer, and the temperature on the stability of the concentrated emulsion, the kinetic process, and the average size of the latices were examined. The morphology of the polymer particles was observed by transmission electron microscopy, and the average size and distribution of the particle diameter were measured by photon correlation spectroscopy. The kinetic equation was R_p = k[M]^0.38[I]^0.89[E]^?0.80 at 30°C (where R_p is the polymerization rate, [I] is the initiator concentration, [M] is the monomer concentration, and [E] is the concentration of the compound surfactant), and the apparent activation energy was 22.69 kJ/mol. The thin‐layer polymerization of the concentrated emulsions, which enabled the removal of the heat of polymerization, was performed first. In comparison with test‐tube polymerization, thin‐layer polymerization provided a more regular morphology of the polymer particles. © 2003 Wiley Periodicals, Inc. J Appl Polym Sci 91: 570–576, 2004     

Stability and copolymerization of concentrated emulsion of styrene and butyl acrylate in the presence of polyurethane macromonomer

A study has been made of the stability and copolymerization of concentrated emulsion of styrene (St) and butyl acrylate (BA) in the presence of polyurethane macromonomer (DPUA), which contains C?C at one end. First, the DPUA macromonomer was synthesized from the appropriate amount of 2,4‐diisocyanate (TDI), polypropylene glycol (PPG), 2‐hydroxyethyl methylacrylate (HEMA), dimethylolpropionic acid (DMPA), and triethylamine (TEA) by four steps. Then, the DPUA was dissolved in St‐BA monomer mixtures. The DPUA/St‐BA concentrated emulsion copolymerization using sodium dodecyl sulfate/cetyl alcohol (SDS/CA) as composite surfactant and polyvinyl alcohol (PVA) as liquid film reinforcer, and ammonium persulfate/sodium hydrogen sulfate (APS/SHS) as redox initiator system was carried out at 30°C. The effect of NCO/OH molar ratio, surfactants' concentration, mass ratio of DPUA/St‐BA, initiators' concentration, volume fraction of the monomer phase (Φ), and temperature on the stability or the copolymerization of the concentrated emulsion of DPUA/St‐BA were investigated. The average size and distribution of the latex particles obtained under different conditions were also analyzed. © 2006 Wiley Periodicals, Inc. J Appl Polym Sci 103: 1992–1999, 2007     

Polystyrene latex synthesized in presence of ultrasonic initiation

The low water solubility of styrene (St) monomer increase the need for a good initiator system to speed up the emulsion polymerization and remove unreacted monomers. Polymerization of styrene monomer in water was performed at 30, 50, and 70°C under ultrasonic irradiation using sodium dodecyl sulfate as surfactant and ammonium persulfate as initiator. Ultrasonic energy was used as a tool to speed up the polymerization. Combining ultrasonic and ammonium persulfate led to a higher conversion and higher rate of polymerization. Ultrasonic energy has an effect on the particle size distribution. The particle size distribution increases with an increase in the monomer conversion of styrene for ultrasonic polymerization, whereas the particle size distribution did not change with an increase in the monomer conversion compared with the conventional thermal polymerization results. Higher molecular weights were obtained under ultrasonic irradiation. FE‐SEM and TEM pictures show different morphology with changing temperature polymerization. © 2011 Wiley Periodicals, Inc. J Appl Polym Sci, 2011     

Emulsion polymerization of pentabromobenzyl acrylate: effect of reaction parameters on the produced flame‐retardant nanoparticles

Flame‐retardant nanoparticles of sizes ranging between 33 ± 6 and 460 ± 50 nm were formed by the emulsion polymerization of the pentabromobenzyl acrylate (PBBA) monomer in the presence of sodium dodecyl sulfate as the surfactant and potassium persulfate as the initiator. The effect of various polymerization parameters, e.g. monomer, crosslinker monomer, initiator and surfactant concentrations, on the size, size distribution and polymerization yield of the poly(pentabromobenzyl acrylate) nanoparticles produced has been elucidated. Poly(pentabromobenzyl acrylate)/polystyrene (PPBBA/PS) nanoblends containing 15% and 70% of PPBBA particles of 33 ± 6 and 460 ± 50 nm diameter were prepared by mixing the particles with a PS solution in methylene chloride, followed by evaporation of the methylene chloride from the mixture. The effect of the size and the content of the PPBBA nanoparticles in the nanoblends on the thermal stability of the PS were also elucidated. Copyright © 2011 Society of Chemical Industry     

Synthesis of cationic flocculants by the inverse microemulsion copolymerization of acrylamide with 60% 2‐acryloxyethyltrimethyl ammonium chloride in the monomer feed. I. Initiation by ammonium persulfate/sodium disulfite redox system

Acrylamide/2‐acryloxyethyltrimethyl ammon‐ium chloride copolymers in inverse microemulsion, with a cationic charge density of 60% and a concentration of active matter of 30 wt %, of interest as flocculants have been obtained by inverse microemulsion copolymerization. Interesting inverse microemulsion formulations from both industrial and economical standpoints were selected from pseudoternary phase diagrams. These formulations were polymerized by semicontinuous free radical copolymerization in inverse microemulsion using sodium disulfite and ammonium persulfate as initiators. Influence of initiators and initiator addition conditions (specific flow rate and concentration) on semicontinuous polymerization and final product properties as flocculants have been studied. A strong difference in copolymer solution viscosity has been found when an aqueous solution of sodium disulfite is used as initiator instead of sodium disulfite/ammonium persulfate couple redox, specially for low sodium disulfite solution feeding flow. © 2006 Wiley Periodicals, Inc. J Appl Polym Sci 103: 2826–2836, 2007     

新型酸液稠化剂的制备与性能评价

酸化处理是油气井增产增注的重要措施之一,而其中稠化剂是酸液中一种重要的酸性添加剂.文章中以二甲基二烯丙基氯化铵（DMDAAC）和丙烯酰胺（AM）为原料,过硫酸铵-亚硫酸氢钠为引发剂,采用水溶液聚合制备共聚物PDA（（Poly DMDAAC-AM）.实验考察了单体配比、总单体质量分数和引发剂用量等反应条件对共聚物特性粘数和单体转化率的影响.结果表明,经红外检测AM和DMDAAC发生了聚合,单体配比n（AM）∶n（DMDAAC）=8∶2,单体总质量分数为20％,引发剂用量为过硫酸铵和亚硫酸氢钠各占单体总质量的0.04％,最高单体转化率为67.70％,最佳特性粘数为505.59 mL/g.实验采用石油工业标准（SY/T6214-1996）对产品性能进行了评价,结果表明产品性能优良,可用作酸液稠化剂.     

Synthesis of nanosized poly(ethyl acrylate) particles via differential emulsion polymerization

Nanoparticles of poly(ethyl acrylate) were synthesized via a semibatch differential emulsion polymerization method with potassium persulfate as the initiator and sodium dodecyl sulfate as the surfactant. The effects of the reaction temperature, aging time, and surfactant/initiator/monomer ratios on the polymer particle sizes were investigated. Poly(ethyl acrylate) with particle sizes of less than 20 nm was synthesized under mild conditions. © 2006 Wiley Periodicals, Inc. J Appl Polym Sci 102: 1609–1614, 2006     

引发剂对纤维素接枝丙烯酰胺反应的影响

分别以硝酸铈铵、过硫酸钾和过硫酸钾/亚硫酸钠为引发剂,以马尾松漂白硫酸盐浆纸浆纤维素为骨架接枝丙烯酰胺,在单体浓度为0.75 mol/L、温度为45℃、反应时间为3 h时,得到硝酸铈铵和过硫酸钾的最佳浓度为3.0 mmol/L和5.0 mmol/L,过硫酸钾/亚硫酸钠在用量为6%时的最佳质量比为1.5,三者相应的接枝率分别为40%、48%和60%。同时比较了不同条件下三种引发剂的接枝效果,结果表明,过硫酸钾/亚硫酸钠的接枝效果最好,但均聚物含量高;硝酸铈铵作为引发剂虽然接枝效果不及前两者,但均聚物含量很低。     

乳液聚合法合成高相对分子质量聚醋酸乙烯酯的研究

采用过硫酸铵/亚硫酸氢钠氧化还原体系低温引发醋酸乙烯酯乳液聚合,合成出分子量为1.07×106、分子量分布为2.75的聚醋酸乙烯酯。讨论了聚合温度、单体用量、十二烷基硫酸钠(SDS)用量、过硫酸铵用量、亚硫酸氢钠用量等因素对聚醋酸乙烯酯黏均分子量的影响,并用GPC法对其进行表征。     

Emulsion and miniemulsion polymerization of isobornyl acrylate

Isobornyl acrylate, a highly hydrophobic monomer, was batch‐polymerized in both emulsion and miniemulsion recipes. Surfactant levels above and below the critical micelle concentration were used, as were two different initiator types: ionic (potassium persulfate) and nonionic (t‐butyl hydroperoxide) Samples were analyzed for degree of conversion, molecular weight, and particle size. The effects of reaction type (emulsion versus miniemulsion), surfactant level, type of initiator (ionic versus nonionic) of the polymer properties are discussed. Issues of monomer transport across the aqueous phase, and mechanisms of nucleation, especially at very low surfactant concentrations are discussed. © 2006 Wiley Periodicals, Inc. J Appl Polym Sci 103: 819–833, 2007     

新型超高相对分子量阳离子聚丙烯酰胺的合成

研究了由过硫酸铵、甲醛次硫酸氢钠、功能性单体 DA及其它助剂组成的低温复合引发体系引发丙烯酰氧乙基三甲基氯化铵 (AETMAC)与丙烯酰胺 (AM)水溶液绝热聚合。考察了影响共聚物特性黏数[η]的因素 :单体浓度 1 8%～ 3 2 % ,引发剂浓度 (9～ 3 0 ) mg/L ,功能单体浓度 (2 .9～ 2 3 .2 )× 1 0 - 3mol/L。由该低温复合引发体系在适宜条件下引发 AETMAC/AM共聚合 ,可得到溶解性能很好、阳离子度为 1 0 %～70 % ,分子量 (1～ 2 )× 1 0 7的 P(AETMAC-AM)干粉。     

植物栽培多彩吸水聚合物制备

采用丙烯酸、氢氧化钠、丙烯酰胺为原料,以N,N-亚甲基双丙烯基酰胺为交联剂,以过硫酸铵、无水亚硫酸钠为引发剂,选择颜色鲜艳又具有水不溶性的颜料为着色剂,采用溶液聚合法合成具有色彩晶莹、吸水不褪色的多彩吸水聚合物。并讨论了交联剂用量、单体浓度、引发剂用量等因素对产品吸水倍数的影响以及颜料的选择、水不溶性颜料的用量对产品着色、褪色的影响。结果表明,适宜的合成条件为:丙烯酸14.2 g,氢氧化钠17.2 g,蒸馏水43.8 g,丙烯酰胺26.6 g,N,N-亚甲基双丙烯基酰胺0.15 g,5%过硫酸溶液2 mL,5%无水亚硫酸钠溶液2 mL,颜料8 mL。     

Particle Nucleation Loci in Styrene-Butyl Acrylate Miniemulsion Copolymerization

Summary Miniemulsion polymerizations of styrene and butyl acrylate in the presence of sodium dodecyl sulfate (SDS) as the surfactant and stearyl methacrylate (SMA) as reactive cosurfactant were carried out by using water-soluble (potassium persulfate) and oil-soluble (2,2-azobisisobutyronitrile) (AIBN) initiators respectively. Effects of the two initiators on the particle nucleation mechanisms are investigated. By comparison with the mean diameter of monomer droplets and polymer particles, it is shown that both homogeneous nucleation and monomer droplets nucleation coexist in the presence of a water-soluble initiator but homogeneous nucleation becomes less significant with SDS concentration increasing. Meanwhile, using oil-soluble initiator, the possibility of homogeneous nucleation is depressed effectively. As a result, monomer droplets are definitely the main loci of particle nucleation.     

Preparation and properties of poly(WPSF‐co‐butyl acrylate) copolymer emulsion with ultrasonic radiation II. Monomer conversion rate and characterization

A stable emulsion of poly(WPSF‐co‐butyl acrylate) based on butyl acrylate, waste polystyrene foam was synthesized through emulsion polymerization using sodium dodecyl sulfate and octyl phenyl polyoxyethylene ether as surfactant, ammonium persulfate and sodium hydrogen bisulfate as mixed redox initiator, under ultrasound irradiation in the absence of inert gas. The effects of various copolymerization conditions on the monomer conversion were reported. The copolymers were characterized by means of IR, ¹HNMR, and gel permeation chromatography. © 2009 Wiley Periodicals, Inc. J Appl Polym Sci, 2009     

Soap‐free emulsion copolymerization of perfluoroalkyl acrylates in the presence of a reactive surfactant

Soap‐free emulsion copolymerization of perfluoroalkyl acrylate (FA)/methyl methacrylate (MMA)/n‐butyl acrylate (n‐BA) was carried out in the presence of sodium 2‐acrylamide‐2‐methyl propanesulfonate (AMPSNa) as a reactive surfactant and potassium persulfate (KPS) as an initiator. An analysis of the effects of concentration of AMPSNa, KPS, FA as well as polymerization temperature on the kinetic features (rate of polymerization) and colloidal characteristics (mean particle diameter, particle disperse index, particle numbers, and surface charge density) was followed. NMR, FTIR, AFM, and fluorine‐selective electrode analysis were used to characterize the composition and morphology of the FA copolymers. Both AFM analysis and contact angle measurements strongly implied that the fluorinated segments migrated to the outmost surface and created films with lower surface energy. © 2007 Wiley Periodicals, Inc. J Appl Polym Sci 104: 2438–2444, 2007     

改性聚乙二醇多磺酸基水处理剂的制备及性能

以过硫酸铵为引发剂,以马来酸酐改性聚乙二醇得到的聚乙二醇酯(PEGMA)、乙烯基磺酸钠(SVS)、丙烯酸(AA)为单体,通过水相自由基共聚反应制备目标共聚物PEGMA-SVS-AA。考察了聚合工艺对其阻碳酸钙垢性能的影响,利用红外光谱对共聚物结构进行表征,得到最佳聚合反应条件为:n(PEGMA)∶n(SVS)∶n(AA)为1∶3∶5,过硫酸铵用量为单体总质量的6%,反应时间2.5 h,控制反应温度为80℃。在该条件下制备的聚合物PEGMA-SVS-AA在模拟工业生产循环冷却水条件下,其阻碳酸钙垢率达到89%。使用XRD和SEM对碳酸钙垢进行了表征,该水处理剂不仅改变了碳酸钙的形貌而且改变了碳酸钙的晶型。     

低相对分子质量聚丙烯酸钠的合成条件研究

以丙烯酸为单体,过硫酸铵为引发剂,通过正交实验,合成了系列聚丙烯酸钠。探讨了反应温度、引发剂用量、单体含量、反应时间对相对分子质量的影响结果。确定了最佳反应条件:反应温度为90℃,引发剂用量为5%,单体含量为30%,聚合反应时间为3 h。     

Synthesis and physicochemical properties of graft copolymer of corn starch and acrylamide

Graft copolymerization of corn starch with acrylamide using ceric ammonium sulphate/citric acid initiation system has been studied under nitrogen atmosphere in aqueous medium. The grafting parameters are favored by increasing monomer concentration and reaction time but are affected by higher concentration of initiator and high temperature. The optimum conditions established for grafting were as follows: the concentration of initiator, 0.003 mol/L; the concentration of citric acid, 0.03 mol/L; monomer/starch, 1:1 feed ratio (w/w); reaction time, 3.0 h; and temperature, 35°C. The extent of grafting was examined by Fourier transform infrared spectroscopy, X‐ray diffraction, and scanning electron microscopy. Both swelling power and solubility increased with the increase in temperature. Graft copolymerization increased swelling power and reduced solubility. Rapid visco‐analyzer pasting profile was studied. Graft copolymerization of corn starch results in high pasting temperature, high peak viscosity, and setback as compared with native starch. Breakdown was retarded at low percentage grafting (6.60%) but increased at high percentage grafting (60.27%). POLYM. COMPOS. 28:47–56, 2007. © 2007 Society of Plastics Engineers     

几种阳离子度PDA共聚物的合成

以丙烯酰胺(AM)和工业单体二甲基二烯丙基氯化铵(DMDAAC)为原料,过硫酸铵(APS)和亚硫酸氢钠(RH)复合物为引发体系,采取一次性加料方法,以特征黏度为考核指标,对几种阳离子度二甲基二烯丙基氯化铵与丙烯酰胺的共聚物PDA进行了制备工艺研究。通过正交优化等实验方法考察了单体起始质量分数、引发剂用量和聚合反应温度3个因素对选定的每一种阳离子度PDA共聚合反应结果的影响,得到了制备系列化具不同阳离子度PDA的各自最佳点的制备工艺条件,比较了在各阳离子度条件下,最佳制备工艺点时单体起始质量分数、引发剂用量和聚合反应温度的变化规律。结果表明,对于制备5%、10%、20%、30%和50%阳离子度的PDA产物,当单体起始质量分数分别为16%、18%、25%、35%和65%,引发剂用量占单体的质量分数分别为8.62×10-5、8.82×10-5、7.35×10-5、5.40×10-5和9.19×10-5,聚合反应温度分别为25、30、30、30℃和25℃时,特征黏度可分别达到17.0、15.0、11.6、9.0 dL/g和6.2 dL/g。此外还对共聚产物PDA进行了红外光谱结构表征。该工艺简单方便、清洁安全,适合于工业化生产。