磺化瓜胶的合成及性能研究

本文以瓜胶(GG)为原料,3-氯-2-羟基丙磺酸钠(CHPS)为磺化剂,氢氧化钠为催化剂,乙醇的水溶液为分散剂,合成磺化瓜胶。讨论了影响瓜胶黏度的主要因素,得出较优的合成条件为:反应温度26℃、反应时间2h、磺化剂加量为瓜胶质量的0.5%、氢氧化钠加量为瓜胶质量的1.0%,制得的瓜胶黏度为104.3m Pa·s。将磺化瓜胶配成压裂液进行性能测试,结果表明其具有较好的性能。     

丙烯酸-2-羟基-3-磺酸钠-丙酯的合成

以环氧氯丙烷为原料,通过磺化、闭环和酯化反应,合成了功能性单体丙烯酸-2-羟基-3-磺酸钠-丙酯。对中间产物3-氯-2-羟基丙磺酸钠、环氧丙磺酸钠及最终产物丙烯酸-2-羟基-3-磺酸钠-丙酯〖JP〗等进行了熔点测试和FTIR分析鉴定,并对闭环和酯化反应的影响因素进行了讨论,确定了最佳反应条件。单因素闭环反应,最佳反应条件：n(NaOH)∶n(NaCHPS)=0.9∶1.0,溶剂为丙酮,NaOH配制成26%的水溶液进行滴定,反应温度35 ℃,滴加时间(1.5～2.0) h,反应时间2.0 h;单因素酯化反应,最佳反应条件：催化剂为苄基三乙基氯化铵,其用量占反应物总质量的1.2％;n(环氧丙磺酸钠)∶n(丙烯酸)=1.0∶1.2时,酯化率较高,反应时间为3.0 h。     

2,3-环氧丙磺酸钠的合成及应用进展

综述了3 氯 2 羟基丙磺酸钠和2,3 环氧丙磺酸钠的合成及其在功能材料方面的应用。由环氧氯丙烷与亚硫酸氢钠反应可以生成3 氯 2 羟基丙磺酸钠,再由3 氯 2 羟基丙磺酸钠在碱性溶液中闭环生成2,3 环氧丙磺酸钠。2,3 环氧丙磺酸钠因其分子结构中既含有环氧基,又含有亲水性的磺酸盐基团,可通过环氧基的开环反应和共聚反应等制备许多性能优异的功能物质如:胶凝化剂、稠化剂、乳化剂、光敏材料、印染保护剂等。     

月桂酸-2-羟基-3-丙磺酸钠的合成

以亚硫酸氢钠、环氧氯丙烷、磷酸钠和月挂酸为原料合成7月桂酸-2-羟基-3-丙磺酸钠,研究了反应温度、反应时间、催化剂用量、反应物摩尔比等对反应的影响,确定了合成目标产物的最佳方案为:亚硫酸氢钠与环氧氯丙烷的摩尔比为1.15:1,环氧氟丙烷滴加到亚硫酸氢钠溶液中,85℃下滴加2 h,反应1.5 h,合成中间产物3-氯-2-羟基丙磺酸钠;3-氯-2-羟基丙磺酸钠加入到磷酸钠溶液中,55℃下反应4 h,合成中间产物2,3-环氧丙磺酸钠;2,3-环氧丙磺酸钠溶液滴加到月桂酸中,90℃下滴加0.5 h,反应2.5 h,合成月桂酸-2-羟基-3-丙磺酸钠,此时产率达85.2%,通过红外光谱时产物进行了表征.     

肉豆蔻酸-2-羟基-3-磺酸钠丙酯的合成

以亚硫酸氢钠、环氧氯丙烷、磷酸钠和肉豆蔻酸等为原料,合成了肉豆蔻酸-2-羟基-3-磺酸钠丙酯,探索了反应温度、催化剂、反应时间、反应物物质的量比等因素对合成的影响。结果表明,适宜的反应条件为:①合成3-氯-2-羟基丙磺酸钠:环氧氯丙烷滴加到亚硫酸氢钠溶液中,反应时间3.5 h,反应温度85℃,②合成环氧丙磺酸钠:3-氯-2-羟基丙磺酸钠加入磷酸钠溶液中,反应温度55℃,反应时间4.0 h;③合成肉豆蔻酸-2-羟基-3-丙磺酸钠:环氧丙磺酸钠溶液滴加到90℃的肉豆蔻酸溶液中,反应时间3.0 h,产率为85.2%。对产品进行了红外光谱表征,产品显示了较好的表面活性。     

3-氯-2-羟基丙磺酸钠的合成研究

以环氧氯丙烷和亚硫酸氢钠为原料合成了3-氯-2-羟基丙磺酸钠,探讨了磺化剂种类及用量,溶剂水的用量,反应温度,反应时间对产率的影响,并用红外光谱及元素分析对产物的结构进行表征。实验表明,磺化剂宜用亚硫酸氢钠;亚硫酸氢钠/环氧氯丙烷比越大,水的用量,反应温度,反应时间适中时,产率越高,最高产率为40.7%;产物的熔点为2531℃。     

2-羟基-3-烯丙氧基丙磺酸钠的合成

采用新方法合成了2-羟基-3-烯丙氧基丙磺酸钠。先由环氧氯丙烷和亚硫酸氢钠合成中间体3-氯-2-羟基丙磺酸钠，然后中间体再与丙烯醇在氢氧化钠催化下生成目标产物2-羟基-3-烯丙氧基丙磺酸钠。2步反应总收率在70％左右，中间体和产物分别进行了光谱表征。     

脂肪醇聚氧乙烯醚丙基磺酸盐的合成与性能研究

以脂肪醇聚氧乙烯醚(AEO-5)和3-氯-2-羟基丙磺酸钠为主要反应原料,合成了脂肪醇聚氧乙烯醚丙基磺酸钠(AESO-5)。考察了反应温度、反应时间、原料摩尔比对产率的影响,并对其理化性能进行了测试。结果表明:在3-氯-2-羟基丙磺酸钠与醇醚钠摩尔比为1∶1.5,反应温度为84℃,反应时间为6 h的条件下,目的产物收率最高为62.97%。产物的表面张力和临界胶束浓度分别为31.06 m N/m和2.2×10-4mol/L。产物与十二烷基苯磺酸钠(SDBS)、脂肪醇聚氧乙烯醚硫酸钠(AES)相比,耐温抗盐性较好。     

2,3-环氧丙磺酸钠催化合成与表征

以环氧氯丙烷、亚硫酸氢钠为原料,采用两步法合成2,3-环氧丙磺酸钠;考察了催化剂、溶剂、反应温度对反应的影响.通过条件和正交实验得出最佳反应条件:反应温度55℃,磷酸钠与3-氯-2-羟基丙磺酸钠为1:1(摩尔比)时,每0.1 mol反应物加50 mL水.在最佳反应条件下,收率达85%以上.     

磺酸功能化黄原胶催化四氢苯并[b]吡喃的绿色合成

黄原胶是一种由微生物发酵而生产的多糖,具有稳定性好、安全环保等特性。由于其分子中含有羟基等活性基团,可通过简单的结构修饰来制备环境友好型催化剂。采用黄原胶与氯磺酸的磺化反应,制备了磺酸功能化黄原胶固体酸催化剂,在无溶剂条件下催化芳香醛、丙二腈和双甲酮(或1,3-环己二酮)的3组分缩合反应,以85%～97%的产率合成了一系列四氢苯并[b]吡喃衍生物。该催化剂具有安全无毒、可生物降解且可重复利用等优点,符合绿色和可持续发展化学的理念。     

Styrene–butadiene rubber/cellulose II/clay nanocomposites prepared by cocoagulation—mechanical properties

In this work, nanocomposites of styrene butadiene rubber (SBR), cellulose II, and clay were prepared by cocoagulation of SBR latex, cellulose xanthate, and clay aqueous suspension mixtures. The incorporated amount of cellulose II was 15 phr, and the clay varied from 0 to 7 phr. The influence of cellulose II and clay was investigated by rheometric, mechanical, physicochemical, and morphological properties. From the analysis of transmission electron microscopy (TEM), dispersion in nanometric scale (below 100nm) of the cellulosic and mineral components throughout the elastomeric matrix was observed. XRD analysis suggested that fully exfoliated structure could be obtained by this method when low loading of silicate layers (up to 5 phr) is used. The results from mechanical tests showed that the nanocomposites presented better mechanical properties than SBR gum vulcanizate. Furthermore, 5 phr of clay is enough to achieve the best tensile properties. © 2010 Wiley Periodicals, Inc. J Appl Polym Sci, 2011     

Effect of dispersing and stabilizing additives on rheological characteristics of the upgraded brown coal water mixture

Upgraded brown coal water mixture (UBCWM) preparation by using an Indonesian upgraded coal produced by upgraded brown coal (UBC) process, was carried out to study the effect of dispersing and stabilizing additives on rheological behavior of the UBCWM. Three kinds of anionic dispersing additives, naphthalene sulfonic formaldehyde condensate (NSF), poly (meth) acrylate (PMA) and poly styrene sulfonic acid (PSS) and three kinds of stabilizing additives, carboxyl methyl cellulose (CMC), rhansam gum (S-194) and gellan gum (S-60) were used in this study. Results indicate that the addition of NSF 0.3 wt.% together with S-194 0.01 wt.% is effective in preparing UBCWM with good slurryability and stability, based on its rheological characteristics with the apparent viscosity at shear rate of 100 s^− 1 and yield stress at zero point of shear rate. The rheological behavior of all of the UBCWM that prepared, exhibits non-Newtonian Bingham plastic. From the economical point of view, the price of S-194 is expensive. On the other hand, CMC is cheap and abundant. Therefore, the addition of CMC 0.01 wt.% together with NSF 0.3 wt.% is also effective in preparing UBCWM with good fluidity and stability.     

纤维素黄原酸脂的制备及处理含铜废水的研究

以纤维素为原料,制备了纤维素黄原酸酯,并将其应用于去除模拟废水中的铜离子。采用5因素4水平正交实验法考察了氢氧化钠浓度、二硫化碳加入量、反应时间、反应温度、氯化镁用量对纤维素黄原酸酯增重率的影响。较优的制备条件:NaOH用量为30mL,CS2为0.3mL,反应时间为1.5h,反应温度为10℃,MgCl2用量为30mL。该制备条件下得到的黄原酸酯的增重率为66.35%,用其处理浓度为30mg/mL的含铜模拟废水,铜的去除率可高达99%。     

Cotton linter nano-fibers as the potential reinforcing agent for guar gum

Cotton linter nano-fibers (CLNFs) were prepared from cotton linters by a refining process. The prepared CLNFs were characterized for morphology, crystallinity and degree of polymerization. CLNF was used as a reinforcing agent in guar gum to improve its performance properties. Guar gum/CLNF nanocomposite films were prepared by a solution-casting process. CLNF was added in concentrations of 0.1, 0.25, 0.5 and 1.0 % (w/w) in guar gum. The prepared guar gum/CLNF nano-composite films were characterized for mechanical, thermal, rheological, crystallinity, water vapor transmission rate (WVTR) and light transparency properties. The enthalpy of melting and melting temperature of guar gum increased with increased concentration of CLNF; but up to 0.25 % (w/w) concentration, above which they started decreasing. Tensile strength and Young’s modulus of guar gum increased by 32 and 35 %, respectively, by 0.25 % (w/w) addition of CLNF; however, it decreased on further increase in the concentration of CLNF. The percentage elongation at break and WVTR decreased by 58 and 57 % for 0.25 % (w/w) CLNF-added guar gum. The observed improvements in the properties were due to better interaction between CLNF and guar gum. CLNF was found to have uniformly dispersed in guar gum on addition up to 0.25 % concentration; however, it started forming aggregates at higher concentration, as evident from scanning electron microscopy. Viscosity increased, whereas transparency decreased with increased concentration of CLNF in guar gum.     

低温硫化NR/BR并用胶的硫化特性及其力学性能研究

采用异丙基黄原酸钠SIP、N-乙基-N-苯基二硫代氨基甲酸PX的复合促进剂体系(用量分别为1.5phhr和0.5phhr)可使天然橡胶/顺丁橡胶并用胶(并用比为70∶30)在90℃~95℃内快速硫化,硫化特性符合缓冲胶工艺的要求,但其性能与HG/T 4124-2009《预硫化缓冲胶》存在一定的差距。     

Synthesis of poly(vinyl alcohol) combs via MADIX/RAFT polymerization

Poly(vinyl acetate) combs have been prepared via macromolecular design via interchange of xanthate (MADIX)/reversible addition-fragmentation chain-transfer (RAFT) polymerization using xanthate functionalized polymer cores. The comb backbones were prepared using well-defined poly(vinyl alcohol) PVA polymers with a degree of polymerization of 20, 100 and 170, respectively. Functionalization with xanthates via R-group or a Z-group approach resulted in the formation of macromolecular MADIX agents. While Z group designed macromolecular xanthate agents appeared to inhibit the polymerization of vinyl acetate (VAc), R group designed macromolecular xanthate agents achieved to mediate efficiently the bulk polymerization of VAc affording PVAc combs. However, the growth of the combs was accompanied at low conversions by the formation of linear polymer chains as a result of the constant initiation (AIBN) and shoulders, which can be attributed to intermolecular coupling reactions. The proportions of single chains and termination products were observed to increase with the degree of polymerization of the macromolecular MADIX agents broadening the molecular weight distribution. As a result of a stable ester link between the branches and the PVA backbone, the branched PVAc architectures were finally hydrolyzed to afford poly(vinyl alcohol) combs.     

新型脂肪族磺酸基强酸型阳离子交换树脂的合成

以2-丙烯酰胺-2-甲基丙磺酸(AMPS)为单体、CuCl/N,N,N′,N′-四甲基乙二胺(TMEDA)为催化体系,氯乙酰化聚苯乙烯微球(PS-acyl-Cl)为大分子引发剂,经原子转移自由基聚合反应(ATRP),于微球表面接枝聚脂肪族磺酸(PAMPS)链段获得脂肪族磺酸基强酸性阳离子交换树脂(PS-g-PAMPS).考察了反应温度、溶剂体系、pH 值、催化剂、反应时间等条件对接枝反应的影响,在优化的反应条件下,使用氯乙酰基担载量为3.82 mmol?g?1的 PS-acyl-Cl,10 h 可获得担载量为1.99 mmol?g?1的 PS-g-PAMPS.产物经过红外,元素分析表征.该 PS-g-PAMPS 较传统的磺酸基树脂有较长的手臂长度,位阻小,易于和其它物质反应,TG 分析显示具有很好的热稳定性.     

Starch polyampholytes with amine and xanthate substituents: Characterization and application

Starch polyampholytes (xanthated starch amines) that contained either diethylaminoethyl or 2-hydroxypropyltrimethylammonium ether and xanthate substituents were prepared, characterized, and evaluated as wet- and dry-strength agents in paper handsheets. In aqueous solutions, these xanthated starch amines (XSA), which had degrees of substitutions (D.S.) of 0.023–0.33 amine and 0.005–0.165 xanthate, underwent intra- and interionic bonding at their isoelectric points to form soft flocculent precipitates. Properties of XSA resembled those of “complex coacervates.” Paper that was prepared from an unbleached kraft furnish treated with XSA (amine/xanthate molar ratios, from 1.5 to 4.0) had significantly stronger wet and dry strengths than paper treated with cationic starch amines typically used in commercial papermaking.     

Synthesis and properties of superabsorbent hydrogels based on guar gum and succinic anhydride

Synthesis of novel superabsorbent hydrogels has been investigated with the reaction of guar gum and succinic anhydride (SA), using of 4‐dimethylaminopyridine as esterification promoter and water or dimethylsulfoxide (DMSO) as reaction solvent, followed by NaOH neutralization. Hydrogels prepared in water exhibited somewhat higher water absorbency than those prepared in DMSO; its maximum water absorbency in pure water and aqueous 0.9% NaCl solution was ca. 200 g/g and 80 g/g, respectively. These values were considerably higher than those of hydrogels obtained from starch in a similar way. The products in this study biologically degraded up to 70–80% after 10 days in activated sludge, which shows their excellent biodegradability. © 2009 Wiley Periodicals, Inc. J Appl Polym Sci, 2009     

去冷沉淀血浆的质量分析

目的比较去冷沉淀血浆(Cryoprecipitate-reduced plasma,CRP)中系列凝血因子、纤维蛋白原(Fibrinogen,Fib)和血管性血友病因子裂解蛋白酶(A disintegrin-like and metalloprotease with thrombospondin-1 repeats 13,ADAMTS-13)水平的变化。方法用140人份新鲜冰冻血浆(Fresh frozen plasma,FFP)制备CRP,采用Biggers一期法测定FFP和CRP中FⅡ、FⅤ、FⅦ、FⅧ、FⅨ、FⅩ、FⅪ、FⅫ的促凝活性;免疫比浊法测定Fib和血管性血友病因子抗原因子活动度(vWF∶Ag)水平;荧光共振能量转移法(Fluorescence resonance energy transfer,FRET)测定70人份FFP和CRP中的ADAMTS13活性及抗原含量。结果与FFP比较,CRP中FⅧ∶C、FⅤ∶C、FⅦ∶C、FⅨ∶C、FⅩ∶C、FⅪ∶C、Fib、vWF∶Ag水平均明显下降,且差异均有统计学意义(P<0.05或<0.001);FⅡ∶C、FⅫ∶C、ADAMTS13抗原含量和活性差异均无统计学意义(P>0.05)。结论 CRP可代替FFP用于血栓性血小板减少性紫癜(Thrombotic throm-bocytopenic purpura,TTP)的治疗,而不适用于FⅧ、Fib及vWF缺乏患者的补充治疗。