聚醚多元醇中微量单体含量的毛细管气相色谱分析

采用气相色谱法测定聚醚多元醇中环氧丙烷单体的含量,以四氢呋喃为溶剂,使用DB-1(50 m×0.32 mm×0.25 μm)型分析柱,氢火焰离子化检测器,用内标法(甲醇为内标物)进行分析定量.微量单体测定结果的相对标准偏差＜10%,试验的回收率在(100±3)%以内,检测限低至4×10-6.该方法还具有分析速度快,准确...     

4种酰胺类合成大麻素的气相色谱-质谱检验方法研究

目的 建立5F-MDMB-PICA、MDMB-CHMINACA、5F-EMB-PICA和AMB-FUBINACA 4种酰胺类合成大麻素的气相色谱-质谱(GC-MS)定性定量检验方法.方法 气相色谱-质谱选用Thermo TRACE TG-5MS毛细管柱(30m×0.25mm×0.25μm),采用起始温度200℃,以20...     

盐酸吉西他滨中甲磺酸酯类基因毒性杂质的GC-MS/MS测定

建立了盐酸吉西他滨中2种甲磺酸酯类基因毒性杂质甲磺酸甲酯和甲磺酸乙酯的气相色谱串联质谱(GC-MS/MS)检测方法.采用VF-WAX ms毛细管色谱柱(30 m×0.25 mm×1.0 μm)对这两种甲磺酸酯类化合物进行分离.结果显示,两种化合物在所测浓度范围内线性关系良好;甲磺酸甲酯、甲磺酸乙酯定量限分别为0.009...     

毛细管气相色谱法检测白酒中的有机酸类组分含量

建立一种毛细管气相色谱法测定白酒中有机酸类组分含量的方法。选择DB-WAX(30m×0.32mm×0.25μm)毛细管气相色谱柱,通过优化气相色谱分离条件,采用内标标准曲线法进行定量。结果表明:在5min内,白酒中30多种组分包括醇类、酯类和有机酸类能够有效分离,稳定性好,各有机酸类呈现良好的线性关系,相关系数都在0.999以上,回收率在83.3%-101.9%之间。     

微波液化木材及聚醚多元醇的制备

以醇解的聚酯(PET)饮料瓶为液化剂,甘油作辅助液化剂,微波辅助加热,用2.5%H2SO4催化液化木材。分别讨论了微波功率、液固比/反应时间和温度对液化率的影响。结果表明,在微波功率500 W,反应时间15 m in,温度150℃,液固比为4的条件下,木材液化率99.16%。以此液化物为起始剂,选用双金属氰化物MMC催化环氧丙烷开环聚合,通过改变环氧丙烷的用量制备了不同聚醚多元醇,并采用傅里叶变换红外(FT-IR)、凝胶色谱(GPC)及热示差扫描(DSC)等分析手段对起始剂和不同聚醚多元醇的结构、分子质量分布和耐热性进行了对比表征。研究表明聚醚多元醇的羟值、酸值、黏度随环氧丙烷用量增加减小,分子质量分布随之变窄,热稳定性下降。     

气相色谱内标法测定d-柠檬烯含量

建立了柠檬烯水剂农药中d-柠檬烯的气相色谱(GC)分析方法。以HP-innowax (30m×0.25mm×0.25μm)毛细管柱为色谱柱,乙酸丁酯为内标物,采用氢火焰离子化检测器(FID),内标法定量测定d-柠檬烯含量。结果表明,峰面积与浓度呈良好的线性关系,r=0.9999,精密度良好,平均回收率为100.3%。所建立的分析方法简便快速,结果准确可靠,适用于农药水剂中d-柠檬烯的含量检测。     

低黏度高相对分子质量聚醚三醇的合成及应用

以低相对分子质量聚醚三醇为起始剂,使用自产聚醚催化剂TMD催化环氧丙烷(PO)开环聚合制备低黏度高相对分子质量聚醚多元醇。讨论了起始剂种类、TMD含量、PO预投量对聚醚三醇性能的影响。结果表明,选用MN-1000做起始剂、TMD催化剂质量分数为35×10~(-6)(占总投料量)、PO预滴量为起始剂质量的12%时,得到黏度为2120 m Pa·s(25℃)、相对分子质量分布指数(D值)为1.07、不饱和值为6.4 mmol/kg、相对分子质量8000左右的聚醚三醇。用其制备的减震用聚氨酯铺装材料的断裂伸长率和回弹率均较高。     

A群脑膜炎球菌多糖原液中苯酚残留量气相色谱检测方法的建立及验证

目的建立A群脑膜炎球菌多糖原液中苯酚残留量气相色谱检测方法,并进行验证。方法采用标准溶液加入法,以乙酸丁酯为萃取剂制备对照品及供试品溶液,采用气相色谱法进行检测,色谱条件为:Agilent DB-WAX[聚乙二醇(PEG)强极性柱30 m×0.25 mm×0.25μm]色谱柱,柱温165℃,进样口温度250℃,检测器温度300℃,流速2 m L/min,载气为氮气,进样分流比5∶1,进样量1μL。对方法的专属性及系统适用性、检测限和定量限、线性范围、精密度、准确度进行验证。采用建立的方法检测9批A群脑膜炎球菌多糖原液苯酚残留量。结果苯酚的保留时间分别为5.046 min,拖尾因子为1.04,与乙酸乙酯的分离度为33.21,理论塔板数大于5 000;检测限为0.535×10-3mg/m L,定量限为1.070×10-3 mg/m L;浓度在4~20μg/m L范围内,与峰面积呈良好的线性关系,相关系数(r)为0.999 9;同一操作人员连续重复检测6次结果的相对标准偏差(RSD)为0.4%,2名试验员不同时间重复检测6次结果的RSD为1.5%;9份加标供试品溶液的回收率为95.8%~100.0%;9批A群脑膜炎球菌多糖原液中苯酚残留量均符合规定。结论建立的A群脑膜炎球菌多糖原液中苯酚残留量气相色谱检测方法,具有良好的重复性及准确性,可用于A群脑膜炎球菌多糖原液中的苯酚残留量检测。     

气相色谱质谱联用法测定纺织品中7种多氟化合物

采用气相色谱质谱联用仪,以DB-WAX色谱柱(30 m×0.25 mm×0.25 um)测定纺织品中含氟醇类和含氟丙烯酸酯类。7种目标化合物方法最低检出限、线性范围和加标回收率为:0.006 mg/kg～0.010 mg/kg、10 ug/L～100 ug/L和80.25%～92.64%。     

低不饱和度超高分子量聚醚多元醇的合成研究

以聚醚二醇为起始剂,环氧丙烷(PO)为主原料,使用双金属络合催化剂(DMC)合成低不饱和度相对分子质量约为12000的聚醚二醇.讨论了起始剂分子量、DMC含量、P O加料速率、搅拌转速及反应温度对制得聚醚的黏度、不饱和度和分子量分布的影响.结果表明,以DDL?6000D为起始剂、DMC质量分数为50×10-6、PO加料...     

Die mit Natriumphenolat katalysierte Addition von Äthylenoxid-Propylenoxid-Gemischen an Monophenylmonoalkylenglykole. II. Die Kinetik der Äthylenoxid-Propylenoxid-Addition an Monophenylmonoäthylenglykol

The dependence of insertion-type addition of ethylene oxide/propylene oxide mixture to monophenyl monoethylene glycol on monomer ratios was investigated. An attempt to determine the reactivity parameters by MAYO and LEWIS method was discarded on account of differing dimensions shown by the rate constants of separate reactions. A rate law to describe the consumption of ethylene oxide has been presented. The dependence of relative reaction rates on the-mole ratios shows preference for addition of ethylene oxide; however, rise in reaction temperature exercises no appreciable effect on the preferred addition.     

Polymerization of ethylene oxide by the activated monomer mechanism

The Polymerization of ethylene oxide catalysed by protonic acids and proceeding via the activated monomer mechanism differs from the polymerizations of substituted epoxides like propylene oxide and epichlorohydrin. The kinetics of ethylene oxide polymerization were investigated and compared with the kinetics of model reactions, namely addition of oligomers of ethylene oxide to ethylene oxide. The mechanism of polymerization involves, besides the addition of monomer to the terminal hydroxyl groups, the addition to the polymer ether groups. This reaction does not take place for substituted oxiranes, most probably because of steric hindrance.     

Polymerization of some oxiranes using the diphenylzinc-butanone system in benzene at 60°C

The diphenylzinc-butanone system was used as polymerization catalyst for some oxiranes in benzene solution at 60°C. This system is greatly influenced by the molar ratio of butanone to diphenylzinc, and the maximum catalytic activity for propylene oxide and ethylene oxide was found for a ratio of unity. GPC results strongly suggest the presence of more than one active species for the system. ¹³C NMR analysis indicates that the resulting poly(propylene oxide) has a head-to-tail arrangement. For the polymerization of propylene oxide with butanone/diphenylzinc = 1, after an initial induction period, the reaction was first-order with respect to monomer with k = 2·51 × 10^?5 s^?1. Ethylene oxide polymerizations using butanone/diphenylzinc = 1 and 5 were also first-order with respect to monomer after an initial induction period with k = 7·80 × 10^?6 s^?1 and k = 5·71 × 10^?6 s^?1, respectively. The diphenylzinc-butanone system was not an effective catalyst for styrene oxide polymerization.     

我国丙烯下游产业产品市场情况

介绍了丙烯下游产业聚丙烯、丙烯腈、环氧丙烷、乙丙橡胶的市场供需,研究了规划发展聚丙烯、丙烯腈、环氧丙烷、乙丙橡胶项目的经济规模、原料消耗和项目投资,并进行投资经济分析,针对企业拥有的丙烯资源情况和经济技术实力提出了发展建议。     

Monodisperse micron-sized polystyrene particles by seeded polymerization using reactive macrosurfactants

Monodisperse micron-sized polystyrene particles could be prepared through a two-staged seeded swelling and polymerization method using reactive surfactants. The seed was obtained by emulsifier-free emulsion polymerization. To prepare conventional surfactant-free monomer emulsion droplet in swelling process, a tri-block diol diacrylate (t-BDDA), which is poly(ethylene oxide)-poly(propylene oxide)-poly(ethylene oxide) tri-block copolymer containing two chain ends capped with acryloyl chloride, was employed as a reactive surfactant instead of conventional surfactants. Thermodynamic consideration of the effect of monomer droplet size and interfacial tension on the swelling process ensured that two-staged monomer swelling could be effectively performed by using t-BDDA as a surface-active macromonomer. From the surface tension measurement and optical microscope observation, it was found that the t-BDDA had a favorable surface activity when the monomer emulsion was prepared under its cloud point. From the X-ray photoelectron spectroscopy, it was found that most of the t-BDDA resided on the final particle surfaces.     

SiO2表面原位接枝聚环氧丙烷高分子刷的制备及表征

通过“Stober”法制备出单分散球形SiO₂粒子,并采用3-缩水甘油醚氧基丙基三甲氧基硅烷对其表面进行功能化修饰,然后,利用异丙醇铝作为多相催化剂,原位引发环氧丙烷（PO）单体开环聚合,制得了聚环氧丙烷（PPO）高分子刷接枝改性的SiO₂（PPO-g-SiO₂）。研究了单体添加量、反应温度及反应时间等因素对聚环氧丙烷高分子刷接枝量的影响规律。采用红外光谱（FT-IR）、X射线光电子能谱（XPS）、透射电子显微镜（TEM）、扫描电子显微镜（SEM）及热重分析（TGA）等分析方法对制备的PPO-g-SiO₂的化学结构、微观形貌以及接枝量进行了表征。结果显示,当单体添加量为2.38 mol·L^-1,反应温度为80℃,反应时间为24 h时,PPO在SiO₂表面的接枝量可达23.56%（质量分数）;其厚度约为15 nm。     

废水中环氧丙烷和环氧乙烷的酸化水解预处理

采用化学酸化水解法,对废水中的环氧丙烷和环氧乙烷进行了预处理,研究了加酸量、反应温度、反应时间等因素的影响。结果表明,采用硫酸为催化剂可将废水中的环氧丙烷和环氧乙烷转化为醇类物质,反应后环烷烃质量浓度降低到100mg/L以下,提高了后继废水处理的安全性。针对该废水实际情况,得到最佳反应条件为反应温度10℃,加酸量(浓硫酸与废水体积比)1‰,反应时间12h。     

Copolymerization of ethylene oxide and propylene oxide by anhydrous potassium hydroxide

Ethylene oxide and propylene oxide have been copolymerized at low temperatures in the presence of anhydrous potassium hydroxide. The monomer reactivity ratios were found to be r(ethylene oxide) = 6.5 and r(propylene oxide) = 0.5.     

多金属氰化络合物催化环氧丙烷的聚合

用多金属氰化络合物(MMC)催化环氧丙烷开环均聚,考察了酸及起始剂对聚合诱导期的影响,以及转化单体/起始剂摩尔比、酸用量、加料方式及催化剂等对聚合物相对分子质量及其分布的影响。并用FTIR、1HNMR、SEC-MALLS对聚合产物结构进行了表征。结果表明,以MMC为催化剂,在w(H2SO4)<5×10-5、温度130℃、连续加料、w(MMC)>1×10-4时,所合成聚醚相对分子质量分布较窄(Mw/Mn=1.1~1.2),且相对分子质量可控;FTIR、1HNMR及SEC-MALLS分析结果表明,所合成聚醚具有预期结构。实验发现,聚合反应体系只存在一种活性中心,其机理可能为配位阳离子聚合。