金属钝化剂Nangarz XL-1合成的研究

研究了以2，6-二叔丁基苯酚，丙烯酸甲酯。草酸二乙酯及乙醇胺为原料合成具有抗氧化及金属钝化双重功能的金属钝化剂Nangarz XL-1的合成工艺。考察了各步反应机理及影响因素。结果表明中间体（3，5-二叔丁基-4-羟基）苯基丙酸甲酯合成最佳条件为：丙烯酸甲酯与2，6-二叔丁基苯酚的质量比为1．10：1，丙烯酸甲酯加入方式为120℃滴加0．5h，在140℃下反应4h，产率96．5％；中间体N，N’-双（羟乙基）草酰胺合成最佳条件为：乙醇胺与草酸二乙酯物质的量比2：1，反应温度为112℃，产率95．5％；产品Nangarz XL-1合成的最佳条件为：反应温度180℃，反应时间4h，催化剂为有机锡，产率90．2％。用红外光谱和核磁共振氢谱表征了产品化学结构。     

月桂酸胺基乙醇酯的合成与表征

以月桂酸、N,N-二甲基乙醇胺和N,N-二乙基乙醇胺为原料,亚磷酸为催化剂,通过酯化反应合成月桂酸二甲胺基乙醇酯与月桂酸二乙胺基乙醇酯。月桂酸二甲胺基乙醇酯合成的较优条件为：月桂酸与N,N-二甲基乙醇胺的摩尔比为1∶1.5,催化剂用量0.2%,回流循环水温60℃,反应温度170℃,在此条件下转化率可达95.91%。月桂酸二乙胺基乙醇酯合成的较优条件为：月桂酸与N,N-二乙基乙醇胺的摩尔比为1∶1.25,催化剂用量0.2%,回流循环水温80℃,反应温度150℃,在此条件下,转化率可达98.65%。     

一步法合成3—[β—（N—甲基磺基乙胺基）乙基砜]苯胺的研究

以3－（β－羟乙基砜）苯胺与甲基牛碘酸反应直接生成3－[β－（N－甲基磺基乙胺基）乙基砜]苯胺，通过正交实验优化了工艺条件。实验证明，反应时间对反应产率的影响最大。最佳工艺条件为：3－（β－羟乙基砜）苯胺：牛磺酸：氢氧化钠＝1：1．2：1．1（摩尔比），反应时间6小时，产率可达89．02％。采用纸色层法、元素分析、红外光谱及质谱对产物3－[β－（N－甲基磺基乙胺基）乙基砜]苯胺的结构进行表征。     

羟乙基乙二胺的连续流制备工艺研究

以乙二胺和环氧乙烷为原料,在具有特殊微结构的连续流微反应器内发生乙氧基化反应合成羟乙基乙二胺。考察了原料物质的量比、乙二胺含水量、反应温度、停留时间等对反应的影响。确定了最佳工艺条件为：n(乙二胺) : n(环氧乙烷) = 3:1、乙二胺含水量控制在5%（质量分数）以内、反应温度为80 ℃、停留时间为60 s。在此条件下,环氧乙烷转化率接近100%,羟乙基乙二胺的选择性为87.4%,二羟乙基乙二胺的选择性为9.2%。间歇釜式反应工艺在相同物料比和反应温度条件下,羟乙基乙二胺的选择性为83.5%,二羟乙基乙二胺的选择性为15.9%,与之相比,连续流微反应器能有效提高羟乙基乙二胺的选择性,降低副反应的发生,同时大大缩短了反应时间,提高了反应效率。     

微波辐射合成N-(2-羟乙基)-邻苯二甲酰亚胺

在微波辐射下，邻苯二甲酸酐和乙醇胺反应可直接合成N-（2-羟乙基）-邻苯二甲酰亚胺。最佳条件为：辐射功率为259W，辐射时间为6min，邻苯二甲酸酐与乙醇胺的物质的量比为1：1.05，产率可达87.1％。     

化学生物组合法合成米格列醇及其表征

以葡萄糖和乙醇胺为原料,催化加氢生成N-羟乙基葡糖胺,葡萄糖转化率为89%。氧化葡萄糖酸杆菌Gouv2007的静息细胞在通气下氧化N-羟乙基葡糖胺脱氢生成米格列醇的前体物质6-脱氧-6-羟乙基氨基-α-L-呋喃山梨糖,再催化加氢生成米格列醇,对从N-羟乙基葡糖胺生成米格列醇的底物转化率为77.3%。采用熔程测定、红外光谱分析、质谱分析对N-羟乙基葡糖胺和米格列醇进行了表征,结果表明:所合成的产物分别被鉴定为N-羟乙基葡糖胺和米格列醇。     

反相乳液聚合制备聚丙烯酰胺

采用反相乳液聚合法合成了聚丙烯酰胺（PAM）,测定了聚合反应转化率及产物特性粘度,并对其官能团进行了表征。考察了加料方式、单体质量分数、乳化剂用量、油水此对产物性能的影响。实验结果表明,最佳合成条件为：单体质量分数22．5％（对水相）,乳化剂质量分数2％（对油相）,油水比为1：2。     

SO_4~(2-)/Al_2O_3型固体超强酸固定床合成N-羟乙基吡咯烷酮的研究

采用在固定床工艺以SO~(2-)_4/Al_2O_3型固体超强酸为催化剂在加热条件下催化γ-丁内酯和乙醇胺脱水合成N-羟乙基吡咯烷酮(NHP)。通过正交试验对影响反应的各因素进行了分析,结果表明:反应温度为280℃、γ-丁内酯与乙醇胺的物质的量比为1:1.3、进料速度为0.3m L/min时产品NHP的反应效果最佳,转化率为78.3%、选择性45.6%。该合成方法反应步骤少,催化剂效率高,可连续反应,具有一定的优势。     

反相悬浮聚合法制备阳离子聚丙烯酰胺

用反相悬浮法,以甲基丙烯酰氧乙基三甲基氯化胺（DMC）和丙烯酰胺（AM）为单体,V-50为引发剂,合成了阳离子聚丙烯酰胺（CPAM）。实验结果表明,较佳工艺条件为：分散剡为浓度3,6％的Span60-Span80（1：1）,引发剂浓度0.6‰,单体配比AM：DMC为1：1,单体浓度为60％。     

4β-[(N-甲基磺基乙胺基)乙基砜]苯胺的合成研究

以4β-（羟乙基砜）乙酰胺基苯胺与甲基牛磺酸反应直接生成4β-[（N－甲基磺基乙胺基）乙基砜]苯胺，通过正交实验优化了工艺条件，其最佳工艺条件为：对应酰化物：牛磺酸：氢氧化钠＝1：1．2：2．5，反应时间4h。产率可达89％，采用纸色层法，元素分析、红外光谱及质谱对产物4β-[（N－甲基磺基乙胺基）乙基砜]苯胺的结构进行表征。     

水性环氧丙烯酸乳液的合成研究

以甲基丙烯酸甲酯、苯乙烯为硬单体,丙烯酸丁酯为软单体,甲基丙烯酸、丙烯酸羟乙酯和双丙酮丙烯酰胺为功能单体,环氧树脂为改性剂,水为分散介质,通过乳液共聚合制备环氧-丙烯酸乳液,讨论了聚合工艺、引发剂用量、反应温度、环氧树脂种类和用量以及软硬单体配比对乳液聚合反应及涂膜性能的影响。     

水性丙烯酸树脂及防白电油水墨的研究

对防白电油水墨用丙烯酸树脂的制备进行了研究,以满足特种纸张防白电油的需要.实验以甲基丙烯酸、丙烯酸乙酯、甲基丙烯酸甲酯、丙烯酸羟乙酯和丙烯酰胺为聚合单体,过硫酸铵为引发剂,在水和乙醇中进行聚合,然后中和成透明的水溶性丙烯酸树脂液.此外,实验还研究了乙醇用量以及交联单体用量对防白电油性能的影响.结果表明,混合溶剂去离子水...     

Narrow‐disperse or monodisperse crosslinked and functional core–shell polymer particles prepared by two‐stage precipitation polymerization

Narrow‐disperse and monodisperse cross‐linked core–shell polymer particles containing different functional groups, such as esters, hydroxyls, chloromethyls, carboxylic acids, amides, cyanos, and glycidyls, in the shell layers in the micrometer size range were prepared by a two‐stage precipitation polymerization in the absence of any stabilizer. Commercial divinylbenzene (DVB), containing 80% DVB, was precipitation polymerized in acetonitrile without any stabilizer as the first‐stage polymerization and was used as the core. Several functional monomers, including methyl methacrylate, ethyl methacrylate, butyl methacrylate, 2‐hydroxyethyl methacrylate, glycidyl methacrylate, methyl acrylate, ethyl acrylate, butyl acrylate, t‐butyl acrylate, i‐octyl acrylate, acrylic acid, acrylamide, acrylonitrile, styrene, and p‐chloromethyl styrene, were incorporated into the shells during the second‐stage polymerization. The resulting core–shell polymer particles were characterized with scanning electron microscopy and Fourier transform infrared spectroscopy. © 2006 Wiley Periodicals, Inc. J Appl Polym Sci 100: 1776–1784, 2006     

含三嗪环的超支化聚酯丙烯酸酯的合成和应用

以丙烯酸甲酯和二乙醇胺为原料,制得N,N-二羟乙基-3-胺基丙酸甲酯（DAMP）;接着,用DAMP与三羟乙基异氰脲酸酯（THEIC）经酯交换反应,合成出一种超支化聚酯多元醇;再以该多元醇与丙烯酸通过酯化反应,制备了可UV固化的超支化聚酯丙烯酸酯。实验结果表明：以对甲苯磺酸为催化剂,当THEIC与DAMP的物质的量比为1∶9时,可制得二代超支化聚酯多元醇;该聚酯丙烯酸酯的玻璃化温度为53.0℃,与环氧丙烯酸酯（9104）混合组成的组合物,具有固化速度快、固化膜柔韧性佳的特点;附着力可达0级,摆杆硬度为0.751。     

Azeotropy in terpolymerization of 2-pyrimidyl acrylamide with different alkyl acrylates and acrylonitrile

2-Pyrimidyl acrylamide monomer (2PA) has been prepared by the reaction of 2-amino pyrimidine with acrylolyl chloride in the presence of triethylamine as catalyst. Its structure was confirmed by IR and ¹H NMR spectroscopy. Ternary copolymerizations of 2-pyrimidyl acrylamide monomer (2PA) with methyl acrylate (MA), methyl methacrylate (MMA), ethyl acrylate (EA), butyl acrylate (BuA) and acrylonitrile (AN) were carried out in THF at 65°C in the presence of a free radical initiator. Experimental terpolymerization data agree well with calculations based on the Alfrey–Goldfinger equation. The determination of unitary, binary and ternary azeotropies of the various systems studied were easily handled by a computer. The ternary azeotropic compositions for 2PA–MA–AN and 2PA–MMA–AN were 32.20:17.5:50.30 and 13.54:52.64:33.82mol%, respectively. Pseudo-azeotropic regions were identified where the deviation between feed and polymer composition is very small.     

Nanosize polymer latices made by microemulsion copolymerization: Preparation and characterization

Polymer nanoparticles were prepared by a methyl methacrylate/butyl methacrylate/2‐hydroxyethyl methacrylate/acrylate or methyl acrylate microemulsion copolymerization process. A microemulsion copolymerization method was used. With this process high polymer : surfactant weight ratios (≥15 : 1), relatively concentrated (～ 30 wt %) lattices, and small (～ 60 nm) particle diameters were obtained. Properties of the latices were characterized in detail by TEM, DSC, dynamic light scattering, spectrophotometry, and tensile strength testing. © 2003 Wiley Periodicals, Inc. J Appl Polym Sci 90: 3625–3630, 2003     

Synthesis of casein-g-poly(methyl acrylate). II

The synthesis of casein-g-poly(methyl acrylate) was studied using the potassium peroxydisulfate–ascorbic acid redox system. The effect of synthetic variables has been investigated in the light of rates of conversion of monomer, graft copolymerization and homopolymerization, percent grafting, and grafting efficiency. The results are compared with the system initiated by pure potassium peroxydisulfate alone.     

四元共聚丙烯酸酯热熔压敏胶膜的合成研究

以丙烯酸-2-乙基己酯(2-EHA)、甲基丙烯酸甲酯(MMA)、丙烯腈(AN)和丙烯酰胺(AM)为共聚单体,采用预乳化法制备聚丙烯酸酯热熔胶,研究了单体用量配比,乳化剂用量、配比及乳化方式,引发剂用量,温度和滴加速度对反应及性能的影响。结果表明：2-EHA/MMA 1/0．6,AN 5％,AM 5％,复合乳化剂3．0％,引发剂过硫酸钾0．3％,80～85℃,反应4h,丙烯酸酯橡胶分子量在10万以上时,制得的热熔压敏胶膜综合性能良好。     

超高相对分子质量聚乙烯纤维粘合涂层用水乳型聚丙烯酸酯微乳液的合成

以甲基丙烯酸甲酯(MMA)、丙烯酸丁酯(BA)、丙烯酸(AA)及丙烯酸羟乙酯(HEA)为单体,以十二烷基硫酸钠(SLS)、OP-10和正辛醇的复合物为乳化剂,当m(BA)∶m(MMA)∶m(AA)∶m(HEA)=50∶50∶3∶10、w(乳化剂)=13%、反应温度为80℃及反应时间为3h时,合成了可用于超高相对分子质量聚乙烯纤维粘合涂层的水乳型聚丙烯酸酯微乳液,单体转化率为99 8%,乳胶粒径为30nm,乳液膜的玻璃化温度为-28℃,应用工艺简单,涂层粘附性好、柔软、耐磨。     

Poly(N‐hydroxyethyl acrylamide)‐b‐polystyrene by combination of ATRP and aminolysis processes

Block copolymers of very hydrophilic poly(N‐hydroxyethyl acrylamide) (PHEAA) with polystyrene (PS) were successfully synthesized by sequential atom transfer radical polymerization of ethyl acrylate (EA) and styrene monomers and subsequent aminolysis of the acrylic block with ethanolamine. Quantitative aminolysis of poly(ethyl acrylate) (PEA) block yielded poly(N‐hydroxyethyl acrylamide)‐b‐polystyrene in well‐defined structures, as evidenced by Fourier transform infrared spectroscopy (FTIR) and ¹H‐NMR spectroscopy techniques. Three copolymers with constant chain length of PHEAA (degree of polymerization: 80) and PS blocks with 21, 74, and 121 repeating units were prepared by this method. Among those, the block copolymer with 21 styrene repeating units showed excellent micellation behavior in water without phase inversion below 100°C, as inferred from dynamical light scattering, environmental scanning electron microscopy, and fluorescence measurements. © 2012 Wiley Periodicals, Inc. J. Appl. Polym. Sci., 2013