丙烯酸乙酯基三甲基氯化铵的常压制备法

对以二甲胺基乙基丙烯酸酯(DMAEA)和一氯甲烷为原料,常压下制取高品质的丙烯酸乙酯基三甲基氯化铵(DMAEA-Q)工艺条件进行了探讨。结果表明,当DMAEA为345.8g,阻聚剂为2.8g,DMAEA与回滴用DMAEA-Q摩尔比为11.3,反应温度45℃,回滴液质量分数29.5%,保温时间1h,最终补水28.5g时,可制得质量分数79.2%,水解率(摩尔分数)0.77%的DMAEA-Q。     

丙烯酸二甲氨基乙酯的合成新工艺研究

以二甲氨基乙醇与丙烯酰氯为原料,以乙醚为溶剂进行N-酰基化反应,合成一种用途广泛的多功能单体丙烯酸二甲氨基乙酯(DMAEA)。通过实验,研究了物料比、反应温度、反应时间对DMAEA转化率的影响。最终确定了一条合成DMAEA的最佳工艺:以乙醚为溶剂,反应温度为5°C,反应时间为4 h,n(丙烯酰氯)∶n(二甲氨基乙醇)=1.0∶1.9时,丙烯酸二甲氨基乙酯的产率为72.1%。     

CaCO3分散剂的合成及工艺优化

以苯乙烯磺酸钠（SSS）、聚乙二醇单甲醚丙烯酸酯（MPEGA）、丙烯酸二甲氨基乙酯（DMAEA）为单体通过水溶液聚合法制备超分散剂SMD用于分散无机颜料,具有低污染的优点。通过中心复合设计法建立数学模型优化工艺条件,经过证实,建立的多元线性回归方程预测准确。当引发剂用量8%,聚合温度66℃,反应时间4.5 h时,制得的超分散剂具有较好分散性能,分散CaCO₃浆料黏度可低至101.43 mPa·s。     

紫外交联改性丝素蛋白的制备及溶胀性能测试

本文采用紫外交联法制备丝素和2-(二甲氨基)丙烯酸乙酯(DMAEA)、丝素和2-羟基乙基丙烯酸酯(HEA)及丝素和季铵盐的改性丝素蛋白凝胶。通过溶胀率、红外光谱表征改性丝素蛋白凝胶的结构特性,通过热重分析研究改性丝素蛋白凝胶的热稳定性。实验结果表明DMAEA改性丝素蛋白凝胶的溶胀性能优于添加HEA和季铵盐的改性丝素蛋白凝胶;盐浓度的影响表明,DMAEA、HEA和季铵盐的改性丝素蛋白凝胶溶胀率均随盐浓度升高而下降。热重分析研究表明,三种紫外聚合的凝胶,在100℃附近开始分解,450℃左右分解完,热稳定较好。三种改性方法中,添加HEA的凝胶的热稳定较好,添加DMAEA的凝胶溶胀率最好。     

四氢呋喃和聚四氢呋喃生产技术进展

四氢呋喃（THF）除生产聚四氢呋喃外。也是重要的有机合成原料和性能优良的溶剂。聚四氢呋喃（PolyTHF）又称为聚四亚甲基醚乙二醇（PTMEG）。由四氢呋喃（THF）通过阳离子开环聚合制取。PolyTHF（PTMEG）是制取嵌段聚氨酯和聚醚弹性体材料的重要原料。     

红薯藤制取草酸生产工艺研究

将红薯藤用硝酸催化氧化制取草酸。本文采用Ｌ_（１６）（４~５）正交实验法并详细分析，讨论了诸因素对草酸产量的影响，获得了从红薯藤制取草酸的最佳条件，从而为草酸的制取，农副产品的综合利用开辟了一条新途径。     

以风化煤为原料制取超细腐殖酸研究

以风化煤为原料制取超细腐殖酸（HA）的工艺中添加自制改性剂RN、十二烷基苯磺酸钠（LAS）、十二烷基硫酸钠（SDS）、聚乙烯醇（PVA）等表面改性剂对反应提取率和粒度分散性的影响情况。     

由氯油制取氯仿

由氯油制取氯仿张光玺，李自英，徐隽（云南大学化学系，昆明６５００９１）氯仿是有机合成的原料，是溶剂和革取剂。氯仿可由甲烷氯化或四氯化碳还原来制取，也可以用乙醇或丙酮作原料利用卤仿反应来合成＂＂。本文采用氯碱厂的副产品氯油（含三氯乙醛）作原料来制取氯仿...     

冷压型煤在炭化过程中的膨胀与收缩特性

用型块收缩仪研究了由鹤壁煤制取的冷压型煤在炭化过程中的膨胀与收缩特性。以Ｌ_（１６）（４×２~３）的正文试验设计方法，选择制取冷压铸造型焦的最佳操作条件。     

联产硫酸钾和化学二氧化锰的新工艺研究

介绍了以锰矿、硫酸、碳铵和氯化钾为原料制取硫酸钾（Ｋ＿２ＳＯ＿４）、联产化学二氧化锰（ＣＭＤ）新工艺的研究内容和结果。     

Hydrogels from 2-(dimethylamino)ethylacrylate with 2-acrylamido-2-methyl-1-propanesulfonic acid: synthesis,characterization, and water-sorption properties

A novel series of copolymer hydrogels of 2-(dimethylamino)ethylacrylate (DMAEA)/2-acrylamido-2-methyl-1-propanesulfonic acid (AMPS) were prepared by solution free radical polymerization at different feed monomer mol ratios. The monomer reactivity ratios were determined by Kelen–Tüdös method. According to that, the monomer reactivity ratios for poly(DMAEA-co-AMPS) were r₁ = 0.125 and r₂ = 2.85, (r₁ × r₂ = 0.356). The effect of reaction parameters, including the concentration of cross-linking reagent N,N′-methylene-bis-acrylamide (MBA) and initiator ammonium persulfate (APS), the monomer concentration, pH, temperature, salt solutions, and solvent polarity on the water absorption have been also studied. The hydrogels achieved water-absorption values of 430 g of water/g of xerogel for the copolymer 1:2 richest in AMPS moiety. This copolymer is also very stable to the temperature effect. The optimum pH for the copolymers is 7. Aqueous solutions of the copolymers showed lower critical solution temperature behaviour (LCST). The phase transition temperatures of aqueous solutions of these copolymer increased with increasing of hydrophilic AMPS unit content in the copolymers. The glass transition temperature (Tg) of hydrogels showed a decrease by increasing of comonomer DMAEA content.     

4-(N,N-二甲氨基)苯甲酸的合成研究

讨论了 4- (N,N-二甲氨基 )苯甲酸的各种合成方法。认为 4- (N,N-二甲氨基 )苯甲醛在Na Cl O2 -乙腈体系中被氧化成 4- (N,N-二甲氨基 )苯甲酸具有操作简便、成本低 ,适合工业化生产     

可聚合单体N,N-二甲基丙烯酰乙二胺的合成条件研究

利用丙烯酸和苯甲酰氯合成丙烯酰氯(AC),AC再与N,N-二甲基乙二胺(DMAEA)合成可聚合单体N,N-二甲基丙烯酰乙二胺。通过红外光谱和核磁共振谱证实产物的结构。考察原料的物质的量比、不同缚酸剂的用量与浓度、稀释N,N-二甲基乙二胺和丙烯酰氯的二氯甲烷的量、加料顺序对产品收率的影响,得出适宜的实验条件为:n(DMAEA)∶n(AC)=1∶1.2,缚酸剂w(NaOH)=25%的用量为25mL,稀释N,N-二甲基乙二胺和丙烯酰氯的二氯甲烷的量分别为80mL和45mL,加料顺序为先加N,N-二甲基乙二胺的二氯甲烷溶液,再加缚酸剂。在上述条件下,产品最高收率可达83%。     

Online monitoring of the copolymerization of 2-(dimethylamino)ethyl acrylate with styrene by RAFT. Deviations from reaction control

Kinetics of copolymerization reactions of 2-(dimethylamino)ethyl acrylate (DMAEA) and styrene by reversible addition fragmentation transfer (RAFT) in N,N-dimethylformamide (DMF) are reported. Novel approaches in the online monitoring of the synthesis of the amphiphilic copolymers by Automatic Continuous Online Monitoring of Polymerization reactions (ACOMP) are presented. Automatic withdrawal of separate reactor streams and their subsequent dilution throughout the reaction with organic and aqueous solvents, respectively, allowed different features to be captured. Thus, light scattering data combined with spectroscopic and viscometric measurements in DMF, together with conductivity measurements in aqueous medium provided in real time comonomer conversion, copolymer mass, reduced viscosity, and composition. Continuous data gathered allowed observing and quantifying the DMAEA-linked macroRAFT control agent decomposition, with significant effects on the reaction kinetics. Deviations from controlled behavior were investigated during (co)polymerization reactions under different conditions.Multi-detector Size Exclusion Chromatography (SEC) and NMR were used to bring additional information on the system investigated.     

A new catalytic transesterification for the synthesis of N, N-dimethylaminoethyl acrylate with organotin catalyst

A new transesterification method for preparing N, N-dimethylaminoethyl acrylate (DMAEA) from methyl acrylate (MA) and dimethylaminoethanol (DMAE) was carried out in the presence of organotin catalyst. Among the catalysts examined, (C₈H₁₇)₂Sn(OCOC₁₁H₂₃)₂(TD) is the most active one for the reaction. The products were characterized by gas chromatography, IR spectroscopy, NMR spectroscopy and Mass spectroscopy. The effects of various reaction conditions such as the different catalysts, the reactants ratio, the amount of catalyst, the reaction time on the DMAE conversion, the selectivity to DMAEA and the DMAEA yield were investigated. Experimental results indicated that the sort of catalyst is vital to improving DMAEA yield. The reactants ratio could effect on the DMAE conversion, the selectivity to DMAEA and the DMAEA yield. The 96.28% conversion of DMAE was obtained over catalyst TD, the yield of DMAEA could reach 94.65%, the selectivity is 98.68%. A possible catalytic mechanism of transesterification of DMAE and MA with organotin catalysts was also presumed.     

Synthesis and antimicrobial activity of some cross‐linked copolymers with alkyl chains of various lengths

Amphoteric polymer hydrogels were prepared by the copolymerization of three kinds of N,N′‐dimethyl‐N‐alkylmethacryloxylethyl ammoniumbromide (DMAEA) with different lengths of alkyl chains (DMAEA‐RB) (R‐ehtyl/hexyl/dodecyl), acrylic acid (AA), and acrylamide (AM). The water content of the AA‐AM‐(DMAEA‐RB) terpolymers decreased with the increasing length of alkyl chains in quaternary ammonium group in the terpolymers and increased with the increasing molar ratio of DMAEA‐RB to 2 mol % and then decreased. Their antibacterial activities against Escherichia coli and Staphylococcus hyicus were investigated by a colony count method. It was found that the copolymer exhibited higher antibacterial activity with increasing chain length of alkyl groups in ammonium groups. For P[AA‐AM‐(DMAEA‐DB)], the DMAEA‐DB content is higher and contact time is longer, its antibacterial activity is better. However, when the contact time and quaternary ammonium content were above 30 min and 2%, respectively, the amount of live cells N(t) in a cell suspension increased in the presence of P[AA‐AM‐(DMAEA‐EB)] or P[AA‐AM‐(DMAEA‐HB)]. © 2010 Wiley Periodicals, Inc. J Appl Polym Sci, 2011     

Synthesis and water absorbency of polyampholytic hydrogels with antibacterial activity

Amphoteric terpolymers of acrylic acid (AA), acrylamide (AM), and N,N′‐dimethyl‐N‐ethylmeth‐acryloxylethylammoniumbromide (DMAEA‐EB) with varied compositions P[AA‐AM‐(DMAEA‐EB)] were synthesized by inverse suspension polymerization. The components of P[AA‐AM‐(DMAEA‐EB)] were verified by FTIR spectroscopy. The water absorption ability and antibacterial activity of the copolymer against Escherichia coli(E. coli) and Staphylococcus hyicus(S. hyicus) suspended in sterilized physiological saline were investigated. The introduction of  N⁺R₄ may increase the water absorbency of P[AA‐AM‐(DMAEA‐EB)] in some degree because of the excellent hydrophilicity of  N⁺R₄. The AA‐AM‐(DMAEA‐EB) hydrogels exhibited high antibacterial activity against bacteria tested. The process of adsorption between live bacteria cells and resins was at least partially reversible. A peak of antibacterial efficiency existed with increasing contact time. The resin killed 96.6% E. coli organisms and 90.3% S. hyicus organisms, respectively, within 30 min of contact at dosage of 0.1g. The concentration of DMAEA‐EB has a special effect on the antibacterial activity of the polyampholytic hydrogels, which is different from polycation. It was observed that the antibacterial activity of the resin with 2 mol % of DMAEA‐EB is superior to the copolymers tested with other compositions. © 2009 Wiley Periodicals, Inc. J Appl Polym Sci, 2009     

pH- and thermo-multi-responsive fluorescent micelles from block copolymers via reversible addition fragmentation chain transfer (RAFT) polymerization

Well-defined pH- and thermo- multi-responsive fluorescent micelles based on the self-assembly of diblock copolymers poly[(N-isopropyl-acrylamide-co-N-vinylcarbazole)-b-2-(dimethylamino)ethyl acrylate], (PNIPAAM-co-PNVC)-b-PDMAEA, are described. The diblock copolymers are prepared via the reversible addition fragmentation chain transfer (RAFT) copolymerization of N-isopropyl-acrylamide (NIPAAM) and N-vinylcarbazole (NVC) followed by chain extension in presence of 2-(dimethylamino)ethyl acrylate) (DMAEA). The micelles are formed in aqueous solutions in a wide range of temperature (25-60 °C), and their sizes increase from 40 to 65 nm when varying pH from basic to acidic. The cross-linking of the PDMAEA-containing shell with 1,2-bis(2-iodoethoxy)ethane (BIEE) results in spherical soft nanoparticles which size is increased by 20-25% when compared to the micelles. The presence of NVC in concentrations as low as 4% in the core of the micelles allow the nanoparticles to be tagged by fluorescence, making them well suited for therapeutic applications.     

Synthesis and characterization of novel sulfobetaines derived from 2,4‐tolylene diisocyanate

Novel sulfobetaines were synthesized from two urethanes derived from 2,4‐tolylene diisocyanate (TDI) blocked with 2‐hydroxyethyl methacrylate (HEMA) and either N,N‐dimethylaminopropylamine (DMAPA) or N,N‐dimethylaminoethanolamine (DMAEA). The first‐stage reaction of TDI with HEMA was carried out in petroleum ether heterogeneously with the precipitation of the intermediate monoadduct product in the reaction solution. The second stage is a homogeneous reaction of the monoadduct with the blocking agent, DMAPA or DMAEA, in tetrahydrofuran (THF). In both reactions, an inhibitor, hydroquinone, and a catalyst, dibutyltin diacetate (DBDAc), were used. The tertiary amine urethanes were quaternized by 1,3‐propane sultone to form the two novel sulfobetaines. The results of the elemental analysis of those products along with their ¹H‐NMR and IR spectra indicated that these materials were, indeed, the compounds expected. The products dissolved in strongly polar organic solvents. The copolymerization of these two monomers with comonomers such as styrene, methyl methacrylate, acrylamide, and HEMA was investigated. © 2001 John Wiley & Sons, Inc. J Appl Polym Sci 82: 3447–3459, 2001