甲基丙烯酸二甲氨基乙酯合成方法的改进

甲基丙烯酸二甲氨基乙酯是含有强碱性氨基和可聚合的乙烯基的单体,具有广泛的用途［１］。它的合成方法主要是酯交换法和酰氯法。酯交换法多采用碱金属的烷氧基化合物作催化剂,对苯二酚作阻聚剂,但由于反应温度高,反应时间长,聚合现象十分严重,产率通常只有４０％～５０％。酰氯法是由甲基丙烯酰氯与二甲氨基乙醇反应制取,这一方法反应条件温和,有效地避免了聚合反应的发生,但反应过程中会产生氯化氢,需加入碱性物质吸收。Ｒｏｗｅｌｌ等人报道用三乙胺作为缚酸剂,酯化产率仅为２５％［２］。本文直接用反应物二甲氨基乙醇作为缚…     

甲基丙烯酸二甲氨基乙酯合成与应用概述

综合文献资料介绍了甲基丙烯酸二甲氨基乙酯的性质、合成方法及应用前景。     

甲基丙烯酸二甲氨基乙酯合成与应用概述

综合文献资料介绍了甲基丙烯酸二甲氨基乙酯的性质、合成方法及应用前景。     

二乙基氨基甲基丙烯酸乙酯的研制

研究了以二乙基氨基乙醇与甲基丙烯酸甲酯为原料 ,二丁基月桂酸锡为催化剂合成二乙基氨基甲基丙烯酸乙酯 (DEAM)的最佳工艺条件。详细考察了配比 ,反应温度及时间对产物收率的影响     

甲基丙烯酸二甲氨基乙酯的合成方法

简要地评述用丙烯酸甲酯或甲基丙烯酸甲酯与二甲氨基乙醇进行酯交换反应是丙烯酸二甲氨基乙酯、甲基丙烯酸二甲氨基乙酯实现工业化生产的重要方法。     

甲基丙烯酸二甲氨基乙酯的气相色谱分析

采用气相色谱分析法,在选定的实验条件下,定量地对甲基丙烯酸二甲氨基乙酯进行分析。该法精密度高、操作简单、分析快速。     

甲基丙烯酸二甲氨基乙酯的制备

介绍了以甲基丙烯酸甲酯（MMA）与二甲氨基乙醇（DMAE）为原料，铅作催化剂来制备甲基丙烯酸二甲氨基乙酯（DMA）的方法，讨论了不同反应物配比，反应温度与反应压力等条件对反应产率的影响，得出了反应的最佳条件。     

甲基丙烯酸二甲氨基乙酯的制备

介绍了以甲基丙烯酸甲酯 (MMA)与二甲氨基乙醇 (DMAE)为原料 ,铅作催化剂来制备甲基丙烯酸二甲氨基乙酯 (DMA)的方法 ,讨论了不同反应物配比、反应温度与反应压力等条件对反应产率的影响 ,得出了反应的最佳条件。     

聚甲基丙烯酸二乙氨基乙酯磁性纳米凝胶的基因转染性能研究

本文以聚甲基丙烯酸二乙氨基乙酯一磁性纳米凝胶作为作为转基因载体,考察了其对细胞的毒性作用及期基因转染的性能,为磁性纳米凝胶在生物医学领域的应有提供了一条新途径。     

Reversible pH-Responsive Hydrogels of Softwood Kraft Lignin and Poly[(2-dimethylamino)ethyl Methacrylate]-based Polymers

Softwood kraft lignin (SKL) pH-responsive hydrogels were prepared through controlled aggregation using poly[2-(dimethylamino)ethyl methacrylate] (PDMAEMA) and poly(2-(dimethylamino)ethyl methacrylate)-block-poly(ethylene oxide)-block-poly(2-(dimethylamino) ethyl methacrylate) triblock copolymer (PDMAEMA-co-PEO-co-PDMAEMA). At low SKL concentrations, the SKL/polymer (PDMAEMA and PDMAEMA-co-PEO-co-PDMAEMA) aqueous solutions exhibited pH-dependent aggregation arising from the formation of strong intermolecular hydrogen bonds. Decreasing the SKL/polymer weight ratio resulted in the pH-reversible soluble-insoluble (S-I) transition to become a soluble-insoluble-soluble (S-I-S) transition, which upon increasing the SKL concentration resulted in hydrogel formation. Under neutral conditions relatively strong hydrogels were formed, which upon either increasing or decreasing solution pH resulted in the hydrogels collapsing to liquid solutions, but were readily reformed upon neutralization. The effects of polymer structure, concentration, and intermolecular interactions on solution behavior and gelation are thoroughly discussed.     

甲基丙烯酸乙基咔唑酯的合成与表征

以新型光电材料的一种原料羟乙基咔唑和甲基丙烯酸甲酯为原料,对甲苯磺酸为催化剂,对苯二酚为阻聚剂,采用酯交换法合成甲基丙烯酸乙基咔唑酯。采用紫外光谱(UV-vis)傅立叶变换红外光谱(FT-IR)对产物的结构进行了表征。     

己酸二乙氨基乙醇酯亚慢性经口毒性

按照GB15670-1995的要求进行了己酸二乙氨基乙醇酯（DA-6）90d的亚慢性经口毒性试验。结果显示,与对照组相比,雌、雄性大鼠高剂量组的体重增长明显减慢（p〈0．05）;雄性大鼠高剂量组AST、ALB两项指标升高（p〈0．05）,肝、肺脏器系数增长（p〈0．05）。高、中剂量组雌、雄性大鼠发生心肌小灶炎症和肾脏小灶炎症的动物数明显增多。根据试验结果,受检样品己酸二乙氨基乙醇酯对大鼠的无作用剂量为：雄性40．2mg/kg bw／d,雌性49．1mg／kg bw／d。     

Fast, multi-responsive microgels based on photo-crosslinkable poly(2-(dimethylamino)ethyl methacrylate)

Multi-responsive microgels based on poly(2-(N,N-dimethylamino)ethyl methacrylate) were developed and their properties were investigated. The primary goal of this research was to speed up the stimulus-response time of the hydrogels to a level usable for actuator applications, by reducing the diffusion distance of water. The gels were prepared by a UV induced photodimerization of a copolymer of 2-(dimethylamino)ethyl methacrylate and 4-cinnamoyl-phenyl methacrylate. Patterning studies showed that these materials can be used as photo-resist materials with high resolution at short exposure times. They showed lower critical solution temperature behavior in water, as well as pH dependent solubility and swelling ratios. While 1 mm thick gels showed response times to temperature and pH-changes of several hours, Si-supported microgels of 300 nm thickness had response times in the range of only a few seconds. The copolymer was prepared by free radical copolymerization, and the reactivity ratios were determined with the extended Kelen Tudos method. Spin-coating of this copolymer on Si supports and subsequent UV-irradiation yielded microgels of variable thickness (200 nm-15 μm), which was determined by confocal scanning laser microscopy. Surface plasmon resonance spectroscopy measurements demonstrated the fast, stimuli-responsive swelling behavior, while differential scanning calorimetry gave insight into the morphology of the networks.     

甲基丙烯酸2-(二乙氧基硫代磷酰氧基)乙基酯的合成及应用

以甲基丙烯酸-β-羟乙酯(HEMA)与O,O-二乙基硫代磷酰氯为原料,在三乙胺作缚酸剂,氯化亚铜(CuCl)作催化剂的条件下,合成了甲基丙烯酸2-(二乙氧基硫代磷酰氧基)乙基酯(DPTEM)阻燃剂,再与丙烯腈共聚得到了阻燃聚丙烯腈共聚物。在n(HEMA)/n(三乙胺)=1,m(CuCl)/m(HEMA)=0.01~0.02,反应温度0~5℃条件下,DPTEM的产率达82%;通过FTIR、1HNMR、MS测试技术表征了DPTEM的结构,证明产品结构正确。丙烯腈共聚物中w(DPTEM)=25%时,极限氧指数(LOI)值可达27。该工艺已通过中试,正在进行扩大化生产。     

甲基丙烯酸-N,N-2-甲基乙胺酯原子转移自由基聚合动力学研究

A kinetic model was developed to describe the atom transfer radical polymerization (ATRP) of 2-(N,N-dimethylamino) ethyl methacrylate (DMAEMA). The model was based on a polymerization mechanism,which included the atom transfer equilibrium for primary radical, the propagation of growing polymer radical, and the atom transfer equilibrium for the growing polymer radical. An experiment was carried out to measure the conversion of monomer, the number-average molecular weight of polymer and molecular weight distribution for the ATRP process of DMAEMA. The experimental data were used to correlate the kinetic model and rate constants were obtained. The rate constants of activation and deactivation in the atom transfer equilibrium for primary radical are 1.0 x 104 L·mol-1.s-1 and 0.04 L·mol-1.s-1, respectively. The rate constant of the propagation of growing polymer radical is 8.50 L·mol-1.s-1, and the rate constants of activation and deactivation in the atom transfer equilibrium for growing polymer radical are 0.045 L.mol-1.s-1 and 1.2 × 105 L·mol-1.s- 1, respectively. The values of the rate constants represent the features of the ATRP process. The kinetic model was used to calculate the ATRP process of DMAEMA. The results show that the calculations agree well with the measurements.     

正己酸二乙氨基乙酯的合成及反应动力学

[目的]以正己酸和二乙氨基乙醇为原料,阳离子交换树脂催化合成正己酸二乙氨基乙酯.考察了反应过程的影响因素,测定了动力学数据.[结果]合成工艺条件,n(正己酸):n(二乙氨基乙醇)为2.0:1,催化剂用量为正己酸和二乙氨基乙醇总质量的2%,甲苯用量为正己酸和二乙氨基乙醇总体积的110%,反应温度不超过130℃,反应时间3.0 h,二乙氨基乙醇的转化率达95.6%,催化剂重复使用4次后,二乙氨基乙醇的转化率为92.8%.表观活化能为73.219 kJ/mol,指前因子为1.9323×107L/(mol·min).[结论]阳离子交换树脂具有较好的催化活性和稳定性,该酯化反应对正己酸和二乙氨基乙醇均为一级反应.     

Copolymerizations of 2-(dimethylamino)ethyl methacrylate with (methyl)acrylates initiated by a neutral Pd(II)-based complex

The copolymerization reactions of 2-(dimethylamino)ethyl methacrylate (DMAEMA) with methyl methacrylate (MMA), butyl methacrylate (n-BMA), methyl acrylate (MA), and butyl acrylate (n-BA), respectively, by an environmentally stable palladium acetylide Pd(PPh₃)₂(CCPh)₂ (PPP) have been investigated. PPP shows relatively high catalytic activity for these copolymerizations. Reactivity ratios of these copolymerizatins have been measured and calculated by the Kelen-Tüdös method for the first time, and their values are as follows: (1) r_DMAEMA=1.13, r_MMA=1.07; (2) r_DMAEMA=0.77, r_n-BMA=0.84; (3) r_DMAEMA=1.54, r_MA=0.09; (4) r_DMAEMA=0.71, r_n-BA=0.14. The mechanism of these copolymerizations was discussed and a radical mechanism was proposed.     

The homo and copolymerisation of 2-(dimethylamino)ethyl methacrylate in supercritical carbon dioxide

This paper describes the free radical dispersion homopolymerisation of 2-(dimethylamino) ethyl methacrylate (DMA) and copolymerisation of DMA with methyl methacrylate (MMA) in supercritical carbon dioxide (scCO₂). The polymerisations are performed in the presence of two commercially available stabilisers, poly(dimethylsiloxane) monomethacrylate macromonomer (PDMS-mma) and the carboxylic acid terminated perfluoropolyether (Krytox 157FSL). Dry, fine powdered polymer product was produced for the copolymer under optimised conditions, but only aggregated solid is formed for homo poly(DMA). The effect of reaction time, stabiliser, copolymer composition and reaction pressure on the yield, molecular weight and morphology of the copolymers has been investigated.     

(S)-2-(ethyl propionate)-(O-ethyl xanthate)- and (S)-2-(Ethyl isobutyrate)-(O-ethyl xanthate)-mediated RAFT polymerization of vinyl acetate

(S)-2-(Ethyl propionate)-(O-ethyl xanthate) (X1) and (S)-2-(Ethyl isobutyrate)-(O-ethyl xanthate) (X2) were used as the reversible addition-fragmentation chain transfer (RAFT) agents for the radical polymerization of vinyl acetate (VAc). The former showed the better chain transfer ability in the polymerization at 60°C. Kinetic study with both RAFT agents showed pseudo-first order kinetics up to around 85% monomer conversion. Molecular weight of the resulting polymer increased linearly with increase in the monomer conversion up to around 85%. The observed molecular weights calculated from ¹H-NMR spectrum [M_n(NMR)] are close to the corresponding theoretical molecular weights [M_n(theor)]. The corresponding polydispersity index (PDI) of the resulting polymers remained almost constant at around 1.2 up to ∼ 65% monomer conversion and then increased gradually with the further increase in the monomer conversion. Chain-end analysis of the resulting polymers by ¹H-NMR showed clearly that polymerization started with the radical forming out of the xanthate mediator. The negligible homo-chain extension and the hetero-chain extension involving synthesis of poly(VAc)-b-poly(NVP) diblock copolymer were occurred. © 2012 Wiley Periodicals, Inc. J Appl Polym Sci, 2012