Photoinitiated synthesis of poly(poly(ethylene glycol) methacrylate-co-diethyl amino ethyl methacrylate) superabsorbent hydrogels for dye adsorption

Random copolymers of poly(ethylene glycol) methacrylate (PEGM), and diethyl amino ethyl methacrylate (DEAEM) were synthesized at low, and high conversions by photoinitiation. Crosslinked poly(PEGM-co-DEAEM) samples were obtained, and characterized by FTIR, SEM, DSC, TGA, and elemental analyses. Swelling behavior of the copolymers revealed that the copolymers acted as superabsorbent hydrogels. The monomer reactivity ratios were calculated using Fineman Ross, Extended Kelen Tüdøs , and Mayo Lewis methods that gave r₁(PEGM) = 0.90, r₂(DEAEM) = 0.14 at low conversions. At high conversions r₁ and r₂ values were calculated as 1.01 and 0.40, respectively. Adsorption isotherms of methyl orange (MO) onto hydrogels were studied using Langmuir, Freundlich, and Temkin models. The experimental data fitted well with the Langmuir equation. The maximum adsorption capacity for MO was 212.7 mg g⁻¹ at pH = 3. The adsorption data gave best fit with the pseudo-second order kinetic model. Thermodynamic evaluation showed spontaneous nature for MO adsorption onto poly(PEGM-co-DEAEM) hydrogels. © 2019 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2019 , 136, 47707.     

One‐pot synthesis of self‐stabilized and carboxyl‐functionalized fluorescent poly(methyl methacrylate) microspheres covalently dyed with tris(8‐hydroquinolinato)aluminium by dispersion polymerization

The dispersion polymerization of methyl methacrylate (MMA) with fluorescent monomer tris[2‐((8‐hydroxyquinolin‐5‐yl)methoxy)ethyl methacrylate]aluminium (Al‐HQHEMA) was investigated to obtain fluorescent microspheres under varying conditions (such as composition of dispersion medium, and content of stabilizer polyvinylpyrrolidone (PVP) and Al‐HQHEMA) in methanol–water at 70 °C with 2,2′‐azoisobutyronitrile as the initiator. Fluorescent microspheres with particle size of 2.039 µm and uniformity of 0.171 were obtained under the following conditions: methanol–water, 7:3 (v/v); PVP, 15 wt% of MMA; Al‐HQHEMA solution, 1.5 mL. Maleic monoester of monomethoxyl poly(ethylene glycol) (Mal‐MPEG) was used as a comonomer to simultaneously incorporate carboxyl groups and PEG chains. With Mal‐MPEG, no aggregation was observed in the measurements of particle size and size distribution for the obtained microspheres after cleaning off PVP, indicating that self‐stabilized fluorescent microspheres were obtained. While without Mal‐MPEG, obvious aggregation was observed. The determination of surface carboxyl content using aqueous acid–base titration showed that most of the carboxyl groups of Mal‐MPEG were located on the surface of the microspheres. © 2015 Society of Chemical Industry     

Temperature control in Lowicryl K4M and glycol methacrylate during polymerization: is there a low-temperature embedding method?

An apparatus for embedding tissues at resin temperatures down to 228 K is described. By placing thermocouples in the resin the temperature has been monitored during embedding at low temperature with glycol methacrylate (GMA) and Lowicryl K4M. Even in this apparatus with a liquid cooling bath the heat of polymerization is not dissipated and the resin temperature rises. This rise is directly proportional to the resin temperature at the onset of polymerization and is higher in Lowicryl K4M than GMA. The initial resin temperature also affects the time taken for polymerization. The time to the onset of the peak and its duration are both increased as the temperature is lowered. This effect is more pronounced with GMA than Lowicryl K4M and polymerization of GMA is inhibited at the lowest temperature used. When Lowicryl K4M, polymerized at low temperature, is warmed up to ambient a further exothermic reaction occurs, which causes the resin temperature to rise well above ambient. Both this temperature peak and that during polymerization are reduced, but not totally eliminated, by reducing the resin volume. Aircooled systems are inefficient compared with the low-temperature apparatus used here and the resin temperature rise is consequently greater and, even with small resin volumes, it can be very high. It is therefore unlikely for published methods that the temperature specified has been maintained in the resin during polymerization. The implications of these findings are discussed in relation to enzyme and antigen survival. Recommendations include use of very small volumes of resin, refrigerated liquid-bath rather than air-cooled systems and contact with a heat sink when specimens are warmed up to ambient temperature. Examples of enzyme reaction, antigen survival and structural preservation obtained with the method are presented.     

A new,less toxic polymerization system for the embedding of soft tissues in glycol methacrylate and subsequent preparing of serial sections

The paper describes a new polymerization system for embedding soft tissues in glycol methacrylate (GMA). The polymerization of GMA is initiated by means of a barbituric acid derivative in combination with chloride ions and dibenzoyl peroxide. The catalyst system contains no aromatic amines which constitutes a toxicological advantage over the commonly employed system of peroxide/aromatic amine. Clear blocks are obtained from which 1–2 μm sections are easy to cut. In combination with an appropriate softener, polyethylene glycol 400 , serial sectioning may be practised.     

甲基丙烯酸甲酯—苯乙烯共聚物分子质量的研究

在６０～９０℃温度范围内,以ＡＩＢＮ为引发剂进行了甲基丙烯酸甲酯（ＭＭＡ）－苯乙烯（Ｓｔ）本体自由基共聚合,用粘度法测定了共聚物的分子质量。在转化率０～９５％范围内,研究了聚合温度、引发剂浓度及单体配比对ＭＭＡ－Ｓｔ共聚物分子质量的影响规律,结果表明自由基聚合过程中凝胶效应使共聚物分子质量随转化率升高而显著增大;推导并关联了共聚物平均分子质量模型,在凝胶效应出现之前,该模型计算值与实验值平均偏差８％,为ＭＭＡ－Ｓｔ共聚物的生产控制提供了理论依据。     

丁炔二醇中微量甲醛的分光光度测定研究

用３甲基２苯并噻唑酮腙（ＭＢＴＨ）作显色剂,用分光光度法测定了丁炔二醇中微量甲醛．表观摩尔吸光系数为５．１７×１０４Ｌ·ｍｏｌ－１·ｃｍ－１,最低检测限为４．８μｇ／Ｌ,加标回收率９９％以上,相对标准偏差小于３％．醛含量在０～１．４ｍｇ／Ｌ范围服从比尔定律．方法重复性好,灵敏度高,操作简便,能满足丁炔二醇质量控制分析要求．     

Fabrication of ultralight 3D graphene/Pt aerogel via in situ gamma-ray irradiation and its application for the catalytic degradation of methyl orange

Abstract

In this work, we reported a facile and environmentally friendly approach for the preparing of 3D graphene/Pt aerogel by gamma irradiation at room temperature. Graphene oxide (GO) and platinum ion are simultaneously reduced and self-assembled into a three-dimensional (3D) macro porous structure. Pt NPs with diameter between 2.3 and 5.5?nm were homogeneously attached onto the graphene sheets of the 3D network structure. The catalytic efficiency towards the degradation of methyl orange (MO) of the 3D GA/Pt composite is 108 times higher than that of the pure Pt NPs under the same experimental conditions.     

在聚砜微滤膜表面接枝聚合叔胺单体DMAEMA及接枝膜对水介质中毒性阴离子的吸附与分离特性

采用相转化法制得了氯甲基化聚砜(CMPSF)微孔滤膜,以乙二胺为试剂对CMPSF膜进行化学改性,膜表面的伯胺基与水溶液中的过硫酸铵构成表面引发体系-NH_2/S_2O_8~(2-),使叔胺单体甲基丙烯酸二甲基氨基乙酯(DMAEMA)发生接枝聚合,获得了多孔接枝膜PSF-g-PDMAEMA。考察了接枝聚合的规律,对接枝膜进行了充分表征,考察研究了接枝膜对2种毒性阴离子CrO_4~(2-)及MoO_4~(2-)离子的吸附性能和膜分离去除行为。研究结果表明,控制水溶液中过硫酸铵的质量分数为1%,温度为50℃,可制得PDMAEMA接枝度为0.64 mg/cm~2的接枝膜。在酸性及中性水溶液中,凭借强烈的静电相互作用,多孔接枝膜PSF-g-PDMAEMA对毒性阴离子CrO_4~(2-)离子及MoO_4~(2-)离子均会产生强吸附作用;以该多孔接枝膜为滤膜进行膜分离过程,通过选择性吸附,可有效地去除水介质中的CrO_4~(2-)离子。     

超声波本体聚合在甲基丙烯酸甲酯-Al2O3陶瓷膜注凝成型中的应用研究

通过探讨水浴加热预聚合、微波恒温预聚合、微波预聚合及超声预聚合反应方式对甲基丙烯酸甲酯(MMA)进行预聚合反应,来确定适合作为Al2O3陶瓷膜注凝成型工艺中的预混液制备方式。结果表明:超声的空化作用能够有效地加快预聚合的反应速率,且在预聚合反应过程中,超声波的机械振动作用使MMA反应均匀,且不会发生局部爆聚现象。适合作为MMA预聚合的引发剂为偶氮二异丁腈(AIBN),其最佳用量为0.08%。发现微波的"致热效应"是MMA聚合速率加快的原因。     

醋酸甲酯在离子交换树脂上的水解动力学

本文用间歇搅拌釜式反应器对醋酸甲酯在离子交换树脂上的水解动力学进行了实验测定,得出了消除内外扩散影响的水解反应速率数据,归纳出了通用的动力学方程。其过程满足单点吸附机理,受表面反应控制。