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IR, 1H NMR, Electronic Properties and Conductivity Studies of N1 ,N4-Bis(Diphme)Benzene-l,4-Diamine Chloride Zirconium (IV) [{(Ar)2NC6H5N(Ar)2}ZrCl4] (Ar = C6H5)
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作者 Salem Et. Ashoor 《Journal of Chemistry and Chemical Engineering》 2011年第3期259-263,共5页
A range of new compounds such as N1,N4-bis(diphenylmethlene)benzene-l,4-diamine zirconium (IV) chloride [{(Ar)2NC6HsN(Ar)z}ZrCl4] (Ar = C6H5) complex counting the chelating amine and chloride in position tra... A range of new compounds such as N1,N4-bis(diphenylmethlene)benzene-l,4-diamine zirconium (IV) chloride [{(Ar)2NC6HsN(Ar)z}ZrCl4] (Ar = C6H5) complex counting the chelating amine and chloride in position trans have been prepared. Well-defined NI,N4-bis(diphenylmethlene)benzene-l,4-diamine zirconium (IV) chloride [{(Ar)2NC6H5N(Ar)2}ZrCl4] (Ar = C6H5) was obtained by stoichiometric addition of {(Ar)2NC6H5N(Ar)2} (Ar = C6H5) and {ZrC14} in ethanol at reflex temperature. IR, 1H NMR, electronic properties using hyperchem program study has been improved for this compound such as bond distance, and this compound was also defined as electric conductivity which proves to be useful for conductively compound. 展开更多
关键词 Electronic conductivity nI n4-bis(diphme)benzene-1 4-diamine n1 n4-bis(diphenylmethlene)benzene-1 4-diaminezirconium (IV) chloride.
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POLYMERIZATION OF N,N'-(PYROMELLITOYL)-BIS-L-LEUCINE DIACID CHLORIDE WITH HYDANTOIN DERIVATIVES BY MICROWAVE IRRADIATION
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作者 Khalil Faghihi 《Chinese Journal of Polymer Science》 SCIE CAS CSCD 2004年第4期343-348,共6页
Facile and rapid polycondensation reactions of N,N'-(pyromellitoyl)-bis-L-leucine diacid chloride 1 with eight different derivatives of hydantoin compounds 2a-h were developed by using a domestic microwave oven in... Facile and rapid polycondensation reactions of N,N'-(pyromellitoyl)-bis-L-leucine diacid chloride 1 with eight different derivatives of hydantoin compounds 2a-h were developed by using a domestic microwave oven in the presence of a small amount of polar organic medium such as o-cresol. The polycondensation reactions proceeded rapidly, compared with the conventional solution polycondensation, and was completed within 7-10 min, producing a series of novel optically active poly(amide-imide)s 3a-h with high yield and inherent viscosity of 0.35-0.65 dL/g. All of the above polymers were fully characterized by FT-IR, elemental analyses, inherent viscosity (η inh ), solubility test and specific rotation. Some structural characterization and physical properties of these optically active poly(amide-imide)s are reported. 展开更多
关键词 Microwave-assisted rapid polycondensation Optically active polymers Poly(amide-imide)s Hydantoin derivatives n n'-(Pyromellitoyl)-bis-L-leucine diacid chloride
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A Novel 2D Architecture from Bismuth and Flexible Ligand N,N'-Diacetic Acid Imidazolium Chloride
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作者 柴小川 张汉辉 +5 位作者 张帅 雷然 陈义平 孙燕琼 孙瑞卿 杨齐愉 《Chinese Journal of Structural Chemistry》 SCIE CAS CSCD 2009年第11期1343-1348,共6页
A new compound {[Bi(trans-DAM)(cis-DAM)(H2O)]NO3·H2O}n 1 derived from bismuth and the flexible ligand N,N'-diacetic acid imidazolium chloride (H2DAMCl) was obtained by hydrothermal synthesis and characte... A new compound {[Bi(trans-DAM)(cis-DAM)(H2O)]NO3·H2O}n 1 derived from bismuth and the flexible ligand N,N'-diacetic acid imidazolium chloride (H2DAMCl) was obtained by hydrothermal synthesis and characterized by single-crystal X-ray diffraction. Compound 1 crystallizes in the monoclinic P21/c space group with a = 9.2298(18), b = 13.339(3), c = 17.090(3) , β = 105.38(2)°, V = 2028.7(7)A^3, Z = 4, C14H18N5O13Bi, Mr = 673.31, Dc = 2.204 g/cm^3, F(000) = 1296, μ = 8.772 mm-1, the final R = 0.0472 and wR = 0.1441 for 4129 observed reflections (I 〉 2σ(I)). In 1, the carboxylic groups from DAM- ligands adopt a cheating mode to link bismuth ions to form a 2D sheet network. These sheets are further connected by hydrogen bonding interactions to give an interesting 3D supramolecular framework. 2D correlation analysis of IR of 1 with thermal and magnetic perturbation was introduced to ascertain the characteristic adsorption of the groups overlapped in the 1D IR spectrum. Additionally, compound 1 exhibits fluorescent emission at room temperature. 展开更多
关键词 n n'-diacetic acid imidazolium chloride BISMUTH crystal structure 2D correlation analysis of IR
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EXTRACTION OF Zn AND Cd FROM CHLORIDE LIQUORS BY TRI-n-BUTYL PHOSPHATE
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《Acta Metallurgica Sinica(English Letters)》 SCIE EI CAS CSCD 1991年第7期1-7,共7页
Studies have been made on the extraction of Zn and Cd by TBP(tri-n-butyl phosphate) from diluent hydrochloric acid solutions of soldium chloride.The experiments show that the species extracted from diluent HCI solutio... Studies have been made on the extraction of Zn and Cd by TBP(tri-n-butyl phosphate) from diluent hydrochloric acid solutions of soldium chloride.The experiments show that the species extracted from diluent HCI solutions of NaCl appear to be predominantly ZnCl_2· 2TBP and CdCl_2·2TBP.For Cd,at lower acidities,anionic complexes of the type H_2CdCl_3 are also extracted.As the acidity is increased,H_2CdCl_4 appear to be predominant complexes in organic phase.For Zn,the acidocomplexes of the type HZnCl_3 appear in organ- ic phase after the acidity of solutions reaching a certain value([HCl]>0.1 mol/L). Furthermore,the ultraviolet absorption spectra of both aqueous and organic phases have been studied,and the infrared spectra of the organic phases have been exomined.The extraction mechanism and temperature effect are also discussed. 展开更多
关键词 EXTRACTIOn solvent extraction Zn CD tri-n-butyl phosphate zinc chloride
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Nitrogen doped carbon catalyzing acetylene conversion to vinyl chloride 被引量:12
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作者 Xingyun Li Xiulian Pan Xinhe Bao 《Journal of Energy Chemistry》 SCIE EI CAS CSCD 2014年第2期131-135,共5页
Commercial production of vinyl chloride from acetylene relies on the use of HgCla as the catalyst, which has caused severe environmental problem and threats to human health because of its toxicity. Therefore, it is vi... Commercial production of vinyl chloride from acetylene relies on the use of HgCla as the catalyst, which has caused severe environmental problem and threats to human health because of its toxicity. Therefore, it is vital to explore alternative catalysts without mercury. We report here that N-doped carbon can catalyze directly transformation of acetylene to vinyl chloride. Particularly, N-doped high surface area mesoporous carbon exhibits a rather high activity with the acetylene conversion reaching 77% and vinyl chloride selectivity above 98% at a space velocity of 1.0 mL.min-l.g-1 and 200 ~C. It delivers a stable performa℃nce within a test period of 100h and no obvious deactivation is observed, demonstrating potentials to substitute the notoriously toxic mercuric chloride catalyst. 展开更多
关键词 ACETYLEnE HYDROCHLORInATIOn vinyl chloride MERCURY-FREE n doped carbon
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Amelioration of Saline Soil by the Application of Gypsum, Calcium Chloride, Rice Husk and Cow Dung 被引量:1
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作者 Mohammad Zulfikar Khan Mohammad Golam Azom +5 位作者 Mohammad Tipu Sultan Sudipta Mandal Mohammad Ariful Islam Rikta Khatun Shaikh Motasim Billah Abu Hena Mohammad Zulfikar Ali 《Journal of Agricultural Chemistry and Environment》 2019年第2期78-91,共14页
A pot experiment was conducted to investigate the effect of cow dung, rice husks, calcium chloride and gypsum on soil reclamation and compare the effect of organic and inorganic amendments on soil reclamation during t... A pot experiment was conducted to investigate the effect of cow dung, rice husks, calcium chloride and gypsum on soil reclamation and compare the effect of organic and inorganic amendments on soil reclamation during the period of 5th March to 20th April, 2017. The experiment was laid to fit a completely randomized design (CRD) with seven treatments [Reference soil (T0), Cow dung (T1), Rice husk (T2), Gypsum (T3), Calcium chloride (T4), Cow dung + Rice husk (T5) and Gypsum + Calcium chloride (T6)] each having three replications for this experiment. After incubation (45 days), the laboratory investigation was carried out in the Soil, Water and Environment Discipline, Khulna University, Khulna, Bangladesh. Results indicate that the individual or combined effect of gypsum (T3) was more effective in changing EC and SAR. Gypsum application in combination with calcium chloride (T6) improved the soil chemical properties by reducing the EC. Among the treatment, calcium chloride (T4) had a remarkable effect in reducing sodium adsorption ratio and gypsum had a remarkable effect in reducing pH. Cow dung (T1), rice husk (T2), combination of cow dung and rice husk (T5) were less effective to reduce EC, pH and SAR. It’s measured for soils of different soil amendments varied significantly 展开更多
关键词 AMELIORATIOn SALInE Soil COW DUnG Rice Husk GYPSUM Calcium chloride C/n Ratio
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Phase Regulation and Defect Passivation Enabled by Phosphoryl Chloride Molecules for Efficient Quasi‑2D Perovskite Light‑Emitting Diodes 被引量:1
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作者 Mingliang Li Yaping Zhao +10 位作者 Jia Guo Xiangqian Qin Qin Zhang Chengbo Tian Peng Xu Yuqing Li Wanjia Tian Xiaojia Zheng Guichuan Xing Wen‑Hua Zhang Zhanhua Wei 《Nano-Micro Letters》 SCIE EI CAS CSCD 2023年第8期181-191,共11页
Quasi-2D perovskites have attracted tremendous interest for application as lightemission layers in light-emitting diodes(LEDs).However,the heterogeneous n phase and non-uniform distribution still severely limit the fu... Quasi-2D perovskites have attracted tremendous interest for application as lightemission layers in light-emitting diodes(LEDs).However,the heterogeneous n phase and non-uniform distribution still severely limit the further development of quasi-2D perovskite LEDs(Pero-LEDs).Meanwhile,the increased defect density caused by the reduced dimension and grain size induces non-radiative recombination and further deteriorates the device performance.Here,we found that a series of molecules containing phosphoryl chloride functional groups have noticeable enhancement effects on the device performance of quasi-2D Pero-LEDs.Then,we studied the modification mechanism by focusing on the bis(2-oxo-3-oxazolidinyl)phosphinic chloride(BOPCl).It is concluded that the BOPCl can not only regulate the phase distribution by decreasing the crystallization rate but also remain in the grain boundaries and passivate the defects.As a result,the corresponding quasi-2D Pero-LEDs obtained a maximum external quantum efficiency(EQE_(max))of 20.82%and an average EQE(EQE_(ave))of around 20%on the optimal 50 devices,proving excellent reproducibility.Our work provides a new selection of molecular types for regulating the crystallization and passivating the defects of quasi-2D perovskite films. 展开更多
关键词 Quasi-2D perovskite Phosphoryl chloride functional group Crystallization control n phase control PASSIVATIOn
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Formation Characteristics of N-Nitrosodimethylamine during Chloramines of PolyDADMAC
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作者 Lahua Jin Chen Ge Jiayi Wang 《Journal of Environmental Protection》 2019年第12期1602-1611,共10页
Interactions of chloramine with organic nitrogen compounds during purification of water for drinking may generate carcinogenic N-nitrosodime-thylamine (NDMA) as byproduct, and it has been found that cationic amine-bas... Interactions of chloramine with organic nitrogen compounds during purification of water for drinking may generate carcinogenic N-nitrosodime-thylamine (NDMA) as byproduct, and it has been found that cationic amine-based water treatment polymers may be one of the important precursors of NDMA. We have analyzed experimentally the influence rule of NDMA formation during chlorination and disinfection, in order to provide technical support for reducing or even avoiding the formation of NDMA. The formation characteristics of nitrosamines during the chlorination of poly-diallyldimethylammonium chloride (polyDADMAC) have been studied during our experiments. The results show that the type of chlorinating agent is crucial for the generation of NDMA;if pH = 7, NDMA has the great potential formation;the NDMA potential formation increases with temperature. The yield of NDMA will be higher as the concentration of monochloramine is 1.5 to 2.5 times of the precursor;the variation of polymer with reaction time can explain the concentration of NDMA in terminal water of pipe network is higher than that in drinking water. 展开更多
关键词 n-nITROSODIMETHYLAMInE Poly-Diallyldimethylammonium chloride MOnOCHLORAMInE COCOnUT Charcoal SPE Tube
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CuCl-catalyzed Oxidative N-Demethylation of Arylamines with tButyl Hydroperoxide 被引量:3
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作者 LIAO Qian XI Chan-juan 《Chemical Research in Chinese Universities》 SCIE CAS CSCD 2009年第6期861-865,共5页
CuCl-catalyzed oxidative N-demethylation of arylamines proceeded in the presence of tert-butyl hydroperoxide. The one-electron transfer route of oxidative N-demethylation competed favorably with the H-atom abstraction... CuCl-catalyzed oxidative N-demethylation of arylamines proceeded in the presence of tert-butyl hydroperoxide. The one-electron transfer route of oxidative N-demethylation competed favorably with the H-atom abstraction route. 展开更多
关键词 ARYLAMInE Cuprous chloride Catalytic oxidation n-DEMETHYLATIOn tert-Butyl hydroperoxide
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A new method for introduction ω-side chain of prostanoid using Barton radical reaction
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作者 Yi Hua Zeng Guang Dian Han 《Chinese Chemical Letters》 SCIE CAS CSCD 2009年第3期253-255,共3页
A new method for introduction to-side chain of prostanoid was described in this note. Starting from acid chloride (3), via Barton radical reaction, a trans α,β-unsaturated ketone sython was introduced.
关键词 Acid chloride n-Hydroxy-2-thiopyridine Barton ester ω-Side chain of prostanoid
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氯化钠相转变 K-型卡拉胶/聚 N-异丙基丙烯酰胺共混凝胶的辐射合成及性质研究 被引量:13
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作者 张艳群 哈鸿飞 《高分子学报》 SCIE CAS CSCD 北大核心 2001年第4期485-488,共4页
用γ辐射技术合成了K 型卡拉胶 (KC)与聚N 异丙基丙烯酰胺共混凝胶 (Blendgels) .合成产物透明 ,有弹性和较好的力学强度 .对不同条件下共混凝胶性能的测定结果表明 ,所形成的共混凝胶有明显的氯化钠相转变性质 ,也保持了聚N 异丙基丙... 用γ辐射技术合成了K 型卡拉胶 (KC)与聚N 异丙基丙烯酰胺共混凝胶 (Blendgels) .合成产物透明 ,有弹性和较好的力学强度 .对不同条件下共混凝胶性能的测定结果表明 ,所形成的共混凝胶有明显的氯化钠相转变性质 ,也保持了聚N 异丙基丙烯酰胺 (PNIPAM)特有的温度敏感性 (LCST为 34℃ ) 展开更多
关键词 K-型卡拉胶(KC) n-异丙基丙烯酰胺 共混凝胶 温度敏感 辐射合成 氯化钠相转变
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Liquid Chromatography Detertmination of Amino Acids by Pre-Column Fluorescence Derivatization with Acridone-N-acetyl Chloride
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作者 Jin Mao YOU Xin Jun FAN +1 位作者 Qing Yu OU Qing Cun ZHU (Lanzhou Institute of Chemical Physics, Chinese Academy of Sciences 730000)(Department of Chemistry, Qufu Normal University, Qufu, Shandong 273165) 《Chinese Chemical Letters》 SCIE CAS CSCD 1998年第7期657-660,共4页
A sensitive liquid chromatographic mcthod for the detection of andno acids with precolumn fluorescence derivatization with acridone-N-acetyl chloride has been developed. Andno acid derivatives were eluted in 4o ndn wi... A sensitive liquid chromatographic mcthod for the detection of andno acids with precolumn fluorescence derivatization with acridone-N-acetyl chloride has been developed. Andno acid derivatives were eluted in 4o ndn with good reproducibility. The reIative standard deviations (n=6) at an analytical concentration of 50 pmol are < 4%. The method described is also suitable for the analysis of andno acids in different biological samples. 展开更多
关键词 Liquid chromatography Acridone-n-acetyl chloride Amino acids Derivatization
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N,N-二异丙基乙二胺盐酸盐的合成 被引量:2
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作者 李茂林 辛成伟 陈新志 《应用化学》 CAS CSCD 北大核心 2005年第12期1384-1386,共3页
N,N-Diisopropylethanoamine was synthesized from diisopropylamine and ethylene oxide,and then chloridized to N,N-diisopropyl-2-aminoethyl chloride,which finally went through amindysis in benzene to(produce) the title p... N,N-Diisopropylethanoamine was synthesized from diisopropylamine and ethylene oxide,and then chloridized to N,N-diisopropyl-2-aminoethyl chloride,which finally went through amindysis in benzene to(produce) the title product N,N-diisopropyl ethanediamine.In these reactions,the optimum molar ratios were 1.2∶[KG-*3/5]1 for ethylene oxide to diisopropylamine,2∶[KG-*3/5]1 for thionyl chloride to N,N-diisoproylethanoamine,and(12∶[KG-*3/5]1) for ammonia to N,N-diisopropyl-2-aminoethyl chloride,respectively.The suitable reaction time,temperature,and solvent were also discussed.The total yield of 81.4% was obtained for the title product. 展开更多
关键词 二异丙胺 环氧乙烷 n n-二异丙基乙醇胺 n n-二异丙基氯乙胺 n n-二异丙基乙二胺
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三聚氯氰催化N-苯基马来酰亚胺的合成
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作者 黄文楚 张海侠 +2 位作者 李林博 刘志鑫 张开旭 《广东化工》 CAS 2024年第11期35-37,共3页
本文对N-苯基马来酰亚胺(N-PMI)的合成工艺进行创新。以顺丁烯二酸酐和苯胺为原料,分别在乙酸乙酯、甲苯和氯苯中合成N-苯基马来酰胺酸(N-PMA);再以三聚氯氰和三乙胺为催化剂,在不同溶剂中制备N-PMI。改进后的工艺操作较为简单、所需原... 本文对N-苯基马来酰亚胺(N-PMI)的合成工艺进行创新。以顺丁烯二酸酐和苯胺为原料,分别在乙酸乙酯、甲苯和氯苯中合成N-苯基马来酰胺酸(N-PMA);再以三聚氯氰和三乙胺为催化剂,在不同溶剂中制备N-PMI。改进后的工艺操作较为简单、所需原料试剂易得,为N-PMI的合成提供了一种新思路。 展开更多
关键词 n-PMA n-PMI 合成 三聚氯氰 工艺创新
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N⁃苯基马来酰亚胺共聚物的合成及对PVC树脂耐热改性效果研究
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作者 孙芳芳 宋运运 《中国塑料》 CAS CSCD 北大核心 2024年第7期49-54,共6页
通过种子乳液聚合结合半连续加料方式,成功聚合出分子结构一致且与聚氯乙烯(PVC)树脂具有良好相容性的聚(N‐苯基马来酰亚胺‐苯乙烯‐丙烯腈)(PNSA)共聚物胶乳,将其与PVC树脂直接复合制备PNSA/PVC复合材料,并对PNAS耐热改性的效果进行... 通过种子乳液聚合结合半连续加料方式,成功聚合出分子结构一致且与聚氯乙烯(PVC)树脂具有良好相容性的聚(N‐苯基马来酰亚胺‐苯乙烯‐丙烯腈)(PNSA)共聚物胶乳,将其与PVC树脂直接复合制备PNSA/PVC复合材料,并对PNAS耐热改性的效果进行评价。结果表明,PNSA纳米胶乳颗粒粒径在155.3~251.5 nm之间,粒径分布均一;PNSA共聚物分子组成呈无规结构,分子结构一致,差示扫描量热曲线呈现单一的玻璃化转变温度(T_(g)),且与PVC树脂具有极佳的相容性;PNSA含量由0升高至50%(质量比,下同)时,复合材料的T_(g)由84.8℃提高到107.2℃,提高了22.4℃,维卡软化温度由71.2℃提高到91.9℃,提高了20.7℃;除耐热性改善以外,复合材料的力学性能也有一定程度的提高,本文的研究有利于PVC应用领域的进一步拓展。 展开更多
关键词 聚氯乙烯 n‐苯基马来酰亚胺 自由基共聚 种子乳液 耐热改性
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Synthesis and Characterization of Phenyl Camellia oleifera Seed Oil Ester Plasticizing PVC
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作者 Wenqing Xiao Yuhang Liu +2 位作者 Yuxin He Qiaoguang Li Yongquan Li 《Journal of Renewable Materials》 EI CAS 2024年第3期615-628,共14页
Plasticizers are essential additives in the processing of polyvinyl chloride(PVC),with phthalate plasticizers being widely used.However,these conventional plasticizers have been shown to be harmful to human health and... Plasticizers are essential additives in the processing of polyvinyl chloride(PVC),with phthalate plasticizers being widely used.However,these conventional plasticizers have been shown to be harmful to human health and environmentally unfriendly,necessitating the exploration of eco-friendly bio-based alternatives.In this study,Camellia oleifera seed oil,a specialty resource in China,was utilized as a raw material and reacted with 4,4′-Methylenebis(N,N-diglycidylaniline)(AG-80)to synthesize Phenyl Camellia seed Oil Ester(PCSOE).PCSOE was employed as a plasticizer to prepare modified PVC films with varying concentrations,with the conventional plasticizer dioctyl phthalate(DOP)serving as a control.Experimental results demonstrate that PSCOE-plasticized PVC films exhibit enhanced hydrophilicity,tensile strength,and thermal stability compared to DOP-modified PVC films.The contact angle of PSCOE-plasticized PVC films ranges from 66.26°to 78.48°,which is generally lower than the contact angle of DOP-modified PVC films at 78.40°,indicating improved hydrophilicity due to the modification with PCSOE.The tensile strength of PSCOE-plasticized PVC films ranges from 17.73 to 20.17 MPa,all surpassing the value of 16.41 MPa for DOP-modified PVC films.Moreover,the temperatures corresponding to 5%,10%,and 50%weight loss for PVC samples modified with PCSOE are higher than those for DOP.Hence,PCSOE presents a viable alternative to DOP as a plasticizer for PVC materials. 展开更多
关键词 Polyvinyl chloride(PVC) Camellia oleifera seed oil 4 4′-Methylenebis(n n-diglycidylaniline) bio-based plasticizer
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PREPARATION AND APPLICATION OF ANTIMONY MONO (ISOOCTYL THIOGLYCOLATE) DI (N-DODECANETHIOL)
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作者 Shu Wanyin Jiang Youyun Qulong (Department of Chemistry, Central South University of Technology, Changsha 410083,China) 《Journal of Central South University》 SCIE EI CAS 1999年第1期33-35,共3页
AntimonymercaptideisanewtypeofheatstabilizerforPVC,whichhasthefolowingcharacteristics:highefficiency,nontox... AntimonymercaptideisanewtypeofheatstabilizerforPVC,whichhasthefolowingcharacteristics:highefficiency,nontoxicorharmfules,low... 展开更多
关键词 heat stabilizer AnTIMOnY mercaptide AnTIMOnY mono(isooctyl thioglycolate) di(n dodecanethiol) polyvinyl chloride
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Difluoromethylation of O-, S-, N-, C-Nucleophiles Using Difluoromethyltri(n-butyl)ammonium Chloride as a New Difluorocarbene Source 被引量:2
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作者 王飞 黄维洲 胡金波 《Chinese Journal of Chemistry》 SCIE CAS CSCD 2011年第12期2717-2721,共5页
Difluoromethyltri(n-butyl)ammonium chloride 1 was found to be an effective difluorocarbene reagent for O-, S-, N-, C-difluoromethylation under basic conditions. It is particularly remarkable that, when only 1.2 equi... Difluoromethyltri(n-butyl)ammonium chloride 1 was found to be an effective difluorocarbene reagent for O-, S-, N-, C-difluoromethylation under basic conditions. It is particularly remarkable that, when only 1.2 equivalent of reagent 1 was used, the difluoromethylated products were obtained in moderate to excellent yields. 展开更多
关键词 DIFLUOROCARBEnE CF2H group DIFLUOROMETHYLATIOn difluoromethyltri(n-butyl)ammonium chloride
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2-羟基-N-甲基乙酰苯胺的合成和表征 被引量:1
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作者 郑灵芝 周忠诚 舒万艮 《光谱实验室》 CAS CSCD 2006年第3期533-538,共6页
以N-甲基苯胺、氯乙酰氯、无水醋酸钠、甲醇等为原料,经乙酰化,酯化及酯交换反应合成了2-羟基-N-甲基乙酰苯胺,三步总收率为88.0%。N-甲基苯胺、氯乙酰氯在三乙胺的催化下,按n(C6H5NHCH3)∶n[ClCH2C(O)Cl]∶n[N(C2H5)3]=1∶1.05∶1,经... 以N-甲基苯胺、氯乙酰氯、无水醋酸钠、甲醇等为原料,经乙酰化,酯化及酯交换反应合成了2-羟基-N-甲基乙酰苯胺,三步总收率为88.0%。N-甲基苯胺、氯乙酰氯在三乙胺的催化下,按n(C6H5NHCH3)∶n[ClCH2C(O)Cl]∶n[N(C2H5)3]=1∶1.05∶1,经乙酰化反应得到2-氯代-N-甲基乙酰苯胺(Ⅰ),收率为93.8%;(Ⅰ)与无水醋酸钠在相转移催化剂四丁基溴化铵的存在下,按n(Ⅰ)∶n(NaOAc)=1∶1.2,经酯化反应合成了2-乙酰氧基-N-甲基乙酰苯胺(Ⅱ),收率为97.3%;(Ⅱ)与甲醇按n(Ⅱ)∶n(CH3OH)=1∶10,在氢氧化钾的催化下,进行了酯交换反应得到2-羟基-N-甲基乙酰苯胺(Ⅲ),收率为96.4%。并利用红外、质谱和元素分析,对各产物进行了表征,确认了分子结构。 展开更多
关键词 2-羟基-n-甲基乙酰苯胺 2-乙酰氧基-n-甲基乙酰苯胺 2-氯代-n-甲基乙酰苯胺 合成
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Williamson反应合成2-月桂氧基-N,N-二甲基乙胺 被引量:1
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作者 沈斌 陈洪龄 《化学研究与应用》 CAS CSCD 北大核心 2010年第7期853-857,共5页
采用Williamson合成方法,以N,N-二甲基乙醇胺(C4H11NO)、氯代十二烷(C12H25Cl)及固碱(KOH)为原料,环己烷为带水剂,合成了2-月桂氧基-N,N-二甲基乙胺(C16H35NO)。对影响醚化反应各因素:原料配比、反应温度、反应时间以及催化剂的种类进... 采用Williamson合成方法,以N,N-二甲基乙醇胺(C4H11NO)、氯代十二烷(C12H25Cl)及固碱(KOH)为原料,环己烷为带水剂,合成了2-月桂氧基-N,N-二甲基乙胺(C16H35NO)。对影响醚化反应各因素:原料配比、反应温度、反应时间以及催化剂的种类进行了探讨。用气相色谱法分析了产物含量,并用FT-IR、GC-MS和元素分析表征了产物结构。实验结果表明最佳工艺条件为:n(C4H11NO)∶n(C12H25Cl)∶n(KOH)=1.7∶1.0∶0.6;醚化反应温度:100℃;醚化反应时间:6h;催化剂:PEG-400(5mol%KOH),在此条件下2-月桂氧基-N,N-二甲基乙胺收率可达84.4%。 展开更多
关键词 2-月桂氧基-n n-二甲基乙胺 n n-二甲基乙醇胺 氯代十二烷 Williamson反应
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