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Knoevenagel condensation of α,β-unsaturated aromatic aldehydes with barbituric acid under non-catalytic and solvent-free conditions 被引量:1
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作者 Cherkupally Sanjeeva Reddy Adki Nagaraj 《Chinese Chemical Letters》 SCIE CAS CSCD 2007年第12期1431-1435,共5页
An efficient route for the synthesis of 5-(arylpropenylidine)-2,4,6-pyrimidinetrione 3 from an appropriate α,βunsaturated aromatic aldehydes 1 and barbituric acid 2 under both non-catalytic and solvent-free microw... An efficient route for the synthesis of 5-(arylpropenylidine)-2,4,6-pyrimidinetrione 3 from an appropriate α,βunsaturated aromatic aldehydes 1 and barbituric acid 2 under both non-catalytic and solvent-free microwave irradiation conditions was described. In this way, a range of biologically important compounds 3 was obtained in good to excellent yields (86-98%) in a very short reaction time (30-80 s). 展开更多
关键词 Barbituric acid Knoevenagel condensation 5-(Arylpropenylidine)-2 4 6-pyrimidinetrione
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SYNTHESIS AND CHARACTERIZATION OF POLY{4-[2-(tert-BUTYLDIMETHYLSILOXY)ETHYL]STYRENE}AND ITS HYDROLYSIS DERIVATIVE 被引量:1
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作者 郭文莉 《Chinese Journal of Polymer Science》 SCIE CAS CSCD 2009年第3期399-405,共7页
The living cationic polymerization of 4-[2-(tert-butyldimethylsiloxy)ethyl]styrene (TBDMES) was studied in methylcyclohexane (MeChx)/methylchloride (MeCl) (50/50 V/V) solvent mixture at -80 degrees C. The initiator 1,... The living cationic polymerization of 4-[2-(tert-butyldimethylsiloxy)ethyl]styrene (TBDMES) was studied in methylcyclohexane (MeChx)/methylchloride (MeCl) (50/50 V/V) solvent mixture at -80 degrees C. The initiator 1,1-diphenylethylene (DPE) capped 2-chloro-2,4,4-trimethylpentane (TMPCl) was formed in situ in conjunction with titanium tetrachloride (TiCl(4)). The Lewis acidity of TiCl(4) was decreased by the addition of titanium(IV) isopropoxide (Ti(OiPr)(4)) to accomplish living polymerization of TBDMES. Hydrolysis of poly(TBDMES) in the presence of tetra-butylammonium fluoride yielded poly[4-(2-hydroxyethyl)styrene] (poly(HOES)). FT-IR, NMR and DSC demonstrated the hydrolysis was complete. 展开更多
关键词 Living carbocationic polymerization Poly[4-(2-hydroxyethyl)styrene] hydrolysis Pendant hydroxyl groups
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Reaction pathways and selectivity in the chemo-catalytic conversion of cellulose and its derivatives to ethylene glycol:A review
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作者 Yao Li Yuchun Zhang +2 位作者 Zhiyu Li Huiyan Zhang Peng Fu 《Chinese Journal of Chemical Engineering》 SCIE EI CAS CSCD 2024年第2期310-331,共22页
Biomass-to-ethylene glycol is an effective means to achieve high-value utilisation of cellulose but is hindered by low conversion efficiency and poor catalyst activity and stability.Glucose and cellobiose are derivati... Biomass-to-ethylene glycol is an effective means to achieve high-value utilisation of cellulose but is hindered by low conversion efficiency and poor catalyst activity and stability.Glucose and cellobiose are derivatives of cellulose conversion to ethylene glycol,and it is found that studying the reaction process of both can help to understand the reaction mechanism of cellulose.It is desirable to develop a reusable,highly active catalyst to convert cellulose into ethylene glycol.This ideal catalyst might have one or more active sites described the conversion steps above.Here,we discuss the catalyst development of celluloseto-ethylene glycol,including tungsten,tin,lanthanide,and other transition metal catalysts,and special attention is given to the reaction mechanism and kinetics for preparing ethylene glycol from cellulose,and the economic advantages of biomass-to-ethylene glycol are briefly introduced.The insights given in this review will facilitate further development of efficient catalysts,for addressing the global energy crisis and climate change related to the use of fossil fuels. 展开更多
关键词 Ethylene glycol CELLULOSE Catalyst Retro-aldol condensation hydrolysis Kinetics
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A meshfree-based local Galerkin method with condensation of degree of freedom for elastic dynamic analysis 被引量:1
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作者 De-An Hu Yi-Gang Wang +2 位作者 Yang-Yang Li Xu Han Yuan-Tong Gu 《Acta Mechanica Sinica》 SCIE EI CAS CSCD 2014年第1期92-99,共8页
Condensation technique of degree of freedom is first proposed to improve the computational efficiency of meshfree method with Galerkin weak form for elastic dy- namic analysis. In the present method, scattered nodes w... Condensation technique of degree of freedom is first proposed to improve the computational efficiency of meshfree method with Galerkin weak form for elastic dy- namic analysis. In the present method, scattered nodes with- out connectivity are divided into several subsets by cells with arbitrary shape. Local discrete equation is established over each cell by using moving Kriging interpolation, in which the nodes that located in the cell are used for approxima- tion. Then local discrete equations can be simplified by con- densation of degree of freedom, which transfers equations of inner nodes to equations of boundary nodes based on cells. The global dynamic system equations are obtained by as- sembling all local discrete equations and are solved by using the standard implicit Newmark's time integration scheme. In the scheme of present method, the calculation of each cell is carried out by meshfree method, and local search is imple- mented in interpolation. Numerical examples show that the present method has high computational efficiency and good accuracy in solving elastic dynamic problems. 展开更多
关键词 Meshfree method Local Galerkin method Moving Kriging interpolation - condensation of degree of freedom Computational efficiency
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Pig Liver Esterase-catalyzed Hydrolysis of Three Diesters of meso-Bicyclic Dicarboxylic Acid and Three Tetraesters of Tetrahydrofuran -2,3,4,5-tetracarboxylic Acid
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作者 MA Guang-En and Tamm Ch. (National Institutes of Pharmaceutical Research & Development, Beijing 102206, P. R. China Institut fur Organishe Chemie der Universitat Basel, CH-4056 Basel Switzerland) 《Chemical Research in Chinese Universities》 SCIE CAS CSCD 2000年第4期369-374,共6页
Three diesters of exo- syn-meso-oxabicyclo (2, 2, 1 ) -hept- 5- ene- 2, 3- dicarboxylic acid and three tetraesters of tetrahydrofuran-2, 3, 4, 5-tetracarboxylic acid were synthesized and tested with enantioselective h... Three diesters of exo- syn-meso-oxabicyclo (2, 2, 1 ) -hept- 5- ene- 2, 3- dicarboxylic acid and three tetraesters of tetrahydrofuran-2, 3, 4, 5-tetracarboxylic acid were synthesized and tested with enantioselective hydrolysis catalyzed by pig liver esterase(PLE). The results of the PLEcatalyzed hydrolysis were discussed. 展开更多
关键词 Oxabicyclo(2 2 1 )-hept-5-ene-2 3-dicarboxylic acid Tetrahydrofuran-2 3 4 5- tetracarboxylic acid ESTERIFICATION hydrolysis Pig liver esterase(PLE)
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Formation conditions and accumulation characteristics of Bozhong 19-6 large condensate gas field in offshore Bohai Bay Basin 被引量:7
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作者 XU Changgui YU Haibo +1 位作者 WANG Jun LIU Xiaojian 《Petroleum Exploration and Development》 2019年第1期27-40,共14页
Based on the study of natural gas resource, low buried hill trap formation mechanism, high quality reservoir control factors and natural gas preservation conditions, the formation conditions and reservoir accumulation... Based on the study of natural gas resource, low buried hill trap formation mechanism, high quality reservoir control factors and natural gas preservation conditions, the formation conditions and reservoir accumulation characteristics of Bozhong 19-6 large condensate gas field were summarized. Large gas generation potential of multiple sets of thick humic-sapropelic source rocks in high maturity stage in Bozhong depression was the basis of large gas field formation. The multi-stage tectonic evolution since Indosinian period formed large-scale buried hill traps. The Tanlu fault activity formed multi-type reservoirs, and buried hill metamorphic rock of Archean and sand-conglomerate of Kongdian Formation were high-quality reservoirs. Thick overpressure lacustrine mudstone and weak neotectonic movement provided good preservation conditions. Bozhong 19-6 gas reservoir was a condensate gas reservoir with very high condensate oil content, and the gas origin was humic-sapropelic and kerogen-cracking gas, and the gas field had large gas thickness, high gas column characteristics and the accumulation process was first oil and then gas. The buried hill reservoir was a massive reservoir and the Kongdian reservoir was a stratified reservoir. The gas field had multi-channel hydrocarbon intense charge from overpressure source rocks, atmospheric-weak overpressure reservoir favorable for accumulation, thick overpressure mudstone caprock favorable for preservation, and natural gas ultra-late rapid accumulation model. 展开更多
关键词 OFFSHORE Bohai Bay Basin Bozhong 19-6 GAS field condensATE GAS low buried HILL METAMORPHIC rock reservoir accumulation characteristics ARCHEAN
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Alkaline Hydrolysis of PP/EHDPET Blend Fibers
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作者 李梅 付中玉 +1 位作者 张大省 王庆瑞 《Journal of China Textile University(English Edition)》 EI CAS 1999年第3期44-47,共4页
Polypropylene superfine fibers or cell porous fibers were prepared from the bi-component blend fibers of polypropylene/easlly hydro-degraded polyester(PP/EHDPET)by alkaline hydrolysis process. EHDPET is a kind of copo... Polypropylene superfine fibers or cell porous fibers were prepared from the bi-component blend fibers of polypropylene/easlly hydro-degraded polyester(PP/EHDPET)by alkaline hydrolysis process. EHDPET is a kind of copolyester that can be rapidly hydro-degraded in the hot alkaline solution. This paper discussed the kinetics of alkaline hydrolysis of EHDPET, and the effect of catalyst, bulk ratio and the content of polypropylene grafted maleic anhydride (PP-g-MAH) on the alkaline hydrolysis process. Meanwhile, the morphological change of the outer surface of blend fibers during this process was also investigated by the technology of scanning electron microscope (SEM). 展开更多
关键词 POLYPROPYLENE ( PP) easily HYDRO - degraded POLYESTER (EHDPET) BLEND fibers ALKALINE hydrolysis .
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Quantum Chemical Calculation on Preparation of YBa_2Cu_3O_(7-δ) Powders by Hydrolysis of Metal Alkoxides
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作者 尹周澜 李新海 +2 位作者 赵秦生 高孝恢 李晶 《Rare Metals》 SCIE EI CAS CSCD 1994年第1期72-76,共5页
The structural characteristics of different alkoxides of Y. Ba and Cu are studied with quantum chemi-cal CNDO /2 calculations. The relative hydrolysis rate coefficients k_M of them are obtained according tothe relati... The structural characteristics of different alkoxides of Y. Ba and Cu are studied with quantum chemi-cal CNDO /2 calculations. The relative hydrolysis rate coefficients k_M of them are obtained according tothe relationship between frontier orbitals and organic chemical reactions. Based on the above results. properexperimental conditions for the preparation of homogeneous ultra-purity. submicro high-T_cYBa_2Cu_3O_(7-δ) superconducting powders are proposed. 展开更多
关键词 Metal alkoxides. hydrolysis. YBa_2Cu_3O_(7-δ) Quantum chemical calcu-lation
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C12-3.43/0.981 Type 12MW Exhaustion and Condensing Stean Turbine
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《China's Foreign Trade》 1999年第7期39-39,共1页
TheQingdaoJienengPowerGroupCompanyinShandongmanufactUreseightseriesofsteamtIJrbinesin140varieties,witheachturbinebelow25MaTheC12-3.43/0.98type12MWexhaustionandcondensingsteamturbinehasthefollowingfeatures:12mW:ipa,435... TheQingdaoJienengPowerGroupCompanyinShandongmanufactUreseightseriesofsteamtIJrbinesin140varieties,witheachturbinebelow25MaTheC12-3.43/0.98type12MWexhaustionandcondensingsteamturbinehasthefollowingfeatures:12mW:ipa,435C,0.981Mpa,andh/h,whichcanbeusedi... 展开更多
关键词 C12-3.43/0.981 Type 12MW Exhaustion and condensing Stean Turbine
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γ-氨丙基倍半硅氧烷的水解聚合机理研究及产物结构表征 被引量:10
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作者 顾哲明 谷晓昱 张军营 《北京化工大学学报(自然科学版)》 EI CAS CSCD 北大核心 2006年第3期107-109,共3页
以γ-氨丙基三乙氧基硅烷(H2N.CH2.CH2.CH2.Si(OC2H5)3)为原料,通过控制其水解缩聚的条件制备聚γ-氨丙基倍半硅氧烷。详细论述了聚γ-氨丙基倍半硅氧烷的水解缩合过程,推断其水解缩合的机理,并利用FTIR、XRD和NMR等手段对聚合产物进行... 以γ-氨丙基三乙氧基硅烷(H2N.CH2.CH2.CH2.Si(OC2H5)3)为原料,通过控制其水解缩聚的条件制备聚γ-氨丙基倍半硅氧烷。详细论述了聚γ-氨丙基倍半硅氧烷的水解缩合过程,推断其水解缩合的机理,并利用FTIR、XRD和NMR等手段对聚合产物进行了结构表征,确定了合成产物的结构,证明产物中存在聚倍半硅氧烷结构。 展开更多
关键词 多面齐聚倍半硅氧烷 水解 缩合
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Enantio-selective preparation of (S)-1-phenylethanol by a novel marine GDSL lipase MT6 with reverse stereo-selectivity 被引量:4
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作者 邓盾 张云 +1 位作者 孙爱君 胡云峰 《Chinese Journal of Catalysis》 SCIE EI CAS CSCD 北大核心 2016年第11期1966-1974,共9页
We previously functionally characterized a novel marine microbial GDSL lipase MT6 and identified that the stereo-selectivity of MT6 was opposite to that of other common lipases in trans-esterification reactions.Herein... We previously functionally characterized a novel marine microbial GDSL lipase MT6 and identified that the stereo-selectivity of MT6 was opposite to that of other common lipases in trans-esterification reactions.Herein,we have investigated the use of MT6 in stereo-selective biocatalysis through direct hydrolysis reactions.Notably,the stereo-selectivity of MT6 was also demonstrated to be opposite to that of other common lipases in hydrolysis reactions.Parameters,including temperature,organic co-solvents,pH,ionic strength,catalyst loading,substrate concentration,and reaction time,affecting the enzymatic resolution of racemic 1-phenylethyl acetate were further investigated,with the e.e.of the final(S)-l-Phenylethanol product and the conversion being 97%and 28.5%,respectively,after process optimization.The lengths of side chains of 1-phenylethyl esters greatly affected the stereo-selectivity and conversion during kinetic resolutions.MT6 is a novel marine microbial GDSL lipase exhibiting opposite stereo-selectivities than other common lipases in both trans-esterification reactions and hydrolysis reactions. 展开更多
关键词 GDSLlipase BIOCATALYSIS Kinetic resolution Direct hydrolysis (S)-1-Phenylethanol Reverse stereo-selectivity
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γ-(2,3-环氧丙烷)丙基三甲氧基硅烷水解研究 被引量:8
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作者 陈奎 张天云 +1 位作者 曹秀鸽 杨光 《化工新型材料》 CAS CSCD 北大核心 2011年第9期96-97,108,共3页
为获得充分水解,且尽量避免缩聚的有机硅氧烷水解产物,以γ-(2,3-环氧丙氧)丙基三甲氧基硅烷(GPT-MS)为例,对有机硅氧烷的水解工艺进行研究。结果表明,中性介质、常温搅拌有利于降低水解得到的Si-OH发生缩聚反应;Si-OH的缩聚反应随着水... 为获得充分水解,且尽量避免缩聚的有机硅氧烷水解产物,以γ-(2,3-环氧丙氧)丙基三甲氧基硅烷(GPT-MS)为例,对有机硅氧烷的水解工艺进行研究。结果表明,中性介质、常温搅拌有利于降低水解得到的Si-OH发生缩聚反应;Si-OH的缩聚反应随着水含量的增加而下降,GPTMS的水解、缩聚反应随着反应温度的提高而加快;GPTMS与水的质量比为100∶28,常温搅拌至溶液无分层且澄清,即可获得水解完全且基本无缩聚反应发生的GPTMS水解产物。 展开更多
关键词 有机硅氧烷 水解 缩聚
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溶胶-凝胶法制备硅铝溶胶增强有机/无机复合薄膜 被引量:12
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作者 陆静娟 郭兴忠 杨辉 《稀有金属材料与工程》 SCIE EI CAS CSCD 北大核心 2008年第A02期111-115,共5页
以甲基三甲氧基硅烷(MTMS)的水解缩聚产物作为主要成膜物质、正硅酸乙酯(TEOS)和异丙醇铝的水解缩聚产物硅溶胶和铝溶胶作为无机增强物、甲基丙烯酰氧基丙基三甲氧基硅烷(KH-570)作为表面改性剂,通过共缩聚反应在聚碳酸酯(PC)板表面制... 以甲基三甲氧基硅烷(MTMS)的水解缩聚产物作为主要成膜物质、正硅酸乙酯(TEOS)和异丙醇铝的水解缩聚产物硅溶胶和铝溶胶作为无机增强物、甲基丙烯酰氧基丙基三甲氧基硅烷(KH-570)作为表面改性剂,通过共缩聚反应在聚碳酸酯(PC)板表面制备硅铝溶胶增强有机/无机复合薄膜;采用乌氏粘度计、TG/DTA、FTIR、UV-VIS、金相显微镜、铅笔硬度测试方法及划格法对涂膜液及薄膜性能进行表征。研究结果表明,加入KH-570改性铝溶胶后的涂膜液稳定性较好,MTMS水解缩聚产物与硅溶胶、铝溶胶通过共缩聚反应在PC板表面形成带有机基团的无机交联网络结构,基本骨架由Si-O-Si、Si-O-Al、Al-O-Al组成;铝溶胶的引入提高了薄膜的耐热性能及薄膜硬度,但KH-570改性的效果不明显;薄膜对PC片有增透效果,涂膜液陈化2d后,加入KH-570改性铝溶胶后薄膜的增透效果更理想;加入KH-570改性铝溶胶后薄膜的表面平整性得到改善。 展开更多
关键词 甲基三甲氧基硅烷 硅溶胶 铝溶胶 表面改性 水解缩聚 薄膜 性能
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复合树脂中硅烷偶联剂γ-MPS水解与缩合机制的研究 被引量:17
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作者 牛光良 王同 +2 位作者 翁诗甫 沈德言 徐恒昌 《口腔颌面修复学杂志》 2002年第4期208-211,共4页
目的:研究复合树脂中最常用的硅烷偶联剂γ-MPS水解与缩合的机制。方法:应用傅立叶变换红外光谱(FT-IR)法对γ-MPS及其水解液在不同状态时的特征吸收谱带进行分析。结果:(1)γ-MPS水解后其分子结构中Si-O-CH3基团消失,水解产物中出现具... 目的:研究复合树脂中最常用的硅烷偶联剂γ-MPS水解与缩合的机制。方法:应用傅立叶变换红外光谱(FT-IR)法对γ-MPS及其水解液在不同状态时的特征吸收谱带进行分析。结果:(1)γ-MPS水解后其分子结构中Si-O-CH3基团消失,水解产物中出现具有反应活性的Si-OH基团,C=O基的伸缩振动向低频率发生位移。(2)γ-MPS水解液放置1h时,溶液中已有线性硅氧烷醇齐聚物存在。(3)随γ-MPS水解液放置时间延长,Si-OH吸收强度减弱,而Si-O-Si吸收强度增强;同时C=O基的伸缩振动向高频率发生位移,表明γ-MPS水解液在不断进行缩合。结论:本研究从分子水平上揭示了硅烷偶联剂γ-MPS水解液随放置时间变化,其分子间发生缩合的规律,为有效合理地使用γ-MPS偶联剂提供理论依据。 展开更多
关键词 复合树脂 硅烷偶联剂 γ-MPS 水解 缩合 红外光谱 发生机制
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α-氰基肉桂酸酯类液晶的合成与性质研究 被引量:2
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作者 丁兴立 韩耀华 +2 位作者 钤秀丽 史子谦 梁晓 《液晶与显示》 CAS CSCD 北大核心 2009年第5期635-639,共5页
以对羟基苯甲醛和氰基乙酸乙酯缩合生成α-氰基对羟基肉桂酸乙酯,再与4种酰氯反应生成α-氰基肉桂酸酯类液晶;以对羟基苯甲醛和氰基乙酸丙基苯酚酯缩合生成α-氰基对羟基肉桂酸丙基苯酚酯,再与2种烷基环己基甲酰氯反应生成α-氰基肉桂... 以对羟基苯甲醛和氰基乙酸乙酯缩合生成α-氰基对羟基肉桂酸乙酯,再与4种酰氯反应生成α-氰基肉桂酸酯类液晶;以对羟基苯甲醛和氰基乙酸丙基苯酚酯缩合生成α-氰基对羟基肉桂酸丙基苯酚酯,再与2种烷基环己基甲酰氯反应生成α-氰基肉桂酸酯类液晶。目标化合物经MS分析确认了结构。通过差示扫描量热仪测量相变温度,对合成产物的液晶相态进行了研究;通过紫外分光光度计测量紫外光谱,研究了合成产物紫外吸收性能。在混合液晶中的应用实验表明,此类化合物可以作为具有液晶性能的紫外吸收剂添加到混合液晶中,改善液晶材料的抗紫外性能。 展开更多
关键词 液晶 α-氰基肉桂酸酯 氰基乙酸乙酯 KNOEVENAGEL condensation
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催化剂对正硅酸乙酯水解-聚合机理的影响 被引量:124
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作者 林健 《无机材料学报》 SCIE EI CAS CSCD 北大核心 1997年第3期363-369,共7页
运用溶胶-凝胶法制备SiO2凝胶,研究了催化剂对正硅酸乙酯的水解-聚合机理及凝胶结构的影响.结果表明催化剂阴离子尺寸导致了不同的水解机理,不同的催化方式及催化剂浓度、pH值、反应水量等对凝胶化时间、结构均有明显影响.
关键词 溶胶凝胶 硅酸乙酯 水解 聚合 二氧化硅 催化剂
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3,5-二硝基-3,5-二氮杂庚烷合成与性能 被引量:2
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作者 陈斌 刘亚静 +2 位作者 高福磊 汪营磊 陆婷婷 《含能材料》 EI CAS CSCD 北大核心 2019年第12期1036-1042,共7页
以1,3-二乙基脲为原料,经硝化、水解、缩合等反应得到了中间体乙硝胺(ENA)及终产物3,5-二硝基-3,5-二氮杂庚烷(DNDA7),ENA收率为80.6%,纯度为99.3%,DNDA7收率为67.7%,纯度为99.0%,总收率为54.6%。采用红外光谱、核磁共振及元素分析表征... 以1,3-二乙基脲为原料,经硝化、水解、缩合等反应得到了中间体乙硝胺(ENA)及终产物3,5-二硝基-3,5-二氮杂庚烷(DNDA7),ENA收率为80.6%,纯度为99.3%,DNDA7收率为67.7%,纯度为99.0%,总收率为54.6%。采用红外光谱、核磁共振及元素分析表征了其结构。优化了硝化、水解和缩合反应条件,确定较佳硝化水解反应条件为:硝化剂为20%发烟硫酸和浓硝酸,硝化温度-5~0℃,水解温度20℃,水解时间30 min;较佳缩合反应条件为:乙硝胺/多聚甲醛摩尔比1∶0.5,反应温度23~25℃,反应时间30 min。利用差示扫描量热技术(DSC)研究了DNDA7热分解特性及与火炸药常用组分的相容性,结果表明,其熔点为77.3℃,热分解峰温为260.8℃,DNDA7与黑索今相容性较好,与奥克托今、硝基胍和聚叠氮缩水甘油醚基本相容,与硝化棉和1,1-二氨基-2,2-二硝基乙烯的相容性较差;利用国军标GJB772A-1997方法测试其撞击感度H50>125.9 cm,摩擦感度为4%。 展开更多
关键词 含能增塑剂 3 5-二硝基-3 5-二氮杂庚烷(DNDA7) 硝化 水解 缩合
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TEOS的溶胶-凝胶行为对合成碳化硅晶须的影响 被引量:2
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作者 李心慰 曲殿利 +2 位作者 吴锋 徐娜 栾旭 《耐火材料》 CAS 北大核心 2016年第6期420-423,共4页
为了制备直晶率高,光洁度好,长径比均匀,强度大的碳化硅晶须,以正硅酸乙酯(TEOS)和蔗糖为原料,无水乙醇为溶剂,pH为1~2的HCl为催化剂,采用溶胶-凝胶法制备碳化硅晶须,重点考察了TEOS溶胶凝胶行为即HCl的引入方式(直接滴加... 为了制备直晶率高,光洁度好,长径比均匀,强度大的碳化硅晶须,以正硅酸乙酯(TEOS)和蔗糖为原料,无水乙醇为溶剂,pH为1~2的HCl为催化剂,采用溶胶-凝胶法制备碳化硅晶须,重点考察了TEOS溶胶凝胶行为即HCl的引入方式(直接滴加法和水溶液法)、水解温度(20、40和60℃)、搅拌时间(15、30、45和60min)对合成碳化硅晶须的影响。结果表明:pH为1~2的盐酸以水溶液的形式加入正硅酸乙酯中,在40℃恒温水浴锅中搅拌30min,可使正硅酸乙酯充分水解缩聚;在氩气气氛下1500oC煅烧1h制得的β—SiCw量最多,表面光洁,直径在60~100nm,直晶率高,且长径比均匀。 展开更多
关键词 碳化硅晶须 正硅酸乙酯 水解-聚合 溶胶-凝胶
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2,4-二硝基-2,4-二氮杂戊烷的合成与热性能 被引量:2
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作者 陈斌 汪营磊 +2 位作者 陆婷婷 刘亚静 高福磊 《火炸药学报》 EI CAS CSCD 北大核心 2018年第6期543-548,共6页
以1,3-二甲基脲为原料,经硝化、水解、缩合等反应合成了2,4-二硝基-2,4-二氮杂戊烷(DNDA5)。采用红外光谱、核磁共振及元素分析对其结构进行了表征;利用DSC研究了其热分解特性及与火炸药常用组分的相容性;同时优化了水解及缩合反应条件... 以1,3-二甲基脲为原料,经硝化、水解、缩合等反应合成了2,4-二硝基-2,4-二氮杂戊烷(DNDA5)。采用红外光谱、核磁共振及元素分析对其结构进行了表征;利用DSC研究了其热分解特性及与火炸药常用组分的相容性;同时优化了水解及缩合反应条件。结果表明,确定的较佳水解反应条件为:硫酸水溶液质量分数20%,反应温度93~95℃,反应时间30 min;较佳缩合反应条件为:甲硝胺和多聚甲醛摩尔比为1. 0∶0. 5,反应温度23~25℃,反应时间30 min,总收率为64. 1%。升温速率10℃/min时,DNDA5的熔点为50. 2℃,热分解峰温为271. 1℃,热安定性较好;DNDA5与RDX和NC的相容性较好,与HMX、NQ和GAP的相容性略差,与CL-20和FOX-7的相容性较差。 展开更多
关键词 有机化学 含能增塑剂 2 4-二硝基-2 4-二氮杂戊烷 硝化 水解 缩合
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甲基丙烯酸3-三甲氧基硅丙酯/苯乙烯细乳液共聚合过程中的水解及缩合反应 被引量:3
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作者 曹志海 单国荣 《高分子学报》 SCIE CAS CSCD 北大核心 2008年第8期759-764,共6页
研究了甲基丙烯酸3-三甲氧基硅丙酯(MPS)和苯乙烯(St)细乳液聚合过程中的水解及缩合反应.用气相色谱仪测定聚合过程中水解产物——甲醇的含量来研究MPS的水解度.MPS分子主要在细乳液液滴与水的界面以及乳胶粒与水的界面上发生水解反应.... 研究了甲基丙烯酸3-三甲氧基硅丙酯(MPS)和苯乙烯(St)细乳液聚合过程中的水解及缩合反应.用气相色谱仪测定聚合过程中水解产物——甲醇的含量来研究MPS的水解度.MPS分子主要在细乳液液滴与水的界面以及乳胶粒与水的界面上发生水解反应.MPS和St比例、介质pH值、乳化剂用量、引发剂类型和用量都会影响MPS的水解程度.缩合产物用29Si固态核磁共振表征,中性条件下,缩合反应受到抑制,在高MPS/St比例的体系中也只生成少量缩合产物.酸性和碱性条件下,缩合产物量均增加,但碱性条件下,体系中仍有一定数量未缩合的硅氧烷存在,这与细乳液聚合独特的液滴成核机理及聚合过程中较少液滴间物质交换有关. 展开更多
关键词 水解 缩合 细乳液聚合 甲基丙烯酸3-三甲氧基硅丙酯
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