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研究了几种有机钛化合物对草酸二甲酯(DMO)与苯酚酯交换反应的催化性能,发现催化活性及选择性顺序依次为二氯二茂钛钛酸四苯酯钛酸丁酯乙酰丙酮氧钛钛酸乙酯钛酸异丙酯,表明二氯二茂钛是一种性能较好的酯交换催化剂.在n(Cp2TiCl2)=0.001 mol、n(DMO)=0.3 mol、n(Phenol)=0.2 mol、T=180℃、t=2 h优化工艺条件下,苯酚转化率可达44.0%,甲基苯基草酸酯(MPO)和草酸二苯酯(DPO)收率分别达37.8%和6.1%,酯交换总选择性为99.8%. 相似文献
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研究了几种有机钛化合物对草酸二甲酯(DMO)与苯酚酯交换反应的催化性能,发现催化活性及选择性顺序依次为二氯二茂钛>钛酸四苯酯>钛酸丁酯>乙酰丙酮氧钛>钛酸乙酯>钛酸异丙酯,表明二氯二茂钛是一种性能较好的酯交换催化剂。在n(Cp2TiCl2) = 0.001 mol、n (DMO) =0.3mol、n (Phenol) = 0.2mol、T=180癈、t=2h优化工艺条件下,苯酚转化率可达44.0%,甲基苯基草酸酯(MPO)和草酸二苯酯(DPO)收率分别达37.8%和6.1%,酯交换总选择性为99.8%。 相似文献
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掺杂La2O3的硫酸钛在缩醛(酮)反应中的催化活性 总被引:4,自引:1,他引:3
硫酸钛掺杂La2O3后经高温焙烧制得一种新型固体酸催化剂。用环己酮缩乙二醇反应表征其催化活性的反应条件为:环己酮200mmol,n(环己酮):n(乙二醇)=1.0:1.5,带水剂环己烷15mL,硫酸钛催化剂[w(La2O3)0.05,400℃焙烧3h]用量4.1%(以环己酮质量计),回流分水1h,收率94.5%。结果表明,催化活性随La2O3含量的增加而升高,随焙烧温度的升高而降低。催化剂吸附吡啶的红外光谱证实催化剂表面存在明显的Broensted酸中心和Lewis酸中心。该催化剂对其它缩醛(酮)反应也有催化活性。 相似文献
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研究了以麦秆为原料用水解-氧化-水解法制取草酸的工艺方法。最佳反应条件:麦秆用量50g,硫酸浓度70%,物料浸泡时间≥3h,m(硝酸):m(麦秆)=2.1:1.0;氧化催化剂V2O5-FeCl3[n(V2O5):n(FeCl3)=1:1]用量0.1g,氧化-水解反应时间5h,反应温度65℃~70℃,草酸二水合物收率75.5%。 相似文献
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反相高效液相色谱法测定植物组织及根分泌物中草酸 总被引:12,自引:0,他引:12
采用反相C1 8柱 ,2 2 0nm紫外检测 ,0 .5 %KH2 PO4 0 .5mmol L四丁基硫酸氢铵 (tetrabutylammoniumhydrogensulfate ,TBA) (pH 2 .0 )的水溶液体系 ,可使草酸及其它测试的 6种有机酸及硝酸有效分离。进一步研究了该方法测定植物组织及根分泌物中草酸的效果 ,结果表明其精确灵敏、回收率高、重复性好 ,并且成本低、操作简便 ,可应用于各种生物材料、食品、饮料等产品中的草酸含量检测。 相似文献
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催化动力学光度法测定生物样品中的草酸 总被引:3,自引:0,他引:3
提出了一种经动力学光度法测定生物样品中草酸的方法。基于在硫酸介质中,草酸能有效地催化重铬酸钾氧化丁基罗丹明B褪色,当反应温度为65℃、反应时间12min时,非催化反应溶液的吸光度A0和催化反应溶液吸光度A的lnA0/A值与草酸浓度在0.20~10.08μg/ml之间存在良好线性关系。反应体系用高浓度NaOH终止后室温下可稳定2h以上。催化反应的表观活化能为13.53kj/mol。方法可直接用于菠菜 相似文献
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Ruicheng Ran Diankui Fu Ji Shen Qingyang Wang 《Journal of polymer science. Part A, Polymer chemistry》1993,31(12):2915-2921
A polystyrene-bonded Ti(IV) chloride catalyst was synthesized by the reaction of a polystyryl lithium (catalyst I , PS—TiCl2) or a polystyryl magnesium (catalyst II , PS-TiCl3) combined with titanium tetrachloride. The catalyst produced is a polymeric organometallic compound containing 0.479 mmol Ti/g catalyst, 0.986 mmol Cl/g catalyst (catalyst I ) and 0.281 mmol Ti/g catalyst, 0.766 mmol Cl/g catalyst (catalyst II ), depending on the method of synthesis. Both catalysts showed very good stability and good catalytic activity in such organic reactions as esterification, acetalation, and ketal formation. They can be reused many times without losing its catalytic activity. © 1993 John Wiley & Sons, Inc. 相似文献
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Superacid catalyst SO42--ZrO2/TiO2 was applied in esterification of Acetic Acid and Butanol. The particle size of ZrO2 in the catalyst was about 12.5 nm. In catalyst preparation conditions, the effect factor order on catalytic activity is H2SO4 concentration > calcination temperature > ZrO2 supported content. The optimum preparation condition is as follows: ZrO2 content 3.5g/g; calcination temperature 600℃, and H2SO4 concentration 0.5mol/L. The catalytic activity is 96.5 vol%.SO42-/MxOy solid superacid is a kind of green catalyst, whose application perspective is bright. In this paper, SO42--ZrO2/TiO2 solid superacid was prepared with nanometer compound carrying method. The acidic strength of catalysts was measured with the following Hammett indicators, 2,4-dinitrofluorobenzene (H0=-14.52) and p-nitrochlorobenzene (H0=-12.70). Catalytic activity was evaluated with esterification reaction of Acetic Acid and Butanol. Reaction temperature was at 105℃, and reaction time was only 1h. The conversion rate of Acetic Acid was analyzed by a gas chromatograph (GC-14C SHIMADZU in Japan)The experimental results showed that H2SO4 concentration had more influences on catalytic activity than other two factors, calcination temperature and ZrO2 supported content. Since sulfur absorbed on the surface of metal oxides is necessary to the acidity of SO42-/MxOy solid superacid,H2SO4 concentration in impregnation solution is needed enough high. But, it can't be too much high,otherwise, Zirconium sulfate formed on the catalyst surface will be harmful influences on catalytic activity. In researched cover, 0.5mol/L H2SO4 concentration is the most suitable, and the catalyst prepared with this concentration has very strong acidity.The optimum preparation condition is as follows: ZrO2 content 3.5g/g; calcination temperature 600℃, and H2SO4 concentration 0.5mol/L. In the catalyst prepared with above conditions, the acidic strength (H0) of the catalyst is smaller than <-14.52, and catalytic activity is 96.5 vol%. When it was re-used in esterification reaction, catalytic activity decreased gradually with re-used times increasing(seen in Table 1). But after catalyst is used repeatedly up to five times, catalytic activity (84.3 vol %)is still higher than that of H2SO4 catalyst.The X-ray diffraction patterns showed that ZrO2 supported in TiO2 belonged tetragonal zirconia phases. Through the calculation of Scherrer formula, the particle size of ZrO2 in the catalyst is about 12.5 nm. After SO42- promoted nanometer ZrO2/TiO2 compound carrier, the diffraction peaks of tetragonal zircoma become broader and the strength weaker. It shows that adding SO4 ions restrains the crystallization of ZrO2, diminishes the size of particles. This might be why SO42--ZrO2/TiO2 has high catalytic activity and stability in acidic catalysis reaction. 相似文献
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硫酸盐水合物催化下的酯化反应 I: 反应级数,活化能及催化剂活性的测定 总被引:1,自引:0,他引:1
The order of esterification reaction of acetic acid and ethanol catalyzed by Fe2(SO4)3.7H2O and CusO4.5H2O has been determined. The reaction order was found to be 2 with respect to acid and ethanol with constant quantities of catalysts. The activity of catalysts can be expressed by Ym value, which is different from catalyst to catalyst. For Fe2(SO4)3.7H2O, Cr2(SO4)3.6H2O, CuSO4.kH2O, NiSO4.7H2O, ZnSO4.7H2O, CoSO4.7H2O, FeSO4.7H2O and MnSO4.5H2O the Ym values are 1.52, 1.21, 0.62, 0.42, 0.47, 0.25, 0.10 and 0.00 respectively. A linear relationship of Ym with the fraction of the second ionization potentiol (P) over radius (r) of metal ion of sulphate salts was found to be Ym=α(P/γ)+b. 相似文献
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Liu XY Huang M Ma HL Zhang ZQ Gao JM Zhu YL Han XJ Guo XY 《Molecules (Basel, Switzerland)》2010,15(10):7188-7196
Sulfonated (SO(3)H-bearing) activated carbon (AC-SO(3)H) was synthesized by an aryl diazonium salt reduction process. The obtained material had a SO(3)H density of 0.64 mmol·g-1 and a specific surface area of 602 m2·g-1. The catalytic properties of AC-SO(3)H were compared with that of two commercial solid acid catalysts, Nafion NR50 and Amberlyst-15. In a 10-h esterification reaction of acetic acid with ethanol, the acid conversion with AC-SO(3)H (78%) was lower than that of Amberlyst-15 (86%), which could be attributed to the fact that the SO(3)H density of the sulfonated carbon was lower than that of Amberlyst-15 (4.60 mmol·g-1). However, AC-SO(3)H exhibited comparable and even much higher catalytic activities than the commercial catalysts in the esterification of aliphatic acids with longer carbon chains such as hexanoic acid and decanoic acid, which may be due to the large specific surface area and mesoporous structures of the activated carbon. The disadvantage of AC-SO(3)H is the leaching of SO(3)H group during the reactions. 相似文献
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磁性纳米固体超强酸的合成、表征及性能 总被引:16,自引:0,他引:16
首次制备了SO42-/Co0.5Fe2.5O4-ZrO2磁性固体超强酸,利用TEM,DTA,XRD和FTIR等手段研究了Co0.5Fe2.5O4磁性基质对ZrO2的粒子大小、晶化温度与结构的影响.考察了磁性固体超强酸的催化性能及催化剂的寿命、回收率和磁性.结果表明,引入Co0.5Fe2.5O4磁性基质不但赋予催化剂以磁性,而且在固体超强酸形成过程中延迟了ZrO2由四方晶相向单斜晶相的转变,有助于稳定样品表面的含硫物种,磁性固体超强酸对酯化反应具有较高的催化活性,可活化再生,并保持磁性. 相似文献
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TiO2空心微球因具有低密度、高活性、易分离而有利于多次重复使用的优点而广受关注.本文介绍一种无氟制备TiO2空心微球的简单方法——磷钨酸钾(K3PW12O40)模板法.首先,将H3PW12O40和KCl溶液混匀,得到白色牛奶状的K3PW12O40模板(式(1)),然后在磁力搅拌下加入一定量的Ti(SO4)2粉末,加热至大约125oC开始回流.回流8 h后,过滤洗涤.滤饼分散在强NaOH溶液中,原位除去K3PW12O40模板(式(2)).最后,将催化剂洗涤到滤液为中性,干燥后即得到TiO2空心微球.3KCl + H3PW12O40= K3PW12O40ˉ+3HCl (1) K3PW12O40+24NaOH =12Na2WO4+ K3PO4+12 H2O (2) Ti(SO4)2+2H2O = TiO2+2H2SO4(3)我们将所制备的TiO2空心微球,采用X射线衍射、透射电子显微镜、扫描电子显微镜、傅立叶红外光谱、固体粉末漫反射和X射线光电子能谱等进行了表征.采用紫外光催化降解阴离子染料(活性嫣红X3B)来评价催化剂的性能.实验结果显示:(1)所制TiO2空心微球直径在0.5–1.0μm;(2)磷钨酸钾模板剂充当晶核,有利于空心微球的晶化;(3)加入的高浓度硫酸钛,水解产生大量的硫酸,抑制硫酸钛水解,不利于TiO2空心微球的晶化(式(3));(4)催化剂的活性随着硫酸钛量的增加而先增后降.4 mmol硫酸钛用量的TiO2空心微球具有最高的光催化活性,是TiO2颗粒样品(无磷钨酸钾模板法制备)的2.1倍.用该方法制备的TiO2空心微球活性高可归因于以下主要原因:(1)TiO2空心微球独特的孔结构;(2)良好的晶化程度(TiO2样品晶化度越高,越有利于光生载流子的分离,抑制复合);(3)样品残余磷钨酸钾模板和TiO2之间存在光生电子转移,有利于空心微球TiO2活性的提高.该法具有操作简单、重复性好、易于批量制备的等优点,有望广泛应用于(光)催化、电化学、分离与纯化以及药物缓释等领域. 相似文献
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SO4^2—/MXOY型固体超强酸及其催化酯化 总被引:36,自引:0,他引:36
SO4^2-/MXOY型固体超强酸用作酯化反应的催化剂,具有催化活性高、选择性好、易与产品分离、无污染、可重复利用等优点。本文综述了SO4^2/MXOY型固体超强酸的研究进展及其在酯化反应中的催化作用。探讨了这类固体超强酸的制备条件、表面结构及其用作酯化催化剂的性能和寿命等问题。 相似文献