硫酸加工天然硼砂矿生产硼酸的相平衡

以Pitzer电解质溶液理论为基础 ,引入离子强度函数来表达高温 (1 0 0℃ )时两电解质之间及电解质与非电解质之间的作用系数 ,计算了 2 5℃和 1 0 0℃时H3BO3-Na2 SO4-NaCl-H2 O四元体系的溶解度 ,计算值与实验测定值相吻合 .应用该四元体系的相图讨论了用西藏天然硼砂生产硼酸的工艺过程 .     

硼酸双甘油酯双硬脂酸酯的合成

以实验室自制的硼酸双甘油酯和硬脂酸为主要原料制备了硼酸双甘油酯双硬脂酸酯。首先考察了反应温度对产品收率的影响,获得了最佳反应温度。在此基础上,系统研究了催化剂用量对产品收率的影响,获得了适宜的催化剂用量。最后,利用红外光谱技术对产品进行了分析,分析结果表明,实验获得的产品即为目标产物。     

硫酸氧钛液相法制备纳米二氧化钛

以硫酸氧钛为原料，液相法在水醇体系中制备纳米二氧化钛。讨论了表面活性剂、硫酸氧钛浓度、反应温度、体系pH、煅烧温度等因素对纳米粒子生成及性能的影响，用X射线衍射仪和透射电镜检测，证明实验获得的产物为粒径20～40nm的锐钛型二氧化钛。研究表明，通过改变工艺条件可控制纳米二氧化钛粒径及尺寸分布。工艺流程简单，制备成本低，易实现工业化。     

硼酸酯类偶联剂的合成

本文报道以价廉易得的原料、简单可行的路线合成硼酸酯之结果。在理论分析的基础上，采用反应一精馏一体化法合成了硼酸三异丙酯，确定了带水剂，考察了原料配比、带水剂浓度对收率的影响，原料配比、浓硫酸催化剂对反应速率的影响。进而以硼酸三异丙酯为中间体，运用酯交换法合成了硼酸酯偶联剂，所确定的合成方法具有操作简便、产品收率高等优点。     

由硼砂和消石灰制备偏硼酸钙

以硼砂和消石灰为原料,经反应、过滤、洗涤及干燥制备出偏硼酸钙(CaO*B2O3*6H2O)产品.经过实验研究确定了适宜的工艺条件:硼钙配料比(氧化硼与氧化钙质量比)在2.2∶ 1左右;液固体积质量比为2.76 mL/g左右;温度为35 ℃;反应时间为8～10 h.在此工艺条件下制得的偏硼酸钙产品含氧化硼质量分数为29%～31%、氧化钙质量分数为23%～25%、氧化钠质量分数≤0.5%.产物的X射线衍射分析和热重分析表明,合成的产品为六水合偏硼酸钙纯相,扫描电镜显示产物为白色的不规则六边形条状晶体.     

对甲苯磺酸催化合成硼酸三乙醇胺酯

以硼酸和三乙醇胺(过量)为原料,以对甲苯磺酸作为酯化催化剂,采用潜溶剂法(适量甲苯作为带水剂,加热回流反应)合成制备硼酸三乙醇胺酯。实验中考察了原料配比对硼酸酯收率的影响。实验结果表明,随着原料配比的增加,硼酸三乙醇胺酯的收率也随之增加;当原料配比达到1∶5.5时,硼酸三乙醇胺酯的收率会随着它们的进一步增加而下降。     

硫酸钛催化合成柠檬酸三丁酯的研究

研究了以硫酸钛为催化剂合成柠檬酸三正丁酯（TBC）的工艺条件，考察了醇酸摩尔比、催化剂用量及反应时间等因素对酯化反应的影响，并确定了最佳反应条件。     

新型钝化材料硫酸氧钛

一前言在毛主席无产阶级革命路线指引下,在市环境保护办公室、市科技局、市化工局的领导下,我厂于一九七三年末承担了试制硫酸氧钛的光荣任务。并且在试验鉴定过程中,得到了广州电器科学研究所、沈阳市电镀厂、沈阳标准件厂、沈阳高压开关厂和低压开关厂的大力协助,经过三结合的努力,终于试制出适合电镀工业用的新型钝化材料——硫酸氧钛。目前,已投入生产。     

硼酸合成方法研究进展

根据不同的硼酸合成原材料,对国内外近些年来在硼酸合成领域的研究进展进行了综述,分析了各种方法的优缺点,探讨了硼酸合成的未来发展方向。     

硫酸钛催化合成乙酸酯的研究

研究了硫酸钛催化下乙酸酯（乙酸正丁酯）的合成,考察了加热温度、原料配比、催化剂用量和反应时间对反应的影响,发现在加热温度为１９０℃,醇酸摩尔比为１．２：１,催化剂用量为０．０１５ｍｏｌ／ｍｏｌ乙酸时,反应９０ｍｉｎ乙酸转化率可达９９．１％。该催化剂对伯醇和仲醇酯化的催化效果都比较理想。加入一定量惰性固体可以改善催化剂的使用效果和寿命。     

钛液水解工艺对金红石二氧化钛消色力的影响

以工业钛液为原料,采用外加晶种常压水解工艺制备了金红石型二氧化钛,研究了水解钛液的组成和操作参数对二氧化钛消色力的影响。实验结果表明：二氧化钛消色力（Tcs）和蓝相光谱值（Scx）随晶种添加量的增加先增大后减小,随判灰延时时间的增加先增大后减小,随钛液F值的增加先稍有增加后明显降低,随钛液二氧化钛质量浓度的增大而增加。在钛液F值（游离硫酸加上与钛结合的硫酸之和与二氧化钛质量浓度的比值）为1.90左右、铁钛比（铁元素与二氧化钛质量浓度的比值）＜0.5、二氧化钛质量浓度为190~200 g/L、晶种添加量（晶种中二氧化钛质量与对应批次水解浓钛液中二氧化钛质量的比值）为2.0%~2.2%、灰点为“基点+20 min”、熟化时间为0~30 min、稀释水在二沸后100 min加入的条件下进行水解,经过一次洗涤—漂白—二次洗涤—盐处理—煅烧,所得金红石型二氧化钛的消色力更好。     

纳米水合硼酸锌的合成

通过改进传统的七水合硼酸锌 (2ZnO·3B2 O3 ·7H2 O)的合成工艺条件 ,合成了纳米级硼酸锌并对产品进行了x -射线、透射电镜等测试表征。     

硼酸与5-苯基-四氮唑复合盐的合成

以苯甲腈、叠氮钠等为原料,经偶合,成盐合成了硼酸复合5 苯基四氮唑。研究了反应时间、反应温度对产品收率的影响。实验表明:在n(苯甲腈)∶n(叠氮钠)=1∶1.1,催化剂用量为反应物总量的25%,120℃反应20h可得到收率90%的5 苯基四氮唑。在n(5 苯基四氮唑)∶n(硼酸)=1∶1,120℃反应30min的条件下,可得到约90%的标题化合物。原料经二步反应后的总收率为81%。     

Supported hybrid catalysts based on zirconocene and tris(pyrazolyl)borate titanium derivatives

A series of hybrid supported catalysts were prepared by combining (iBuCp)₂ZrCl₂ and {Tp^Ms*}TiCl₃ complex (Tp^Ms* = HB(3‐mesityl‐pyrazolyl)₂(5‐mesityl‐pyrazolyl)^?) sequentially grafted onto MAO (methylaluminoxane)‐modified silica according to a Plackett Burmann 2³ design. Supported catalysts were prepared taking into account the immobilization order, silica pretreatment temperature, and grafting temperature. Grafted metal content was comparatively determined by Rutherford backscattering spectrometry (RBS), X‐ray photoelectronic spectroscopy (XPS), and inductively coupled plasma–optical emission spectroscopy (ICP–OES). The resulting catalysts were evaluated in terms of catalyst activity and polymer properties. According to RBS measurements, grafted metal content remained comprised between 0.1 and 0.5 wt % Zr/SiO₂ and 0.1 and 0.3 wt % Ti/SiO₂ depending on the immobilization order and on silica pretreatment temperature. All the systems were shown to be active in ethylene polymerization having external MAO as cocatalyst. Catalyst activity seemed to be governed by the zirconocene species, influenced slightly by Ti ones. Resulting polymers were characterized by DSC and GPC. The polyethylenes mostly presented higher molecular weight than those produced by homogeneous catalysts or by zirconocene grafted on bare or on MAO‐modified silica. © 2005 Wiley Periodicals, Inc. J Appl Polym Sci, 2006     

Synthesis and characterization of a homoleptic titanium dihydrobis(pyrazol-1-yl)borate complex

The neutral titanium(III) complex Ti(BP)₃ {BP = dihydrobis(pyrazol-1-yl)borate} was synthesized by reacting TiCl₃(THF)₂ with an excess of the potassium salt of the ligand in THF. The compound was isolated as a green solid and characterized by elemental analysis, NMR and IR spectroscopy, Mass spectrometry and magnetic and conductivity measurements. The molecular ion was detected in the Mass spectrum. ¹¹B NMR data suggested a distortion from the ideal octahedral geometry caused by the d¹ electronic configuration of the metal centre and this hypothesis was confirmed by means of DFT calculations.     

硼酸镁晶须的合成及表征

以氢氧化镁和硼酸为原料,利用高温-助熔剂-湿法工艺合成了高品质的硼酸镁晶须。采用XRD、SEM、HR-TEM、SAED等手段表征,系统研究了焙烧温度、焙烧时间、硼镁物质的量比及助熔剂添加量对晶须形貌的影响。结果表明,在焙烧温度为850 ℃、焙烧时间为4 h、n（硼）∶n（镁）=3∶1、n（钠+钾）∶n（镁+硼）=4∶1的条件下,可合成直径为0.5~0.8 μm、长径比为40~240且表面光滑的硼酸镁晶须。还对硼酸镁晶须的高温-助熔剂-湿法工艺合成生长机理进行了探讨。     

硼酸三甲酯无“三废”合成工艺

以硼酸、甲醇为原料,用甲酰胺对产物进行萃取提纯,合成硼酸三甲酯,探索了最佳工艺条件。利用气相色谱、色谱-质谱联用、红外光谱等分析表征手段,鉴定反应产物,最佳工艺条件：n硼酸：n甲醇=1∶3.5;回流时间为4 h。此工艺无＂三废＂排放,有利于工业化生产。     

Structural analysis of oxyfluoride borate glass and BaF2 crystallization from phase separation

Oxyfluoride glass and glass-ceramics are being studied due to the possibility of their utilization in many applications, such as thermoluminescent dosimeters, optical fibers, fluorescent concentrators, and temperature sensors. In order to improve the properties of glass, they are often crystallized. For this crystallization to be effective, knowledge and control of the structure of the starting material is required. Much work was done on silicate glass; however, a great interest exists in obtaining these kinds of materials in other matrices such as germanates, phosphates, and borates. Here, we present a structural study of some oxyfluoride borate glass with different concentrations of PbF₂ by means of Nuclear Magnetic Resonance (NMR), Raman, and Fourier Transform Infrared (FTIR) spectroscopies. We also analyzed glass-crystallization using Differential Scanning Calorimetry (DSC). The crystallization study was complemented with the use of Transmission Electron Microscopy (TEM) and Selected Area Electron Diffraction (SAED), for the purpose of identifying possible mechanisms of crystallization. Our results indicate, from the structural point of view, that the glass present groups with one or two BO₄ species, such as diborate or pentaborate. The small variation in the BO₄ fraction with the increase in PbF₂ concentration would be an indication of the formation of F⁻BO_3/2 species. Oxyfluoride borate glass containing BaO as a cation modifier and 30% PbF₂ represents a good starting point for obtaining glass-ceramics with a narrow size distribution of BaF₂ nanocrystals. We also propose that the possible mechanism for oxyfluoride borate glass crystallization started with a separation of phases.     

微波辅助合成低水硼酸锌

采用氧化锌、硼酸为原料，利用微波加热合成低水硼酸锌（ZB-2335），以缩短反应时间、提高反应效率。实验中考察了反应温度、微波辐射时间、原料比等因素的影响；确定了适宜的反应条件为：反应温度105—110℃，微波辐射时间55min，氧化锌与硼酸的物质的量比1：11，氧化锌与水的物质的量比1：140，产率达97．6％。产品的组成分析结果符合要求，其失水温度高于340℃。微波加热条件下的反应速率约是常规加热法反应速率的13倍，该方法具有不引入外来离子，产物单一，不需精制、分离，反应母液可以重复利用，反应过程容易控制等特点，是合成阻燃剂ZB-2335的较佳路线。     

新型含氮取代茂钛络合物的合成

合成了两个新型含氮茂钛络合物,经过元素分析、核磁共振、质谱确证结构。一个络合物单晶经过X－射线测试。