由乙腈一步法制备乙酸丁酯的研究

以丁醇和制备丙烯腈的副产物乙腈为原料 ,采用一步法合成了乙酸丁酯。通过正交实验得到了影响反应的 4种因素。确定了最佳的工艺条件为 :催化剂的量为样品质量的 40 % ;n(CH3CN)∶ n(C4 H9OH) =1∶ 1 .0 5 ;反应温度为 1 0 5℃ ;反应时间为 8h。在此反应条件下 ,乙酸丁酯的收率为 88.8% ,纯度可达 99.5 %。并用气相色谱及红外光谱对产品的纯度进行了表征     

两步法合成双氰胺工艺

采用两步法由氰氨化钙合成双氰胺,通过正交试验,考察了水解温度、聚合温度、聚合时间对产品收率的影响,确定了最佳的工艺条件:水解温度42℃、聚合温度70℃、聚合时问150 min,此条件下,双氰胺收率可达85.73％。     

PEG20000中试放大的工艺研究

在一定温度和催化剂作用下 ,分别利用本体聚合和溶剂聚合的方法 ,在 1L、10 0L不锈钢高压反应釜中合成了相对分子质量为 2 0 0 0 0的聚乙二醇 ,并讨论了聚合反应机理 ,研究了催化剂用量、反应温度、反应时间对聚合反应的影响。经过红外、核磁共振、凝胶色谱、化学分析等方法对产物进行了表征。     

啤酒酵母菌种的石蜡保藏技术

啤酒酵母菌种用液体石蜡技术保藏具有设备简单、操作方便,成活率高,变异少,优良种性能保持较长时间的优点,实用价值高。本文从液体石蜡保藏菌种的机理、保藏效果、保藏等具体技术操作及其使用方法都作了较为详细的介绍,相信能为啤酒菌种的保藏带来较大的好处。     

场激活加压燃烧合成WC-Ni复合材料的工艺参数研究

以钨、碳和镍为原料,在电场激活下,材料的燃烧合成和致密化同时进行,短时间内完成了碳化钨镍复合材料的制备。研究了场激活 加压燃烧合成中的工艺参数,如脉冲电流、能量控制模式、升温速率、最高温度和压力对反应的影响。测量了在反应合成和致密化前后的样品 收缩率。所制备的复合材料的相对密度,490N载荷下Vickers硬度和断裂韧性分别为99.2%,13.965GPa和5.9MP·m1/2。     

纳米稀土复合超强酸SO42-/ZrO2-La2O3催化合成乙酸冰片酯及其动力学初探

采用纳米稀土复合固体超强酸SO4^2-／ZrO2-La2O3催化合成乙酸冰片酯，并对反应条件和该反应的动力学进行了探究。结果表明，在反应温度为120℃，催化剂用量为天然冰片质量的6％．天然冰片与乙酸的摩尔比为1：6，反应时间为8h时，反应的酯化率和选择性可达到93．14％和99．8％．研究发现，该催化剂可重复使用，并能活化再生。给出了反应速率方程，测出了反应的活化能。     

A new colloidal precursor cooperative conversion route to nanocrystalline quaternary copper sulfide

A novel milk-like Cu-thiourea colloid has been synthesized. Nanocrystalline quaternary copper sulfide Cu₂FeSnS₄ was obtained through the Cu-thiourea colloidal precursor cooperative conversion route at low temperature. The samples were characterized by means of X-ray powder diffraction, transmission electron microscopy, scanning electron microscopy, inductively coupled plasma atomic emission spectroscopy, and X-ray energy dispersive spectroscopy techniques. The reaction details and features were described and discussed.     

The reaction of ceria coatings on mica with H2S: An in-situ X-ray diffraction study

Thin layers of ceria were deposited on the surface of mica platelets in solution. The reaction of such particles with hydrogen sulfide yields a red colored special effect pigment. The ceria layer reacts with H₂S to produce a variety of sulfide and oxysulfide phases. The reaction path discovered in situ by time and temperature resolved X-ray diffraction is CeO₂→CeS₂→C-Ce₂S₃→Ce₁₀S₁₄O. The reaction itself is extremely variable depending on gas flow, heating rates and decomposition atmospheres. Effects on the thin film are recorded by scanning electron microscopy (SEM) and revealed a destruction of the layer once red Ce₁₀S₁₄O was formed. The product layer then reveals the typical nonwetting behaviour of a liquid on a surface.     

A comparative study of the gas sensing behavior of nanostructured nickel ferrite synthesized by hydrothermal and reverse micelle techniques

A comparative study of gas sensing behavior of nanocrystalline nickel ferrite synthesized by micro-emulsion and hydrothermal method to liquefied petroleum gas (LPG) is presented. Nanocrystalline nickel ferrite synthesized by hydrothermal method indicated higher electrical conductivity and gas sensitivity at low operating temperature compared to nanocrystalline nickel ferrite synthesized by reverse micelle technique. This difference in the gas sensing behavior can be attributed to the presence of more oxygen vacancies (i.e. non-stoichiometry) in the hydrothermally synthesized nickel ferrite. Incorporation of palladium had a catalytic effect and the operating temperature was significantly reduced in both the samples. The higher operating temperature of the reverse micelle nickel ferrite material makes the sensor response speed faster (∼10 s) compared to the hydrothermally synthesized material (∼1 min).     

Electrical conductivity and gas sensitivity of Zn-Sb-O thick films

The thick film of Zn-Sb-O was prepared by coating the paste of nanoparticles mixture (Sb₂O₃:ZnO=1:3) on the alumina substrate, followed by sintering at 500-900 °C for 2 h in air. The electrical resistance and gas-sensing properties to benzene, alcohol and acetone of Zn-Sb-O films were found to be dependent on the change of phase structure caused by sintering temperature.