促进剂ZDMC连续化合成工艺研究

研究采用管式反应器连续化合成促进剂ZDMC(二甲基二硫代氨基甲酸锌)的工艺,并分析工艺参数对产品质量的影响。最佳工艺条件为:二甲胺、二硫化碳、氢氧化钠、氯化锌物质的量比为1.0∶1.3∶1.01∶0.502,二甲胺质量分数为40%,氢氧化钠质量分数为32%,氯化锌质量分数为15%,反应温度为40℃,水、二甲胺、二硫化碳、氢氧化钠、氯化锌体积比为7∶25∶10∶15∶75;采用该工艺条件,在管式反应器中进行连续化合成反应,所得产品质量满足GB/T 11409—2008要求,收率在98.5%以上。

固定床法连续化合成哌嗪新工艺的研究

简要综述了哌嗪的合成路线 ,重点探讨了采用固定床反应器以N (β 羟乙基 )乙二胺为原料合成哌嗪的工艺方法 ,筛选出一种高活性、高选择性的镍、铜、铬、锌、锰 /γ 氧化铝催化剂 ,确定了催化剂的最佳组成及制备方法。优化了合成哌嗪时的反应温度、反应压力等参数 ,并确定了最佳工艺条件。哌嗪产率可达 90 %以上。

2,2′-亚乙基双(4,6-二叔戊基苯酚)的清洁化合成工艺

以2,4-二叔戊基苯酚、无水三聚乙醛为反应原料,采用含有表面活性剂、酸性催化剂的水作为反应溶剂,缩合反应合成2,2′-亚乙基双(4,6-二叔戊基苯酚)。研究了清洁化生产工艺过程,使反应母液能够反复循环,解决了传统生产工艺中含酚废水的排放问题。在n(2,4-二叔戊基苯酚)∶n(无水三聚乙醛)=2∶1.2、m(酸催化剂)=11.0 g、m(溶剂)=180 g、m(乳化剂)=0.5 g、反应温度80～83℃、反应时间5 h的合成条件下,原料2,4-二叔戊基苯酚的转化率大于94.3%,产品的收率大于93.3%。

模块化合成化学在制备系列钼酸铵工艺中的应用

根据模块化合成化学的基本原理对制备系列钼酸铵的工艺进行了研究,结果发现,系列钼酸铵不仅是具有一定结构、组成与功能的独立实体,而且是能够相互转换的一组模块单元。依据钼酸根缩合数的高低进行升级与降级反应,可以划分为"模块化合成工艺"及"模块化拆分工艺"等两种模块化设计。系列钼酸铵模块包括:二钼酸铵、七钼酸铵、八钼酸铵、十钼酸铵及十二钼酸铵等。自由基理论认为,模块化合成工艺是由下级钼酸铵模块,与氢自由基的极性键的接口作用,完成向上级钼酸铵的转换;模块化拆分工艺是由上级钼酸铵模块,与氧自由基的非极性键的切口作用,拆分成下级钼酸铵的工艺。在模块化合成化学理论指导下的钼酸铵制备工艺具有出类拔萃的优势与无限美好的发展空间;该工艺的特点包括极低的酸或水合氨的耗用指数、完美的晶体结构、均匀的粒度分布、规范的操作工艺、低廉的生产成本、友好的环境保护等。

糊精氮化铅球形化工艺参数的研究

通过起爆药在有机玻璃管壳中压药上浮试验和流散性测定,发现球形糊精氮化铅中粒径<45μm颗粒的含量增多,使药剂装药性能下降、流散性变差,压药容易上浮;频繁压爆、毫秒延期电雷管瞬爆是压药上浮所致。提出两项质量控制指标:药剂堆积密度≥2.00 g/cm3;粒径<45μm颗粒的质量分数≤20%。工艺参数:3%(质量分数)氮化钠溶液加入8%(质量分数)硝酸铅溶液,水药质量比301,工业酸性糊精质量分数(外加)5%,氮化钠溶液碱度0.080%,化合温度60℃。保持一定的加料速度和搅拌强度,能稳定生产出满足雷管装配需求的起爆药。

光纤通信与射频通信集成电路工艺技术

一、引言在社会信息产业迅猛发展和高新技术不断出现的今天,通信系统与集成电路已经成为相互依赖、密不可分的整体。我国集成电路长期以来由于种种原因落后于国外,通信系统中的关键集成电路大多依赖进口,这不仅极大地威胁着我国信息网络的安全,

Melting purification process and refining effect of 5083 Al-Mg alloy

To improve the poor stability of casting process of Al alloy with high Mg content, which leads to poor final product quality, the melting purification process and the influences of the refiner on the microstructure and defect of 5083 alloy were studied. The results show that the optimized process for the rotary impeller degassing of 5083 alloy is as follows： a rotary speed of 250-400 r/min; a gas flow of 1.2-2.0 L/s, a refining time of 10-15 min. This optimized process can reduce the gas content in the solid alloy to 2× 10^-3 mL/g or lower. Due to the addition of grain refiner, the cast microstructure of 5083 alloy is refined. The Al-5Ti-IB wire shows the best refining effect among all the refiners. The refining effect is improved with the increase of grain refiner addition amount. And the refinement effects become stable when Ti content reaches 0.1% or higher. The surface crinkling defect of the billet can be easily found in the alloy refined with Al-5Ti-IB wire compared with the alloys refined with other refiners.

Effect of element fitting on composition optimization of Al-Cu-Ti amorphous alloy by mechanical alloying

In order to minimize the crystal phase in Al-Cu-Ti amorphous powder,Al65Cu35-xTix amorphous powders were optimized via ball milling through adjusting the amount of Cu and Ti elements and the ball milling time.The results show that increasing the mole fraction of Ti can decrease the amount of Al Cu2Ti,Cu9Al4,and Al2Cu intermetallics formed during the process of ball milling;and prolonging the ball milling time can reduce the element crystalline phase to almost none.The optimal composition is determined to be Al65Cu16.5Ti18.5.TiH2 forms in all selected Al65Cu35-xTix amorphous powders during the process of optimization.H atom is decomposed from toluene and reacts with Ti during ball milling,leading to the formation of TiH2.The volume fraction of TiH2 in Al65Cu16.5Ti18.5 amorphous powder is measured to be 4.30%.

酸碱度对起爆药质量的影响

介绍了介质酸碱度在起爆药化合时对其质量的影响 ,重点分析了现行起爆药化合时介质酸碱度的影响趋势 。

Simulation of Low-Temperature Coal Tar Hydrocracking in Supercritical Gasoline

The aim of this paper was preliminary design of the process for low-temperature coal tar hydrocrackmg m supercritical gasoline based on Aspen Plus with the concept of energy self-sustainability. In order to ensure the correct- ness and accuracy of the simulation, we did the following tasks： selecting reasonable model compounds for low-tem- perature coal tar; describing the nature of products gasoline and diesel accurately; and confirming the proper property study method for each block by means of experience and trial. The purpose of energy self-sustainability could be pos- sibly achieved, on one hand, by using hot stream to preheat cold stream and achieving temperature control of streams, and on the other hand, by utilizing gas （byproduct of the coal tar hydrocracking） combustion reaction to provide energy. Results showed that the whole process could provide a positive net power of about 609 kW-h for processing the low- temperature coal tar with a flowrate of 2 268 kg/h. The total heat recovery amounted to 2 229 kW-h, among which 845 kW＇h was obtained from the gas combustion reaction, and 1 116 kW＇h was provided by the reactor＇s outlet stream, with the rest furnished by hot streams of the products gasoline, diesel and residue. In addition, the process flow sheet could achieve products separation well, and specifically the purity of product gasoline and diesel reached 97.2% and 100%, respectively.

An Integrated Process of a Two-Stage Fixed Bed Syngas Production and F-T Synthesis for GTL in Remote Gas Field

A novel process for catalytic oxidation of methane to synthesis gas (syngas), which consists of two consecutive fixed-bed reactors with air introduced into the reactors, integrated Fischer-Tropsch synthesis, was investigated. At the same time, a catalytic combustion technology has been investigated for utilizing the F-T offgas to generate heat or power energy. The results show that the two-stage fixed reactor process keep away from explosion of CH4/O2. The integrated process is fitted to produce diesel oil and lubricating oil in remote gas field.

Preparation of pure SbCl_3 from lead anode slime bearing high antimony and low silver

A novel treatment process of lead anode slime bearing high antimony and low silver was developed by a potential-controlled chloridization leaching and continuous distillation.The experimental results show a high Sb 3+ concentration,489.2 g/L,in the leaching solution for two-stage countercurrent leaching process,and the leaching rates of Sb,Cu,Bi more than 99% when the potential is controlled at 450 mV.When the leaching solution is distillated and concentrated at 120°C,almost all the silicon compound is evaporated into the concentration distillate and exists as amorphous hydrated silica.By the continuous distillation,high pure SbCl3 could be prepared,and AsCl3 is enriched in the distillate while metals Bi,Cu are enriched in the continuous distillation residue.As a result,the recovery rate of Sb is more than 95%.

盐酸达克罗宁的药学研究进展

盐酸达克罗宁化学名为4-丁氧基-3-哌啶基苯丙酮盐酸盐,是一种安全、低毒的局部麻醉药,对皮肤、黏膜穿透力强,局部麻醉作用迅速、持久,具有止痛、止痒、杀菌等作用。美国药典第35版已收录本品[1],中国药典尚未收录。但我国在制剂和临床上也广泛使用该药多年,现就近几年我国在达克罗宁的药化合成工艺、制剂的制备、制剂的质量控制等方面的药学研究进展情况作一些归纳总结,现综述如下。

Three-dimensional Ordered Silica Colloidal Film Self-assembly Deposited on a VerticalSubstrate

A method for preparation of particle crystal film constructed from monodisperse silica colloidal particles in diameter of about 300 nm is reported. The films were prepared from an ethanol suspension by vertical deposition that relies on capillary forces to assemble colloidal crystal particles on a vertical substrate. The 3D ordered films were characterized by transmission spectra and scanning electric microscope (SEM). The effect of evaporation temperature, particle concentration and sintered temperature on the quality of colloidal particle crystal film was investigated.

River Water Purification via a Coagulation-Porous Ceramic Membrane Hybrid Process

Membrane filtration technology combined with coagulation is widely used to purify river water.In this study,microfiltration(MF)and ultrafiltration(UF)ceramic membranes were combined with coagulation to treat local river water located at Xinghua,Jiangsu province,China.The operation parameters,fouling mechanism and pilot-scale tests were investigated.The results show that the pore size of membrane has small effect on the pseudo-steady flux for dead-end filtration,and the increase of flux in MF process is more than that in UF process for cross-flow filtration with the same increase of cross-flow velocity.The membrane pore size has little influence on the water quality.The analysis on membrane fouling mechanism shows that the cake filtration has significant influence on the pseudo-steady flux and water quality for the membrane with pore size of 50,200 and 500 nm.For the membrane with pore size of 200 nm and backwashing employed in our pilot study,a constant flux of 150L·m 2·h 1was reached during stable operation,with the removal efficiency of turbidity,total organic carbon(TOC)and UV254 higher than 99%,45%and 48%,respectively.The study demonstrates that coagulation-porous ceramic membrane hybrid process is a reliable method for river water purification.

Peracetic Acid Synthesis by Acetaldehyde Liquid Phase Oxidation in Trickle Bed Reactor

In this paper,shorter residence time（a few minutes）with high yield in the trickle bed process for per- acetic acid synthesis by acetaldehyde liquid phase oxidation can be realized on the selected packing material SA-5118.For acetaldehyde in acetone with ferric ion as catalyst,the optimized process conditions were presented. The main factors influencing the yield,selectivity and conversion are residence time,temperature and acetaldehyde concentration,respectively.The temperature range checked is from 30 to 65℃.High yield of 81.53%with high se- lectivity of 91.84%can be obtained at higher temperature of 55℃when the residence time is 5.5min and the acet- aldehyde concentration is 9.85%（by mass）.And there is a critical acetaldehyde concentration point（Cccp）between 18%and 19.5%（by mass）.At temperature less than 55℃,the highest yield to peracetic acid at each temperature level increases with temperature when the acetaldehyde concentration is below Cccp and decreases with temperature when the acetaldehyde concentration is above Cccp.

Behavior of silver and lead in selective chlorination leaching process of gold-antimony alloy

The behavior of silver and lead in the selective chlorination leaching process of gold-antimony alloy was analyzed in detail and appropriate recovery methods were developed.A reduction method by adding gold-antimony alloy powder was adopted to recover silver according to the thermodynamics calculation.The reducing rate of silver can exceed 99%at 80℃for 1.5 h when the dosage of gold-antimony alloy powder is 10%.The dissolution equilibrium curved surfaces of PbSO4 and PbCl2 under different conditions were drawn.The experimental results are well consistent with theoretical analysis that indicate lead may be precipitated in the form of lead chloride.The grade of gold in the residue can be further concentrated to 94.5%after being washed with hot water. These two methods have been applied successfully in the practice.

Investigation into Syngas Generation from Solid Fuel Using CaSO4-based Chemical Looping Gasification Process

Chemical-looping gasification （CLG） is a novel process for syngas generation from solid fuels, sharing the same basic principles as chemical-looping combustion （CLC）. It also uses oxygen carriers （mainly metal oxide and calcium sulfate） to transfer heat and oxygen to the fuel. In this paper, the primary investigation into the CLG process with CaSO4 as oxygen carrier was carried out by thermodynamic analysis and experiments in the tube reactor. Sulfur-contained gas emission was mainly H2S rather than SO2 in the CLG process, showing some different features from the CLC. The mass and heat balance of CLG processes were calculated thermodynamically to determinate the auto-thermal operating conditions with different CaSO4/C and steam/C molar ratios. It was found that the CaSO4/C molar ratio should be higher than 0.2 to reach auto-thermal balance. The effect of temperature on the reactions between oxygen carrier and coal was investigated based on Gibbs free energy minimum method and ex- perimental results. It indicated that high temperature favored the CLG process in the fuel reactor and part of syngas was consumed to compensate for auto-thermal system.

TIG welding-brazing joint of aluminum to stainless steel with hot wire

TIG welding-brazing process with high frequency induction hot wire technology was presented to create joints between 5A06 aluminum alloy and SUS32! stainless steel using ER1100 filler wire with different temperature. The joints were evaluated by mechanical test and microstructural analyses. The welding procedure using hot fiUer wire （400 ℃ ） significantly increases strength stability by 71% and average value of tensile strength by 30. 8 % of the joints, compared with cold wire. The research of microstructures in interfaces and welded seams reveals that using 400 ℃ hot filler wire can decrease the thickness of intermetallic compounds （ IMCs ） from 6 to 3.5 txm approximately, which is the main reason of mechanical property improvement.

Wet friction performance of C/C-SiC composites prepared by new processing route

C/C-SiC composites with SiC island distribution Were prepared via a new processing route. The fabrication process mainly included silicon infiltration by ultrasonic vibration, chemical vapor deposition （CVD）, siliconizing, liquid phase impregnation and carbonization. The wear and friction properties were tested by an MM-1000 wet friction machine. The results show that SiC phases are mainly distributed between carbon fibers and pyrocarbons as well as among the pryoearbons. The dynamic friction coefficient of the composites decreases gradually from 0.126 to 0.088 with the increase of the surface pressure from 0.5 to 2.5 MPa at the same rotary speed. Furthermore, under the constant surface pressure, the dynamic friction coefficient increases from 0.114 to 0.126 with the increase of the rotary speed from 1 500 to 2 500 r/min. However, the coefficient decreases to 0.104 when the rotary speed exceeds 4 500 r/min. During the friction process, the friction coefficient of C/C-SiC composite is between 0.088 and 0.126, and the wear value is zero after 300 times brake testing.