水合肼法制备硫酸肼的研究

首先用尿素氧化法制备水合肼，然后加入浓硫酸得产物硫酸肼。实验结果表明，硫酸肼的收率与浓硫酸的滴加速度有关，而硫酸肼的纯度与浓硫酸的滴加速度和硫酸肼的沉降时间有关。制取水合肼较为适宜的工艺条件为：n（尿素）：n（次氯酸钠）：n（氢氧化钠）=（1．10～1．12）：1．00：（2．27～2．43），低温反应温度控制在20℃以下，高温反应时应快速升温至回流反应，反应时间控制在5min左右。制备硫酸肼时，滴加硫酸的速度控制在1h左右。     

ADC发泡剂生产中加酸工艺的改进

介绍了中平能化集团开封东大化工有限公司ADC发泡剂生产中氯化洗水循环利用的试验情况,用氯化洗水与浓硫酸混合后与水合肼反应生成联二脲,解决了加入浓硫酸瞬时肼尿液局部分解的问题,采用n（浓硫酸）：n（氯化洗水）=1：2的配比可使联二脲收率达到94．70％。     

尿素法制备水合肼的研究

以氯气和氢氧化钠为原料制备次氯酸钠溶液,控制其中游离碱含量在10.8%左右,有效氯在8.0%左右。次氯酸钠与尿素经过低温反应和高温反应,合成水合肼。实验分析了尿素法生产水合肼的各种影响因素,实验表明,尿素、次氯酸钠与氢氧化钠的摩尔比为(1.10~1.12)∶1∶(2.30~2.42),低温反应温度控制在20℃以下,高温反应阶段快速升温至回流后反应5 m in左右时,水合肼收率可达75.1%左右。     

尿素法生产水合肼氧化反应工艺条件的探讨

尿素生产水合肼分四个过程：次氯酸钠与尿素的配制、氧化反应、蒸发、精馏，其中氧化反应是关键岗位，工艺控制的好坏，直接影响水合肼生产的消耗。从反应历程入手，本文分析了氧化反应条件的理论依据及影响因素，从而寻求出合理的工艺控制条件。     

三乙胺催化合成2,5-二巯基-1,3,4-噻二唑

采用三乙胺作为催化剂，合成了DMTD(2，5-二巯基-1,3，4-噻二唑)。将产率从传统工艺的82.50％提高至90.01％。并探讨了三乙胺的催化机理。通过试验得到了该反应的最佳反应条件：反应温度为80℃：配料比为n(水合肼)：n(二硫化碳)：n(氢氧化钾)=1．0：3．5：2．0；每摩尔水合肼需加三乙胺40mg。同时用红外光谱仪鉴定了产物的结构。并进行了氮元素的分析及熔点的测定。结果均与理论值相符。     

尿囊素合成新工艺

尿囊素合成新工艺是以乙二醛为原料，采用FeSO4-H2O2催化氧化法合成乙醛酸，溶液不需分离，再与尿素进行缩合两步法合成尿囊素；将缩合后的滤液回收利用，提高产品收率。通过对氧化和缩合反应条件的研究，得出较佳氧化反应温度为5℃～8℃，配料n(H2O2)：n((CHO)2)为0．9：1．0，n((CHO)2)：n(尿素)为l：4，催化剂为H3PWl2O40，加入量是乙醛酸质量的0．6％，缩合反应温度为75℃～80℃，反应时间3h。按此工艺条件生产尿囊素其收率由文献值40％提高到68．6％(以乙二醛计)。产品经过熔点测定、元素分析和红外光谱鉴定，其纯度达99．6％，符合国家药典标准规定的含量要求。     

乙烯酮氯化法合成氯乙酰氯

研究了乙烯酮氯化法合成氯乙酰氯。考察了溶剂、溶剂比、氯气配比、反应温度及反应器型式等对乙烯酮氯化的影响。得出溶剂及溶剂比对乙烯酮氯化有重要影响。以空塔或填料塔作反应器，在反应温度10℃～30℃，反应物配比乙烯酮：氯气=1：1．02～1．05，氯乙酰氯：溶剂磷酸酯≤1．0的条件下，基本无二氯乙酰氯产生，氯乙酰氯收率94％～96％，纯度可达91．5％。     

改进ADC发泡剂生产工艺的实验研究

本文采用４２％烧碱生产高浓度次氯酸钠，加入４２％烧碱配成有效氯：氢氧化钠＝１：２．４－２．５（摩尔比），再将合成、缩合所需尿素一并投入次氯酸钠中、生产水合肼粗溶液，粗溶液经冷却除去十水碳酸钠后，加本中和、缩合、洗涤、氧化、洗涤、离心、干燥、过筛即得ＡＤＣ产品。     

关于提高水合肼收率的探讨

目前,我国生产水合肼的厂家,基本上都是用次氯酸钠与尿素反应生产水合肼。国外除个别国家用尿素生产水合肼外,发达国家尿素法生产基本上已经淘汰。我们认为,在我国目前的生产条件下,研究提高水合肼的收率是很有意义和必要的。     

水合肼的生产现状及展望(连载四)——第五节 国内尿素法制肼的几种流程

1 几种制肼流程 1.1 罐式反应器流程 这是一种比较老式的流程,早在50年代在我国已使用,适用于一些产量小的企业。 操作方法:先在罐式反应器内加入一定量的次氯酸钠(有效氯在8％～9％),再加入定量的尿素液(尿素液内已加进反应所需的添加剂),迅速开蒸汽,搅拌反应1～2分钟即得粗肼,含肼量只有35～40g/1(3％左右),而且还有很多杂质,所以称为粗水合肼(俗称氧化液)。其流程见图4所示:     

乙烯酮(双乙烯酮)下游产品废水的治理技术

乙烯酮(双乙烯酮)是十分重要的化工中间体,其下游产品较多。江苏某化工厂开发生产乙烯酮(双乙烯酮)下游产品三十多个,年生产规模三万多吨,是国内以乙烯酮(双乙烯酮)为中间体生产精细化学品的综合骨干企业。针对乙烯酮(双乙烯酮)下游产品废水特点,该厂结合企业实际,开展了产品优化,结构调整,清洁生产,资源循环利用,节水降耗等工作,从源头削减了污染物的生产。同时投资二千多万元新建预处理装置三套,6000m3/d废水生化处理装置一套,使全厂乙烯酮(双乙烯酮)下游产品的废水得到了有效的治理。     

几种乙炔加压设备性能的比较

阐述并比较了几种加压设备在乙炔加压清净过程中的性能和特点。     

三种煤样燃烧热的测定

本文通过三个厂家提供的三种煤样燃烧热的测定,由测定结果综合得出3号煤样燃烧最完全、燃烧热也最大,是三个煤样中最好的一种。     

Semi-empirical equation of state of metals. Equation of state of aluminum

A semi-empirical equation of state for metals is described. Its capabilities are demonstrated by the example of the equation of state for aluminum. New experimental data are presented on the location of the isentrope of aluminum for unloading from the state at p = 229.71 GPa on the shock adiabat to an aerogel (SiO₂) of density 0.08 g/cm³. __________ Translated from Fizika Goreniya i Vzryva, Vol. 44, No. 2, pp. 61–75, March–April, 2008.     

小议汽车涂装工艺设计对涂装成本的影响

论述了涂装工艺设计对涂装设备投资、涂装生产成本的影响。     

水泥水化热测定方法综述

水泥水化热是中、低热水泥和核电工程用水泥的一项关键的技术指标。全球范围内测定水泥水化热的方法有溶解法、直接法/半绝热法、等温传导量热法三种。本文总结了中、美、欧相关方法标准,对其测试原理、仪器设备、试验过程等方面进行了比对,并对其在领域的应用做了简单的概括。     

Measurement of the gradient of viscosity with composition of mixtures of non-ideal gases

A perturbation viscometer is a differential capillary viscometer that measures the logarithmic viscosity gradient of the viscosity-composition curve for gas mixtures. Measurements are made at different gas mixture compositions. Integration of the logarithmic viscosity gradients measured over the full composition range gives the mixture viscosity relative to the viscosity of one of the pure components of the gas mixture. This method is attractive because, for measurements of equal precision, integration of the gradients is potentially an order of magnitude more precise than measurement of the viscosities directly. It can also work at high and low temperatures and perhaps high pressures.The perturbation viscometer has been used to make measurements on ideal gas mixtures at ambient and elevated temperatures. The situation is more complicated when the gas mixtures are non-ideal. Extra effects due to density differences, molar volume change on mixing and differential thermal expansion may be measured in addition to the desired viscosity change producing systematic errors in the results. Thus, a more sophisticated apparatus is required. The standard perturbation viscometer has been modified to separate out the extra effects to permit measurement of the true change in viscosity. In addition, the theoretical operation of the modified apparatus has been revised to account for the design changes to permit calculation of the viscosity-composition profiles from the results.The apparatus has been tested using helium-HFC-125 mixtures and two new viscosity-composition profiles are presented for these mixtures at 23 and . Internal consistency tests have been used to confirm that the data produced are of high quality with an estimated uncertainty in the viscosity ratio data at of 0.9% and at of 1.5%.     

Calorimetric and Computational Study of Enthalpy of Formation of Diperoxide of Cyclohexanone

A thermochemical rather simple experimental technique is applied to determine the enthalpy of formation of Diperoxide of ciclohexanone. The study is complemented with suitable theoretical calculations at the semiempirical and ab initio levels. A particular satisfactory agreement between both ways is found for the ab initio calculation at the 6–311G basis This set level. Some possible extensions of the present procedure are pointed out.     

塔设备改造选型的分析

就当前扩产增容中塔设备设计和改造时板式塔和填料塔的选型问题加以分析。在评述目前国内常用的几种塔板和新型填料之后，着重介绍一种新型塔板（导向梯形浮阀塔板）和一种新型填料（波环填料——乾隆帕克）。     

Effect of degree of deacetylation of chitin on the properties of chitin crystallites

In the present article, chitin from crab shell was systematically deacetylated using a NaOH treatment with control of the reaction time. The degree of deacetylation, monitored using solid-state NMR, revealed that the reaction was pseudo-first order. Based on this, swollen and NaOH-saturated particles are proposed as the reaction system. The weight loss of the partially saponified and neutralized samples after HCl hydrolysis increased linearly with the degree of deacetylation. The crystallinity of the samples was found to increase after acid hydrolysis. According to conductimetric titration, the surface charge density of the crystallites, after acid hydrolysis, was found to increase with base treatment time. The effect of surface charge on the formation of a chiral nematic phase, due to the rodlike nature of the crystallites, was explored. These results show that because the contribution of charged particles to the ionic strength was significant the double layer compression was affected, especially since the surface charge density was close to the Manning limit. © 1997 John Wiley & Sons, Inc. J Appl Polym Sci 65:373–380, 1997