3,4—二氯硝基苯合成工艺改进

对邻二氯苯硝化合成３,４二氯硝基苯反应中的异构体组成进行探讨,对位组分收率提高了１０．１４％。     

3,4-二氯苯酚的合成研究

以邻二氯苯为原料,经硝化、还原、重氮化合成3,4-二氯苯酚,通过正交试验,找出了三步反应的优化反应条件。硝化反应混酸（硝酸：硫酸）物质的量比为1：3．5,邻二氯苯与硝酸的物质的量的比为1：1．3,反应温度为50℃,3,4-二氯硝基苯收率94．0％;用铁粉作还原剂,以7．0％NH4Cl水溶液作为还原介质,3,4-二氯苯胺的收率92．5％;重氮化反应的优化条件为3,4-二氯苯胺：亚硝酸钠：硫酸的物质的量比为1：1．2：8,3,4-二氯苯酚收率为91．7％。     

3，4－二氯三氟甲苯的合成方法

本文介绍了以对氯甲苯为原料．经光氟化、氟化、核氟化，制备３．４－二氟三氟甲苯，并为工业化生产提供了可行的工艺条件。     

3，5－二氯－1－甲基－4－吡唑羧酸的制备

３，５－二氯－１－甲基－４－吡唑羧酸酯作为起始原料，用一步法制备了３，５－二氯－１－甲基－４－吡唑羧酸。     

3，5－二氯－1－甲基－4－吡唑羧酸的制备

３，５－二氯－１－甲基－４－吡唑羧酸酯作为起始原料，用一步法制备了３，５－二氯－１－甲基－４－吡唑羧酸。     

连续化合成3,4-二氯硝基苯

以1,2-二氯苯为原料,以硝酸/硫酸为硝化剂,经连续硝化反应合成了3,4-二氯硝基苯,原料1,2-二氯苯的转化率达到99.8%以上,产物3,4-二氯硝基苯的纯度达到97%,二硝化物杂质含量低于0.1%。     

由2，4－二硝基氯苯制备3，4－二氟硝基苯

２，４－二硝基氯苯经二步氟化反应，制得低成本３，４－二氟硝基苯。     

有机中间产品3，5-二氯硝基苯合成条件的研究

研究了以2,6-二氯-4-硝基苯胺为原料,合成3,5-氯苯胺的中间体3,5-二氯硝基苯的工艺条件。通过实验讨论了硫酸用量、乙醇用量、反应温度、时间、催化剂等各种因素对产品产率的影响,确定了最佳合成条件。结果表明：在最佳合成条件下,得到的产品收率可达79．6％。     

影响热压铸产品流蜡的因素探讨

低压注射成型即热压铸成型工艺是精密陶瓷成型方法中较常见的一种工艺方法,其中成型后产品的脱蜡工序是整个生产工序中较重要的一个环节,在此环节币容易出现产品“流蜡”缺陷。本文从产品排蜡的机理分析了影响排蜡过程中导致流蜡的几个影响因素。     

ANALYSIS OF FACTORS AFFECTING THE SYNTHESIS OF ALLYL PHENYL ETHER BY TRI-LIQUID-PHASE CATALYSIS

In order to improve the selectivity of allyl phenyl ether (ROPh), the main product, in the etherification of allyl bromide (RBr) and sodium phenolate (NaOPh) with tetra-n-butylammonium bromide (QBr) as a phase-transfer catalyst, the technique of tri-liquid-phase phase-transfer catalysis, instead of the liquid-liquid one, was employed. The reaction was performed in a batch reactor, and the factors affecting the conversion and selectivity were investigated. The possibility of reusing the phase-transfer catalyst was also evaluated. Experimental results indicate that the addition of a small amount of Na₂CO₃ will benefit the formation of a third liquid phase and enhances both the conversion of RBr and the overall yield of ROPh. Both the conversion and the overall yield are maximal when the mole fraction of QBr in the mixture of NaOPh and QBr is about 0.3. A high reaction temperature enhances the conversion and the overall yield. Under optimal conditions, complete conversion and near 100% yield can be obtained within 10 minutes. Although the reaction rate by the tri-liquid-phase catalysis is slightly lower than that observed with the same amount of catalyst by conventional liquid-liquid phase-transfer catalysis, the selectivity of ROPh is higher and the catalyst can be easily reused by the reuse of the third liquid phase without any loss of its catalytic activity in the former case. Because the reuse of catalyst was found to be feasible, the production of ROPh with a continuous-flow reactor becomes possible.     

ANALYSIS OF FACTORS AFFECTING THE SYNTHESIS OF ALLYL PHENYL ETHER BY TRI-LIQUID-PHASE CATALYSIS

In order to improve the selectivity of allyl phenyl ether (ROPh), the main product, in the etherification of allyl bromide (RBr) and sodium phenolate (NaOPh) with tetra-n-butylammonium bromide (QBr) as a phase-transfer catalyst, the technique of tri-liquid-phase phase-transfer catalysis, instead of the liquid-liquid one, was employed. The reaction was performed in a batch reactor, and the factors affecting the conversion and selectivity were investigated. The possibility of reusing the phase-transfer catalyst was also evaluated. Experimental results indicate that the addition of a small amount of Na₂CO₃ will benefit the formation of a third liquid phase and enhances both the conversion of RBr and the overall yield of ROPh. Both the conversion and the overall yield are maximal when the mole fraction of QBr in the mixture of NaOPh and QBr is about 0.3. A high reaction temperature enhances the conversion and the overall yield. Under optimal conditions, complete conversion and near 100% yield can be obtained within 10 minutes. Although the reaction rate by the tri-liquid-phase catalysis is slightly lower than that observed with the same amount of catalyst by conventional liquid-liquid phase-transfer catalysis, the selectivity of ROPh is higher and the catalyst can be easily reused by the reuse of the third liquid phase without any loss of its catalytic activity in the former case. Because the reuse of catalyst was found to be feasible, the production of ROPh with a continuous-flow reactor becomes possible.     

改性压实水泥抗压强度影响因素的研究

采用ＤＳＰ原理和压实技术相结合，掺加硅灰和ＣａＣＯ３等细颗粒矿物外加剂改变压实水泥材料基质。研究了成型压力、细粉掺量、养护制度等因素对压实水泥强度的影响。结果表明，掺加适量硅灰和提高成型压力可显著提高压实水泥的抗压强度，掺加ＣａＣＯ３对强度无明显影响；压实水泥存在最佳养护龄期，超过此龄期强度倒缩。     

炭膜处理印染废水的影响因素

用不同孔径的酚醛树脂基管状微滤炭膜,对两种模拟染料废水溶液进行处理,考察了膜孔径、原料液浓度、测试压力和测试时间对截留率和膜通量的影响。实验结果表明,微滤炭膜对模拟染料废水有较好的处理效果,截留率和膜通量受膜孔径及操作条件的影响。     

DNBP的合成及动力学研究

ＤＮＢＰ是一种重要的苯乙烯用阻聚剂,笔者提出了在有机溶剂中用硝酸直接硝化制ＤＮＢＰ的新方法,实验确定了反应条件对ＤＮＢＰ收率的影响,并获得了适宜的合成工艺条件。在此基础上,进行了上述反应的动力学研究,获得了此硝化反应的动力学方程方式为（－ｒＡ＝１．５８＊１０＾４ｅｘｐ（－１７５８６／ＲＴ。     

间歇合成PET中影响产品色相的因素

探讨了间歇合成 PET(包括间歇法、半连续法 )中影响产品色相的因素主要有原材料质量 ,乙二醇与对苯二甲酸 ( EG/ PTA)的摩尔比、添加剂、氮气纯度等。     

乳化结晶法精制粗蒽的影响因素

采用乳化结晶法,研究了粗蒽精制过程中溶剂、温度、助剂及分离时间的作用。实验结果表明,只有与水部分互溶的溶剂、粗蒽、水、乳化剂、添加剂形成的乳化液才能有效、高选择性地分离蒽与其他组分。溶剂种类和分离温度是影响产物蒽量与蒽收率的主要因素。粗蒽精制的适宜参数为：醛作溶剂,分离温度95℃,升温速率10℃／min,尿素用量2％,分离时间30min。     

非均相硝化反应器的最佳中试容积

在5个几何相似的具有双排蛇管的模拟硝化反应器中,测定了不同工况下液液湍流搅拌分散系统的Sauter直径和固液混合系统相两相的停留时间分布（RTD）。关联出了Sauter直径与相比、转速、搅拌浆叶直径之间的关系式,得到了固液系统流体流动模型的模型参数。由各参数随硝化反应器容积的变化规律,确定了硝化反应器的最佳中试容积。     

影响爆轰合成纳米金刚石收率因素

利用负氧平衡炸药爆轰合成纳米金刚石的成功,是人工合成金刚石技术的又一重大进展,由于纳米金刚石其金刚石和纳米结构的双重特性而受到广大工程技术专家的关注.炸药爆法是目前合成纳米金刚石的唯一方法,TNT和RDX则是最常用的两种炸药.提高产品品质,降低生产成本,以利于其产业化和应用的推广,是摆在研究者面前的重要课题.文章就影响爆轰合成纳米金刚石收率的因素--合成参数、药包几何形状、引爆物功率和冷却介质等问题做了较为详细的阐述,以达到合成参数进行综合优选的目的.