Synthesis and characterization of novel copolymers with the trimethylsilyl group for deep‐UV photoresists

N‐(4‐Acetoxyphenyl) maleimide (APMI) and three kinds of comonomers bearing a trimethylsilyl group were copolymerized at 60°C in the presence of azobisisobutyronitrile (AIBN) as an initiator in 1,4‐dioxane to obtain the three IP, IIP, and IIIP copolymers. These copolymers were removed from the acetoxy group in a transesterification process into new IVP, VP, and VIP copolymers with a pendant hydroxyl group. Two modified processes were adopted to prepare photoresists using these copolymers. The first process involved mixing the dissolution inhibitor, o‐nitrobenzyl cholate, with the new copolymers. Second, o‐nitrobenzyl cholate was introduced into the copolymers using 1,8‐diazabicyclo[5.4.0]undec‐7‐ene (DBU) in dimethylformamide (DMF). The cyclic maleimide structure is responsible for the high thermal stability of these copolymers. After irradiation using deep–UV light and development with aqueous Na₂CO₃ (0.01 wt %), the developed patterns showed positive images and exhibited good adhesion to the silicon wafer without using any adhesion promoter. The resolution of these resists was at least 0.8 μm and an oxygen‐plasma etching rate was 1/5.3 to that of hard‐baked HPR‐204. © 2002 Wiley Periodicals, Inc. J Appl Polym Sci 83: 2791–2798, 2002; DOI 10.1002/app.10255     

R12TAB/正丁醇/正癸烷/水体系相态的研究

绘制了阳离子表面活性剂R12TAB／正丁醇／正癸烷／水体系的拟三元相图，确定了微乳液区、微乳液／液晶共存区及不同液晶区域的范围。用^2HNMR和差示扫描量热法(DSC)与液晶纹理相互对照，研究了该体系的液晶结构特点。结果表明：含质量分数为25％～75％正癸烷的各相图内，除了存在着层状、六角状单相液晶区和层状／六角状／立方状共存的混合液晶区域外，还存在着液晶／微乳液共存的区域，且随着正癸烷质量分数的增加，微乳液及液晶区域逐渐缩小。     

高沸点溶剂法合成原乙酸三甲酯

对低沸点溶剂法制备原乙酸三甲酯工艺进行了改进，比较了煤油、2-乙基己醇、氯苯、异佛尔酮、邻苯二甲酸二丁酯、乙二醇二丁醚等高沸点溶剂对反应的影响，筛选出最优高沸点溶剂煤油：研究了新反应体系的醇解pH值、溶剂的循环使用次数对反应的影响及溶剂循环损耗率，结果表明，醇解的最佳pH值为5．6；随着溶剂循环次数增加，原乙酸三甲酯收率从83．6％(1次)逐渐下降到76．7％(16次)；溶剂次平均损耗率4．6％。实现了直接蒸馏产品，溶剂循环使用的新工艺。避免了旧工艺先蒸溶剂，后蒸产品，产品大量分解，收率低等缺点。     

溴化十六烷基三甲基铵胶束高效液相色谱的研究和应用

研究了苯、苯胺、苯酚和甲苯在以溴化十六烷基三甲基铵(CTAB)水溶液为移动相,YWG-NH_2为固定相时的保留行为。当柱温为45℃、移动相组成为5%正丙醇(或9%乙醇)的0.03mol/L CTAB 时,苯、苯胺、苯酚和甲苯分离最佳。还计算了溶质传质过程的焓值及其在水、胶束、固定相间的分配系数。     

高分子和盐对3-十二烷氧基-2-羟丙基三甲基溴化铵泡沫性能的影响

测定了3-十二烷氧基-2-羟丙基三甲基溴化铵(C12TAB)在PVP、PEG和溴化钠存在下的泡沫性能。结果表明：含量相同时，C12TAB／NaBr混合体系的起泡性能高于C12TAB／高分子体系，而稳泡性能低于后者。含量相同的C12TAB／高分子体系，PVP对C12TAB的影响好于PEG。     

活性中间体失水甘油基三甲基氯化铵的性质研究

以环氧氯丙烷和三甲胺为原料 ,常温下合成活性中间体失水甘油基三甲基氯化铵 (GTA)。通过对GTA的吸水性和水解性的定量分析可知 :温度上升水解加快 ,吸水减慢 ;吸水与水解都随时间延长加强。在较低浓度的GTA水溶液中 ,随时间的延长GTA逐渐水解失效 ,但质量分数为 70 %～ 80 %的GTA稠浆的分解速率常数却很小。     

HPCS-AM-DAC共聚物的合成及絮凝性能研究

以羟丙基壳聚糖(HPCS)、丙烯酰胺(AM)、丙烯酰氧乙基三甲基氯化铵(DAC)为原料合成三元高分子共聚物(HPCS-AM-DAC)。采用FTIR、1HNMR、XRD、SEM对其结构和形貌进行了表征。考察了反应温度、引发剂硝酸铈铵用量、单体滴加时间及DAC用量对产物阳离子度及特性黏数的影响。结果表明,在水为25 mL、丙烯酰胺为2 g、HPCS为1 g、反应温度70℃、引发剂用量为1.7%(以HPCS质量为基准,下同)、单体滴加时间为35min、DAC为3.5g的条件下,产物的阳离子度和特性黏数均达到较佳值,分别为63.01%和468.81mL/g。采用壳聚糖(CTS)、HPCS、HPCS-AM-DAC及市售阳离子聚丙烯酰胺(CPAM)对高岭土模拟废水进行絮凝实验,考察了絮凝体系pH、不同絮凝产品投加量对浊度去除率的影响。结果表明,在浊度为200NTU的高岭土模拟废水中,HPCS-AM-DAC絮凝的适宜pH为2～6,适宜投加量为2～5 mg/L,在该条件下浊度去除率均在96%以上。     

烷氧基羟丙基三甲基溴化铵/正丁醇/水体系的相行为

绘制了3-十二烷氧基-2-羟丙基三甲基溴化铵(R12TAB)／正丁醇／水三元体系的相图，确定了不同区域的范围。用电导法测定了微乳液区域内由W／O型微乳液经双连续结构到O／W型微乳液的变化过程。用^2HNMR和差示扫描量热法(DSC)并与液晶纹理对照，研究了该体系的液晶结构特点。结果表明，固定R12TAB和正丁醇的比例，随含水量的增加，体系的液晶相结构发生如下变化，从层状液晶→层状与六角状液晶共存→层状、六角状与立方状液晶共存→层状液晶与微乳液共存。     

Effects of residual concentration of collector CTAC on flotation behavior of illite

ABSTRACT

In present study, illite flotation behavior with Cetyl Trimethyl Ammonium Chloride (CTAC) as the collector has been studied to investigate the effects of its residual concentration on froth stability and flotation. Results showed that, with increasing conditioning time, the residual concentration (frother concentration) and froth height decreased simultaneously, while the adsorbed amount (particle hydrophobicity) increased. Increasing CTAC conditioning time decreased the residual concentration in solutions, resulting in poor froth stability and flotation recovery at high pH; the adsorption rate of CTAC on illite surface was relatively high at higher pH due to strong electrostatic mechanism, making CTAC residual concentration decrease.     

高真空扩散泵油275^#生产工艺改进

简述了高真空扩散泵油275^#的生产工艺,分析了水解釜材质和精馏系统存在的问题,提出了改造意见,并比较了改造效果。结果表明,将水解釜材质由搪瓷更换成不锈钢后,既节约原材料消耗,又减少水洗过程中的物料损失和排污量,从而大幅度降低了产品的生产成本;精馏系统装置经过改造后,产品中的三甲基五苯基三硅氧烷含量比改造前生产的产品高出15个百分点,提高到84%以上;且产能翻一番。