苯酚改性脲醛树脂合成工艺及性能的研究

用苯酚作为改性剂,采用高温(90℃)缩聚反应合成改性脲醛树脂胶粘剂,改进了合成工艺,缩短了反应时间。通过引入苯环改善了耐水、耐老化性能。分析了各因素对改性脲醛树脂的影响,得到甲醛、尿素、苯酚摩尔比为10:8:1时树脂性能最佳,胶合强度和木破率均达到GB／T 17656-1999标准规定值。     

双亚磷酸酯类抗氧剂626合成的工艺

摘要以新工艺合成了双（2，4-二叔丁基苯基）季戊四醇二亚磷酸酯（抗氧剂626）。先以三氯化磷与2，4-二叔丁基苯酚反应合成出中间体（2，4-二叔丁基苯基）二氯亚磷酸酯，再将其与季戊四醇反应合成出产品。探索了反应条件，溶剂及催化剂的种类等因素对产品收率和质量的影响，筛选出最佳的合成工艺条件为：以甲苯或二甲苯为熔荆，体系保持负压至常压，第一步反应温度40—50℃，反应2h，第二步反应温度50—130℃，反应6h，反应收率为86％。     

微波消解法测定化学需氧量

探讨利用微波消解法代替回流加热，缩短了测定时间，并与标准法进行准确度比较。     

反相高效液相色谱法测定meso-四苯基卟啉钴的纯度

采用反相高效液相色谱法测定合成meso-四苯基卟啉钴的纯度;以甲醇乙腈二氯甲烷(体积比为55∶35∶10)为流动相,ShimpackCLCODS柱(150mm×6.0mmi.d,5μm)为分离柱,流速为1.5mL/min,检测波长420nm;meso四苯基卟啉钴的测定在1.0～10μg/mL时线性关系良好(相关系数r=0.9993),加标回收率为97.03%～101.42%,重复进样的相对标准偏差RSD为0.64%～2.92%(n=5)。方法的准确度高,精密度好,实际应用效果好。     

聚醋酸乙烯酯树脂聚合度的快捷检测方法

通过实验得出不同聚合度、不同质量分数下的黏度数据，并作出平均聚合度-质量分数-黏度三者的关系曲线。在此基础上，提出通过检测聚醋酸乙烯酯树脂的质量分数和黏度，直接查出对应的聚合度的快速检测方法。     

神经网络-光度法同时测定食品中防腐剂和甜味剂

根据食品中常用防腐剂本甲酸和山梨酸及甜味剂糖精钠在紫外区均有吸收的特点，建立了一种以紫外分光光度法为基础对该三组分同时测定的方法，光谱数据采用作者自编的径向人工神经网络MATLAB程序进行处理，苯甲酸、山梨酸和糖精钠的平均标准偏差分别为1.60%、5.23%和1.21%，回收率大为95.0-102.0%之间，将该法应用于食品中二组分的测定，获得较为满意的结果。     

氧化淀粉变性基团的分析方法

介绍了淀粉工业中氧化淀粉变性基团羧基和羰基的测定方法     

Poly(p-tert-butoxycarbonyloxystyrene): a convenient precursor to p-hydroxystyrene resins

An efficient synthetic route to pure, high molecular weight poly(p-hydroxystyrene) is reported. The route involves synthesis of a new monomer, p-tert-butoxycarbonyloxystyrene, polymerization by radical initiation or by cationic initiation in liquid SO₂, followed by thermolysis or acidolysis of the tert-butoxycarbonyl protecting group. Porous, crosslinked resin beads containing the nucleophilic, phenol pendant group have been prepared in a similar fashion from the precursor terpolymer of p-tert-butoxycarbonyloxystyrene, styrene and divinylbenzene. The utility of this resin for solid-phase synthesis has been demonstrated.     

气相色谱-质谱联用法测定金属皂中的多环芳烃

建立了金属皂中16种美国环保局(EPA)优先监控的多环芳烃的气相色谱-质谱(GC/MS)联用测定方法,样品先用二甲基亚砜萃取,再用环己烷进行反萃取,经硅胶柱净化后,用GC/MS分离测定。优化了16种多环芳烃(PAHs)的分离测定条件,结果16种PAHs的平均回收率为75.32%￣98.72%,精密度实验相对标准偏差(RSD)为2.19%￣6.93%,检测限(S/N=5)为0.002￣0.010mg/kg。该方法灵敏度高、准确性好,完全可以满足金属皂中多环芳烃的检测要求。     

The mechanism of the poisoning of ammonia synthesis catalysts by oxygenates O2, CO and H2O: an in situ method for active surface determination

The effect of adding an oxygenated poison (O₂, CO or H₂O) to a hydrogen/nitrogen stream producing ammonia over a triply promoted (K₂O, CaO, Al₂O₃) commercial catalyst is not unsurprisingly rapidly to poison the catalyst. However, immediately the oxygenated poison reacts with the catalyst and before total poisoning has occurred, which in these experiments took 10 min, there was an explosive release of ammonia producing concentrations in the gas phase in excess of the equilibrium value. This is thought to be due to a convulsive reorganisation of the surface of the catalyst in forming regions of an oxide overlayer, resulting in the expulsion of the standing surface nitrogen atom coverage as ammonia. However, in contradistinction to the observation of complete poisoning of the triply promoted catalyst shortly after switching the water (2.9%) into the hydrogen/nitrogen stream, when polycrystalline iron was used as the catalyst, after the initial pulse of ammonia was observed, the small quantity of water (2.9%) in the hydrogen/nitrogen stream resulted in an increased rate ( ×3) of ammonia synthesis which declined only slightly over the twenty minute duration of the experiment. The difference in behaviour between the triply promoted catalyst and the polycrystalline iron is thought to be due to the relative ease of reduction of the latter, so that submonolayer quantities of oxide can be stabilised on the surface of the polycrystalline iron. The promoting effect of this oxide overlayer is either structural or electronic; no distinction can be made from these experiments. The technique of injecting either O₂ or CO into a hydrogen/nitrogen stream which is producing ammonia over promoted catalysts in quantities insufficient to cause complete poisoning and measuring the oxygen coverage of the catalyst to a measured decrease in the ammonia synthesis rate, appears to be a ready, in situ method for the determination of the active catalyst area.