气相色谱法测定2—叔丁基—4,5—二氯—3（2H）—哒嗪酮

本文采用以ＯＶ－１０１为固定液，邻苯二甲酸二乙酸为内标物的气相色谱分析，ＦＩＤ检测２－叔丁基－４，５－二氯－３（２Ｈ）－哒嗪酮。该法标准偏差０．３２，变异系数１．０６％，该方法回收率在９９．３％，该方法回收率在９９．３－１００．８％。     

2,5—二巯基—1,3,4—噻二唑的催化合成

以低碳叔胺为催化剂合成了２，５－二巯基－１，３，４－噻二唑，反应收率高达９９．０％，产品纯度达９９．７８％。讨论了催化剂处类对反应收率的影响。     

N,N—二甲基—（2Z,4E）—壬二烯胺的合成

通过２－甲基吡啶的烷基化，部分还原，Ｈｏｆｆｍａｎ消除开环，立体选择性合成了马尾松毛虫性信息素的前体Ｎ，Ｎ－二甲基－（２Ｚ，４Ｅ）－壬二烯胺，其全合成的总化学产率为２５．４％，异构体纯度高达９２．０％，并分析了ＮａＢＨ４还原２－烷基吡啶的机理。     

高效液相色谱法测定2—特丁基—4,5—二氯—3（2H）—哒嗪酮

采用高效液相色谱法，以甲醇作流动相测定２－特丁基－４，５－二氯－３（２Ｈ）－哒嗪酮。该法标准偏差为０．１７，变异系数为０．２３％，平均回收率为９９．８５％。方法线性关系了用气相色普法相关系数为０．９９９９，回归方程为ｙ／０．００８２＋１．３０８５ｘ。     

α相和β相氮化硅的形成机理与动力

使用气流磨粉碎的硅粉（Ｓｉ）（Ｓｉ９９．３％，ｄｐ＝５．１μｍ，Ｓｇ＝３．２ｍ＾２／ｇ）和氮气（Ｎ２）（纯度９９．９９９８％）为反应物，在１３００～１３６７℃下反应形成β－Ｓｉ３Ｎ４，其反应机理与动力学参数被研究。反应产物由ＸＲＤ进行定量分析，相形成的机理和它们的形态用扫描电镜（ＳＥＭ）确定，我们发现α相和β相的形成机理不同，β－Ｓｉ３Ｎ４在１３００℃的实验数据适合于界面化学反应控制的动力学模型，     

2,4—二羟基苯甲酸合成工艺研究

介绍了合成２，４－二羟基苯甲酸的改良水溶液法新工艺，循环反应收率高达９０％，综合收率８５％，产品纯度９９．４％（化学法测定）。     

愈创木酚的合成研究

在水－甲苯二元非均相体系中,以ＰＥＧ－８００为相转移催化剂,由邻苯二酚、一氯甲烷和氢氧化钠合成了愈创木酚。得出了最佳反应条件：ｎ（邻苯二酚）：ｎ（一氯甲烷）：ｎ（ＮａＯＨ）＝１．０：１．４：１．１（ｍｏｌ：ｍｏｌ：ｍｏｋ）,反应温度为１４０℃,反应时间为４ｈ,ＰＥＧ－Ｌ８００用量５％,产品纯度达９９％,产率为８０％。     

苯乙烯—丙烯酸丁酯—丙烯酸羟乙酯共聚物的合成及其与二异氰酸 …

当混合溶剂乙酸丁酯／二甲苯质量比为１：１,过氧化苯甲酰（ＢＰＯ）为１％,苯乙烯（Ｓｔ）／丙烯酸丁酯（ＢＡ）＋丙烯酸羟乙酯（ＨＥＡ）（质量比）为６２：３８,反应温度为１３３℃时,可获得卖座经率为９５．３％,「η」为０．１６ｄＬ／ｇ的Ｓｔ－ＢＡ－ＨＥＡ共聚物。该共聚物（ＨＥＡ的结合量为２－４％）在同一溶剂中加入甲苯二异氰酸酯（ＴＤＩ）或聚醚型二异氰酸酯（ＰＥＤＩ）,当一ＮＣＯ／－ＯＨ摩尔比为１．２－１     

2,4—二氯苯甲酰氯的合成

２，４－二氯甲苯经光氯化、水解、氯酰化、精馏合成２，４－二氯苯甲酰氯，总收率达９０％以上，产品纯度大于９９％。     

4—甲基苯基苯甲酮的合成研究

以苯甲酰氯,甲苯为原料,在催化剂三氯化铝存在下合成了４－甲基苯基苯甲酮。物料配比为苯甲酰氯：三氯化铝：甲苯＝１：１．４：６．２（摩尔比）。在反应温度１００℃,反应时间８ｈ条件下,产品收率８７．５％,纯度大于９９％。用色质 红外光谱证实了结构。     

Separation of ethylene glycol, 1,2-butanediol and 1,2-propanediol with azeotropic distillation

1,2-butanediol (1,2-BDO) and 1,2-propanediol (1,2-PDO) are inevitably side produced in the ethylene glycol (EG) production processes from non-petroleum routes, but are very difficult to separate by the ordinary distillation method because of the closeness of their boiling temperatures to EG, thus compromise the economy of these processes. The azeotropic distillation process using 1-octanol (CPO) as an entrainer to separate EG and 1,2-BDO mixture with or without 1,2-PDO was studied in this paper. Four binary vapour–liquid equilibrium data of EG-1,2-BDO, EG-CPO, 1,2-BDO-CPO, and 1,2-PDO-CPO were measured using an Ellis equilibrium kettle and regressed with the thermodynamic model of non-random two liquid to obtain the corresponding binary interaction parameters. On this basis, azeotropic distillations with CPO as an entrainer were designed to separate EG and 1,2-BDO with or without 1,2-PDO. The complete separation processes, including the azeotropic distillation and CPO recovery process consisting of extraction with H₂O and subsequent distillation, were simulated and optimized with Aspen Plus for both the EG-1,2-BDO binary mixture and the EG-1,2-BDO-1,2-PDO ternary mixture. The simulation results show that the azeotropic distillation method with CPO as an entrainer can effectively separate the mixture of EG-1,2-BDO and EG-1,2-BDO-1,2-PDO, achieving EG of 99.90% purity with 99.98% recovery and 1,2-BDO of 99.30% purity with 99.45% recovery for the binary mixture, and achieving EG of 99.90% purity with 99.80% recovery, 1,2-BDO of 99.35% purity with 99.35% recovery, and 1,2-PDO of 90.59% purity with 94.38% recovery for the ternary mixture. These processes are promising for industrial application and can significantly improve the economy of non-petroleum EG production.     

萘哌地尔合成工艺的改进

改进了萘哌地尔的合成工艺条件：投料比n（3-（1-萘氧基）-1,2-环氧丙烷）∶n（邻甲氧基哌嗪氢溴酸盐）∶n（K2CO3）=1.01∶1∶1.5,以氯仿-水的非均相溶液为反应溶剂,在回流温度（60~63℃）反应5h制得萘哌地尔粗品;再以丙酮-水（4∶1）为溶剂,精制得到高纯度的成品（纯度≥99%）。该工艺条件温和,操作简便,产品质量稳定可靠,两步总收率达到72.3%。     

左旋异胡薄荷醇的催化合成

以(+)-香茅醛为起始原料,溴化锌为环化催化剂制取(-)-异胡薄荷醇,反应收率为70.7%。反应粗品经分馏后,(-)-异胡薄荷醇含量在94%以上,后者经丙酮重结晶,可获得光学纯度为99.6%(e.e.)的(-)-异胡薄荷醇。     

比沙可啶的合成工艺研究

以2-吡啶甲醛为起始原料,在浓硫酸催化下,与苯酚缩合得到4,4'-二羟基二苯基-(2-吡啶)-甲烷和2,4'-二羟基二苯基-(2-吡啶)-甲烷,利用二者在乙酸乙酯中溶解度的差别,分离得到4,4'-二羟基二苯基-(2-吡啶)-甲烷,用氢氧化钠转变得到酚钠盐后,经乙酰化得到比沙可啶。其结构经核磁共振氢谱确证,纯度经液相色谱分析为99%。改进后的合成工艺操作简便,收率可达58%。     

农药中间体1-己烯5-酮的合成研究

利用乙酰乙酸乙酯与溴丙烯在EtOH／EtONa条件下发生取代反应，然后在NaOH溶液中加热水解，产物在H2SO4溶液中加热脱羧得1-己烯-5-酮，产率为72-75％。产物结构经IR、NMR谱图得到确认。     

One-Step Extraction and Concentration of Polyunsaturated Fatty Acids from Fish Liver

The fatty acids (FA) eicosapentaenoic acid (20:5ω-3; EPA) and docosahexaenoic acid (22:6ω-3; DHA), which have several health benefits, have been concentrated from mako shark liver (Isurus oxyrinchus). The process was carried out in one single step, in which fish liver oil was simultaneously extracted, saponified and concentrated. Additionally, the polyunsaturated fatty acids (PUFA) concentrate was winterized to crystallize the remaining saturated FA, resulting in a further increase in the concentration of DHA and EPA. Two variables, temperature and water concentration in the saponification mixture, were optimized to increase the concentration of ω-3 PUFA. Best results were obtained at 12 °C and 0% water content in the mixture, obtaining 17.8% purity and 77.6% yield of EPA; DHA purity and yield were 33.3 and 82.2%, respectively.     

高纯度叶黄素的制备及稳定性研究

金盏菊萃取物20g,加入正丁醇40mL,密封搅拌均匀后(55℃),加入维生素C0 2g,再加入40mLw(NaOH)=20%的水溶液在70℃进行皂化反应8h。皂化物中加入400mL水,搅拌均匀后,过滤,得到叶黄素,w(C40H56O2)=94%。将其用V(CH2Cl2)∶V(CH3OH)=2∶1结晶,叶黄素质量分数可提高至w(C40H56O2)=98%,抗氧化剂、温度、光、氧气对叶黄素的稳定性具有重要影响。     

四乙酰基二氯乙酰基六氮杂异伍兹烷的硝解研究

研究了几种硝解剂及硝解条件对四乙酰基二氯乙酰基六氮杂异伍兹烷（TADCIW）硝解产物的纯度和得率的影响。讨论了有关的机理,用发烟硝酸-浓硫酸或碱金属硝酸盐-浓硫酸硝解TADCIW,可得到纯度很高的四硝基二氢乙酰基六氮杂异伍兹烷（TNDCIW）,得率达到94%-98%,硝解时间短,硝硫混酸可以再利用;但用发烟硝酸-五氧化二磷或浓硝酸-浓硫酸硝解TADCIW的得率很低。     

双环戊二烯二甲酸的合成与表征

利用双环戊二烯加热分解制得环戊二烯，在四氢呋喃中ＣＰＤ与Ｎａ反应得到ＣＰＤＮａ，再与干冰混合，加水溶解，中和，过滤，干燥，即得双环戊二烯二甲酸。考察了ＣＰＤＮａ与干冰混合反放置时间对收率和产物纯度的影响。     

Production of high purity rare earth mixture from iron-rich spent fluid catalytic cracking (FCC) catalyst using acid leaching and two-step solvent extraction process

Acid leaching and a two-step solvent extraction procedure were developed to produce high purity mixture of La and Ce from iron-rich spent FCC catalyst discharged from Dzung Quat refinery (Vietnam). Acid leaching of the spent catalyst with 2M HNO₃ and a solid-to-liquid ratio of 1/3 at 80 °C in 1 h dissolved almost 90% of La while 12% of Al and 25% of Fe were transferred to the leachate. The extraction of RE metals and main impurities such as Al and Fe by a mixture of di-2-ethylhexyl phosphoric acid (D2EHPA) and tributyl phosphate (TBP) was investigated. Experiments showed that it was necessary to remove Fe before extracting RE and the optimum extraction conditions for a high recovery of RE while 0% of Al extraction were pH-1, contact time=10min, and D2EHPA/TBP volume ratio= 4: 1. At these conditions, the extraction yields of La(III) and Ce(III) were 72% and 89%, respectively. A two-step solvent extraction was developed to achieve a high purity of RE mixture, which included (1) the removal of impurity Fe by 25% (v/v) diisooctyl phosphinic acid (DiOPA) in n-octane for 140 min, (2) the extraction of rare earths by a mixture of di-2-ethylhexyl phosphoric acid (D2EHPA) and tributyl phosphate (TBP) in n-octane for 10 min without the need for adjusting the pH of the leaching solution.