壳聚糖硫酸盐催化合成衣康酸二甲酯

以壳聚糖和硫酸为原料,制备了壳聚糖硫酸盐,利用红外及元素分析对壳聚糖硫酸盐进行了结构表征。将其用于催化衣康酸与甲醇合成衣康酸二甲酯的反应,考察了酸醇比、时间、催化剂用量、温度等条件对衣康酸二甲酯收率的影响,得到的最佳工艺条件为：壳聚糖硫酸盐用量占反应物料总质量的2%,n(甲醇)∶n(衣康酸)=7∶1,反应温度为140 ℃,反应时间6 h,在此条件下,产品收率为86.6%。衣康酸二甲酯经气质定性分析,气相色谱检测纯度大于98%。催化剂经简单干燥处理,循环使用5次后产品收率为84.0%。     

Enzymatic Glycerolysis of Palm and Palm Kernel Oils

Glycerolysis of palm and palm kernel oils were carried out using commercial lipases from Candida antarctica (Novozym 435) and Mucor miehei (Novozym 388) as catalyst (500 units lipase/g oil) at 40°C and with an oil:glycerol molar ratio of 1:2 in a solvent-free system. Novozym 435 catalyzed the glycerolysis of palm and palm kernel oils giving reaction products in similar compositions. Partial acylglycerols contents of the glycerolysis products obtained from palm and palm kernel oils were 64% (wt) and 66% (wt), respectively. However, partial acylglycerols contents of the glycerolysis products obtained from palm and palm kernel oils conducted with Novozym 388 as catalyst at the same conditions were 44% (wt) and 56% (wt), respectively. On the other hand, free fatty acid contents of the glycerolysis products of palm and palm kernel oils obtained using Novozym 388 were higher, 25–30% (wt), than those obtained by Novozym 435, 4–5% (wt). The monoacylglycerols fraction with the highest content of oleic acid, 62.7% (wt), was obtained from the palm kernel oil glycerolysis reaction catalyzed by Novozym 435.     

Enzymatic Glycerolysis of Palm and Palm Kernel Oils

Glycerolysis of palm and palm kernel oils were carried out using commercial lipases from Candida antarctica (Novozym 435) and Mucor miehei (Novozym 388) as catalyst (500 units lipase/g oil) at 40°C and with an oil:glycerol molar ratio of 1:2 in a solvent-free system. Novozym 435 catalyzed the glycerolysis of palm and palm kernel oils giving reaction products in similar compositions. Partial acylglycerols contents of the glycerolysis products obtained from palm and palm kernel oils were 64% (wt) and 66% (wt), respectively. However, partial acylglycerols contents of the glycerolysis products obtained from palm and palm kernel oils conducted with Novozym 388 as catalyst at the same conditions were 44% (wt) and 56% (wt), respectively. On the other hand, free fatty acid contents of the glycerolysis products of palm and palm kernel oils obtained using Novozym 388 were higher, 25-30% (wt), than those obtained by Novozym 435, 4-5% (wt). The monoacylglycerols fraction with the highest content of oleic acid, 62.7% (wt), was obtained from the palm kernel oil glycerolysis reaction catalyzed by Novozym 435.     

硫酸高铈催化合成乙酸丙酯

以硫酸高铈为催化剂,冰乙酸和正丙醇为原料,环己烷为带水剂合成乙酸丙酯,研究正丙醇与冰乙酸物质的量比、反应时间、催化剂用量及重复使用次数对酯化率的影响。经正交实验及单因素实验得到反应的最佳合成条件为:冰乙酸用量0.1 mol,醇酸物质的量比1.5,硫酸高铈用量1.1 g,反应时间2.0 h,此条件下,酯化率约为99%。该催化剂具有催化活性高、操作简单和不污染环境等优点。     

一锅法合成O-甲基-N-硝基异脲

采用尿素、硫酸二甲酯、硝酸、硫酸为原料一锅法合成O-甲基-N-硝基异脲。研究了反应温度、时间、催化剂、原料配比对反应收率的影响,确定了优化的工艺条件:原料配比n(尿素)∶n(硫酸二甲酯)=1.3∶1,温度70℃,催化剂50%硫酸,反应时间4 h,总收率为43%,含量在99%以上。     

Preparation and shaping of solid acid SO42-/TiO2 and its application for esterification of propylene glycol monomethyl ether and acetic acid

The solid acid SO42-/TiO2 was prepared by immersion method and applied for synthesis of propylene glycol methyl ether acetate (PMA) through esterification reaction of propylene glycol monomethyl ether (PM) and acetic acid (HAc).The optimal catalyst preparation condition was determined by orthogonal analysis of parameters in a five-factor and four-level test.The obtained solid acid catalysts were characterized in detail by means of X-ray powder diffraction,thermogravimetry,pyridine adsorbed IR analysis,scanning electron microscopy,and BET surface area method.Synthesis of PMA was studied in this paper through experimental investigation of reaction conditions such as temperature,molar ratio of reactants,catalyst dosage and agitation speed.Based on its possible reaction mechanism,a pseudo-homogeneous kinetic model was established and its activation energies Ea+ and Ea-.65.68 × 103 J· mol-1 and 57.78 × 103 J· mol-1,were estimated.To prepare shaped solid acid catalyst SO42-/TiO2,the shaping method of impregnation-shaping-impregnation was applied.The optimal molding formulation of solid acid catalyst,obtained from the orthogonal test,was found to be binder 7 wt％,reinforcing agent 20 wt％,pore forming material 2.5 wt％,and lubricant 4 wt％.The results of performance test of catalyst demonstrated that the shaped solid acid catalyst exhibited high activity and stability.     

固体酸SG/p-TSA催化合成乙酸乙酯

采用浸渍法制备硅胶(SG)/对甲苯磺酸(p-TSA)催化剂,并用XRD对其进行了表征。利用冰醋酸和无水乙醇为原料,以SG/p-TSA为催化剂合成乙酸乙酯。考察了反应时间,催化剂的用量,原料配比等对该反应的影响。最佳合成条件为:反应温度为100℃,反应时间为100 min,酸醇摩尔比为1.0∶1.9,催化剂用量为5%,产率为95.40%。催化剂不经处理可重复使用,使用3次以后的产率为81.11%。     

十二水合硫酸铁铵催化合成己二酸二丁酯的工艺研究

以十二水合硫酸铁铵为催化剂,己二酸与正丁醇为原料合成了己二酸二丁酯,讨论了醇酸物质的量比、催化剂用量、反应时间、带水剂等因素对酯化率的影响,确定了最佳工艺条件为：以0．1mol己二酸为基准,醇酸物质的量比为5．0：1,催化剂用量为5．og,反应时间为1．0h,不用带水剂,己二酸二丁酯的酯化率为98．2％。该催化剂具有催化活性高,反应时间短,酯化率高,与目前工业中使用的硫酸相比环境污染小,对设备几乎无腐蚀等优点,且十二水合硫酸铁铵价格低廉易得,性质稳定,不溶于反应体系,是一种很有发展前景的催化剂。     

对氨基苯甲酸乙酯的合成新方法

以高脱乙酰度的壳聚糖为原料,制备了酯化催化剂壳聚糖硫酸盐。以对氨基苯甲酸、无水乙醇为原料,在壳聚糖硫酸盐的催化下,通过微波辐射加热,合成出对氨基苯甲酸乙酯。讨论了催化剂用量、反应时间、微波辐射功率等条件,结果表明,微波辐射功率为300 W,对氨基苯甲酸0.01 mol,酸醇物质的比为1∶15,催化剂用量0.5 g,反应10 min时,反应条件最佳,收率达83.6%。     

硫酸钛催化合成乙酸丁酯的研究

以硫酸钛为催化剂合成了乙酸丁酯,确定了酯化反应适宜条件。结果表明,当冰乙酸用量为0.10mol,丁醇用量为0.083mol,硫酸钛用量为1.4g,回流反应90min时,乙酸丁酯收率可达92.6%。     

氨基磺酸法合成烷基糖苷硫酸酯铵盐的研究

以烷基糖苷和氨基磺酸为原料,在催化剂作用下合成了烷基糖苷硫酸酯铵盐。研究了催化剂种类、催化剂用量、投料比、反应温度等对反应的影响,确定了较佳的合成条件：n（APG）：n（氨基磺酸）=1：1.15,催化剂CAT用量为反应物料的3%,反应温度为110℃,反应时间为3h,产品中阴离子活性物含量为88.9%。     

硫锆催化合成三醋酸甘油酯的反应动力学

研究了甘油和乙酸以氧化锆负载硫酸为催化剂合成三醋酸甘油酯的反应动力学,建立了酯化反应动力学方程. 考察了温度、催化剂用量、反应时间以及反应原料摩尔配比对反应速率的影响. 实验结果表明,反应时间10 h,催化剂用量为甘油的5%(w),甘油/乙酸=1:8(摩尔比)的条件下,三醋酸甘油酯的收率达93.8%. 100~130℃时,反应活化能为113.245 kJ/mol.     

盐酸甲氧那明的合成工艺研究

设计了1种合成盐酸甲氧那明的新工艺,以邻羟基苯乙酸为起始原料,经甲基化、Dakin—West反应、甲胺缩合成盐得到盐酸甲氧那明;考察了该工艺中催化剂、投料比、重结晶溶剂对反应收率和产品质量的影响。结果表明,在中间体邻甲氧基苯丙酮的制备中,邻羟基苯乙酸、硫酸二甲酯、氢氧化钠、醋酐、Ⅳ一甲基咪唑的较佳投料摩尔比为1：2．5：4．0：2．5：0．2．在邻甲氧基苯丙甲胺的制备中,邻甲氧基苯丙酮、质量分数33％的甲胺乙醇溶液、Pt／C的较佳投料质量比为1：0．6：0．01．重结晶溶剂甲苯、乙醇质量比优选为5：1,总收率为46．5％（以邻羟基苯乙酸计算）。该工艺具有37-业化前景。     

硫酸高铈催化合成乙酸正丁酯

采用硫酸高铈催化乙酸和丁醇酯化合成乙酸正丁酯。研究结果表明,硫酸高铈是该酯化反应较理想的催化剂,具有催化活性高、操作工艺简单、价格低廉和可重复使用等特点。在最佳反应条件：醇酸物质的量比为1.7∶1,催化剂用量0.6 g,反应时间50 min,酯收率达87.8%。     

乙烯基交换合成壬酸乙烯酯工艺研究

以壬酸和醋酸乙烯酯为原料,硫酸汞为催化剂,通过乙烯基交换反应制备了壬酸乙烯酯。采用气相色谱研究了原料配比、催化剂用量、反应时间对产率的影响,建立了内标法检测分析方法,并以气质联用及核磁共振对产物的结构进行了分析和表征。结果表明,当壬酸与醋酸乙烯酯物质的量比为1∶7,催化剂用量为原料总质量的1.5%,反应时间为6 h时,产物产率达92%以上。     

邻乙氧基苯甲酸合成方法的改进

采用两种新方法合成了邻乙氧基苯甲酸：以水杨酸甲酯和溴乙烷为原料在碘化钾催化下先制得邻乙氧基苯甲酸甲酯，再经水解、酸化得邻乙氧基苯甲酸；由水杨酸和硫酸二乙酯经碱性下取代、酸化制得了邻乙氧基苯甲酸。两种方法的收率分别为89．2％和92．2％。     

水杨酸甲酯的合成工艺研究

通过水杨酸和甲醇为原料,分别在浓硫酸和硫酸氢钾催化作用下合成了水杨酸甲酯。考察了酸醇摩尔比、反应时间及催化剂用量对酯收率的影响。结果表明,使用硫酸氢钾做催化剂,n(水杨酸):n(甲醇)摩尔比=1:5,反应5 h,所获得的水杨酸甲酯的收率为最好,平均收率可以到达70%。     

Effect of coupling agent on polylactic acid/polypropylene and polylactic acid/polyamide 6 foam composites

The main part of polymer materials generated from fossil fuels do not degrade after completing their usage life and then begin to be waste in the environment. This situation has led to the emphasis on environmentally friendly, biodegradable, and bio-based polymers obtained from renewable sources as an alternative. In recent years, several studies are concentrated on especially lightweight and carbon dioxide (CO₂) emission limitations. In this work, the goal was to investigate at the same time environmentally friendly and lightweight polymer foam composites based on polylactic acid (PLA) polymer without lowering the performances of the materials. In this aim, polymer foam composites containing polypropylene (PP), polyamide 6 (PA6) and PLA were produced (PLA/PA6 (30:70) and PLA/PP (30:70)) with a chemical blowing agent (CBA) introduced at 1.5 wt.% to the polymer mixture. To improve the interpolymer compatibility and foaming activity maleic anhydride-grafted polylactic acid (PLA-g-MA) was utilized as coupling agent (CA) in different ratios (1, 3 and 5 wt.%). From the evaluation of the polymer mixtures in terms of their lightness, thermal and mechanical strength, the most appropriate CA ratios were determined as 1 wt.% for foamed PLA/PP (30:70) mixtures and 3 wt.% for foamed PLA/PA6 (30:70) mixtures.     

Development of biodiesel from karanja,a tree found in rural India

Development of biodiesel from karanja tree, mainly found in rural India has been investigated. The biodiesel was developed from oil expelled from the seeds of the tree. Molecular weight of the oil was determined and found to be 892.7. Both the acid as well as alkaline esterification were subsequently performed to get the final product. NaOH was found to be a better catalyst than KOH in terms of yield. Maximum yield of 89.5% was achieved at 8:1 molar ratio for acid esterification and 9:1 molar ratio for alkaline esterification, 0.5 wt.% catalyst (NaOH/KOH) using mechanical stirrer.     

Effects of electrodeposited Co and Co–P catalysts on the hydrogen generation properties from hydrolysis of alkaline sodium borohydride solution

Co and Co–P catalysts electroplated on Cu in sulfate based solution without or with an addition of H₂PO₂⁻ ions were developed for hydrogen generation from alkaline NaBH₄ solution. The microstructures of the Co and Co–P catalysts and their hydrogen generation properties were analyzed as a function of cathodic current density and plating time during the electrodeposition. An amorphous Co–P electrodeposit with micro-cracks was formed by electroplating in the sulfate based solution containing H₂PO₂⁻ ions. It was found that the amorphous Co–P catalyst formed at 0.01 A/cm² exhibited 18 times higher catalytic activity for hydrolysis of NaBH₄ than did the polycrystalline Co catalyst. The catalytic activity of the electrodeposited Co–P catalyst for hydrolysis of NaBH₄ was found to be a function of both cathodic current density and plating time, that is, parameters determining the concentration of P in the Co–P catalyst. Especially, Co–13 at.% P catalyst electroplated on Cu in the Co–P bath at a cathodic current density of 0.01 A/cm² for 1080 s showed the best hydrogen generation rate of 954 ml/min g-catalyst in 1 wt.% NaOH + 10 wt.% NaBH₄ solution at 30 °C.