蔗糖脂肪酸酯的合成

以蔗糖和硬脂酸乙酯为原料合成蔗糖酯.讨论了原料配比、时间、皂含量、催化剂用量及配比对蔗糖酯得率的影响,得到最优条件：蔗糖/硬脂酸乙酯=1/0.8,反应5 h,加入6%的脂肪酸皂和7%的催化剂,乙醇钠/碳酸钾=1/4;反应温度130～135℃.     

无溶剂法合成蔗糖硬脂酸酯的工艺研究

以乙醇代替有毒的甲醇与硬脂酸在酸催化下进行反应制出了硬脂酸乙酯。以硬脂酸乙酯与蔗糖为原料在催化剂和乳化剂的作用下，进行酯交换反应合成出蔗糖硬脂酸酯。详细考察了该合成反应过程中乳化剂、催化剂用量，反应温度，原料配比，反应时间等因素对蔗糖硬脂酸酯产率的影响，得出了较佳合成工艺条件，即硬脂酸乙酯：蔗糖摩尔比为2．15：1，乳化剂与蔗糖质量比为0．1：1，催化剂与反应物料质量比为0．14：1，反应温度－120℃，压力－4．35kPa,反应时间－3.5h。以蔗糖计，蔗糖酯产率约75．2％。此外，还把蔗糖硬脂酸酯制成易挥发衍生物，建立了分析其组成的气相色谱方法。     

微波辐射法制备蔗糖多酯

以蔗糖和硬脂酸乙酯为原料,以活性炭附载磷钨酸为催化剂,在微波辐射下合成脂肪替代品——蔗糖多酯。考察了反应条件对酯得率的影响,优化出合成蔗糖多酯的较佳工艺条件为:糖酯比为1:13,催化剂的用量为原料的3%,辐射功率为456W,反应时间为40min,在该条件下合成蔗糖多酯产物的收率可达84.16%。该催化剂对蔗糖多酯的合成具有良好催化活性,微波辐射与传统加热方式相比,具有反应时间短、产率高等特点,微波辐射还可改善催化剂的催化性能。结果表明,采用蔗糖和硬脂酸乙酯为原料能合成蔗糖多酯,平均酯化度为6.578。     

硬脂酸蔗糖酯的合成及工艺优化

以碳酸钾为催化剂,在丙二醇溶剂中,通过硬脂酸乙酯与蔗糖反应,得到硬脂酸蔗糖酯,采用气相进行含量的分析。研究了温度、摩尔比（硬脂酸乙酯：蔗糖、蔗糖：丙二醇）、催化剂用量、反应时间等5个因素对反应的影响。选用L16（5^＋）正交实验,得到合成硬脂酸蔗糖酯的最佳条件为：蔗糖和硬脂酸乙酯摩尔比1．4：1、蔗糖和丙二醇摩尔比为1：17、温度70℃、反应时间9h、催化剂用量1．5％时,蔗糖酯的含量为93．96％。     

蔗糖硬脂酸酯的合成反应机理及动力学

在前期确立的合成反应较佳工艺条件下，研究了蔗糖与硬脂酸乙酯的反应机理，提出了蔗糖与硬脂酸乙酯反应过程的溶解－反应动力学模型，建立了该模型的动力学方程，并求取了模型参数，经检验证实，该模型可信度较高。     

马来酸酐改性蔗糖酯的制备及性能

为了克服蔗糖酯的水溶性差和有盐与酸性条件下乳化性能差的缺陷,该文采用马来酸酐对硬脂酸蔗糖酯进行改性,在硬脂酸蔗糖酯分子中引入羧基,设计合成了阴离子-非离子两性表面活性剂马来酸硬脂酸蔗糖酯(Sucrose stearate-maleate,MSS)。通过1HNMR和ESI-MS确证了产品结构。与硬脂酸蔗糖酯相比,MSS具有优良的水溶性。在酸性和有盐条件下,MSS的乳化性能较硬脂酸蔗糖酯得到了显著提高。同时发现,MSS还具有优异的硬水稳定性(5级)。     

锗钨酸催化合成硬脂酸乙酯的研究

以硬脂酸和无水乙醇为原料,锗钨酸为催化剂,催化合成硬脂酸乙酯。考察了原料醇酸比、反应时间、催化剂用量等工艺条件对酯化反应产率的影响,并用正交实验优化出较佳的合成条件：醇酸比为9∶1、催化剂与反应物质量比为1∶100、反应时间6h、在此条件下硬脂酸乙酯产率可达95%以上。     

硬脂酸乙酯的合成研究

本文以硬脂酸和无水乙醇为原料、浓流酸为催化剂,进行硬脂酸乙酯的合成研究。采用正交实验考察了醇酸的量比、反应时间及反应温度对合成硬脂酸乙酯的影响,实验结果表明:醇酸的量比为12．7、反应时间为6h及反应温度为80℃是最佳反应条件。     

蔗糖-6-乙酯的制备及提纯

以蔗糖和原乙酸三乙酯为原料,对甲苯磺酸为催化剂,酯化合成蔗糖-4,6-环酯,水解生成蔗糖-4-乙酯和蔗糖-6-乙酯,在叔丁胺作用下蔗糖-4-乙酯发生酰基迁移,转化为蔗糖-6-乙酯。考察了物料比、反应温度、催化剂和水的用量对反应的影响。研究表明适宜的条件为:6.84 g蔗糖需要10 mL原乙酸三乙酯、50 mg对甲苯磺酸,0℃反应180 min,加3 mL水裂解反应90 min,再加1 mL叔丁胺,酰基迁移反应90 min。产品经二氯甲烷析晶纯化,纯度达到96.5%。用ESI、1HNMR进行了表征。     

硬脂酸乙醇酰胺聚氧乙烯醚的合成及性能

以聚乙二醇(600)为原料,通过三步合成了硬脂酸乙醇酰胺聚氧乙烯醚。首先合成硬脂酸乙醇酰胺。然后,在碱性条件下,酰胺与环氧氯丙烷反应生成环醚。最后环醚与聚乙二醇(600)反应生成聚氧乙烯醚。正交试验确定较佳工艺条件为：环醚：聚乙二醇(mol)为1：1．2,反应时间5h,反应温度130℃产品收率达90％。通过红外光谱图确定了产品的结构并对产品的表面物性进行了分析。结果表明产品具有较好的降低水表面张力的能力．并具有良好的增稠、润湿,性能。     

Deactivation in Continuous Deoxygenation of C18-Fatty Feedstock over Pd/Sibunit

Catalytic continuous deoxygenation of stearic acid, ethyl stearate and tristearin without any solvents was investigated using Pd/Sibunit as a catalyst in a trickle bed reactor at 300 °C. The main emphasis was to investigate the effect of gas atmosphere and catalyst deactivation. In addition to liquid-phase analysis made offline by GC, also online gas-phase analysis with IR were performed. The main liquid-phase product coming from all reactants was n-heptadecane. In addition to deoxygenation, which was observed for all substrates, also C₁₈ and C₁₆ alkanes were formed from tristearin. The relative ratios between stearic acid, ethyl stearate and tristearin conversions to alkanes after 3 days time-on-stream were 2.8/2.3/1.0, respectively using 5 % H₂/Ar as a gas atmosphere, whereas rapid catalyst deactivation occurred with all substrates under H₂-lacking atmosphere. The spent catalyst’s specific surface area profile along the downward reactor was maximum in the middle of the catalyst beds with the highest pore shrinking in the beginning and at the end of the reactor catalyst segments in the case of stearic acid and tristearin deoxygenation whereas that decreased consecutively as ethyl stearate passed through the reactor.     

微波辐射催化合成硬脂酸乙酯

采用微波辐射技术,以硬脂酸和无水乙醇为原料,浓硫酸为催化剂制备了硬脂酸乙酯,通过正交设计实验优化了微波工艺条件。结果表明,微波辐射技术对硬脂酸乙酯的催化合成具有非常好的效果,优化的最佳工艺条件为,微波功率130W,辐射时间45min,酸醇摩尔比1．0：1．8,催化剂质量分数0．60％。在此条件下反应转化率达87．32％。     

直接法合成硬脂酸锌的正交试验设计及最佳工艺条件的确定

研究了硬脂酸和氧化锌在催化剂作用下直接合成硬脂酸锌的方法 ,并通过正交试验和验证实验确定了合成的最佳工艺条件 :反应时间 90min ,反应温度 135℃ ,过氧化物作催化剂 ,其用量为硬脂酸量的 3%。以此工艺生产的硬脂酸锌质量与文献值相符 ,且流程缩短 ,工艺简单 ,成本低 ,无废水     

Hydrocarbons for diesel fuel via decarboxylation of vegetable oils

Deoxygenation reaction of vegetable oils over a carbon-supported metal catalyst was studied as a suitable reaction for production of diesel-fuel-like hydrocarbons. Stearic acid, ethyl stearate, and tristearine have been used as model compounds. Catalytic treatment of all the three reactants resulted in production of n-heptadecane as the main product with high selectivity.     

Kilogram-scale ester synthesis of acyl donor and use in lipase-catalyzed interesterifications

Scaling up of Lipozyme-catalyzed ester synthesis with >99% conversion and a reflux trap to remove product water from the reaction mixture is reported. Ethyl stearate was synthesized in 2000-g batch reactions from technical stearic acid. The ethyl stearate was purified to 97% by crystallization and interesterified with sunflower seed oil by means of a lipase catalyst to investigate reaction parameters of temperature, substrate ratio, enzyme content and catalyst water activity. The endpoint of the reaction was defined as the incorporation of stearate into sunflower seed oil corresponding to the amount of stearate necessary to be incorporated into palm oil mid-fraction to produce a cocoa butter substitute. No tristearate was formed at the reaction endpoint in any of the reactions conducted. Reaction times decreased and levels of free fatty acids and diglycerides increased with increasing temperature and with increasing ratio of acyl donor to triglyceride. Increasing the enzyme content of the reaction mixture reduced reaction times but caused higher levels of free fatty acids and diglycerides. In reactions catalyzed by Lipozyme of defined water activity, the shortest reaction times were obtained at intermediate water activity, while free fatty acid and diglyceride levels increased with water activity. When the interesterification reaction was carried out in refluxing pentane with the condensed solvent dried by passage through a reflux trap, the free fatty acid and diglyceride levels were reduced to 6 and 3.3%, respectively.     

无溶剂法合成二甘醇葡萄糖苷硬脂酸酯

在无溶剂条件下 ,以硬脂酸钠作为催化剂 ,利用二甘醇葡萄糖苷与硬脂酸直接酯化合成二甘醇葡萄糖苷硬脂酸酯 ,在反应温度为 180℃ ,反应时间 10h ,催化剂用量为反应物总质量11 1%的条件下 ,硬脂酸的转化率达 95 0 %     

AlCl_3/D_(72)树脂催化合成硬脂酸甲酯的研究

由AlCl3/D72 树脂为催化剂 ,以硬脂酸与甲醇为原料催化合成硬脂酸甲酯。研究了催化剂的用量、酯化反应时间、酸醇物质的量比对酯化反应的影响。催化剂能使用多次催化效果较好。     

Weak Boundary Layers in Styrene-Butadiene Rubber

In this paper two kinds of weak boundary layers (WBL) in synthetic vulcanized styrene-butadiene rubber are described.

i) WBL produced by the presence of antiadhesion compounds of the rubber formulation (zinc stearate, microcrystalline paraffin wax). These WBL cannot be effectively removed by solvent wiping, whether followed by washing with an ethanol/water mix or not. Although this treatment allowed a significant removal of zinc stearate, the paraffin wax concentration on the surface was not greatly reduced, thus, poor adhesion of rubber was obtained. Chlorination with small amounts of ethyl acetate (EA) solutions of trichloro isocyanuric acid (0.5-5 wt% TCI/EA) and/or an extended halogenation treatment increased the adhesion strength and effectively eliminated the zinc stearate from the rubber surface. If an additional heat treatment (50°C/24h) of the chlorinated rubber was also carried out, the WBL was more effectively eliminated and the resulting adhesion was independent of the amount of chlorination agent applied to the rubber surface. Furthermore, this heat treatment favoured the elimination of WBL in the untreated rubber and also contributed to the removal of WBL produced by an excess of halogenation agent.

ii) WBL created by an excess of chlorination agent applied to the rubber surface. The excess of chlorination agent produced lack of adhesion in the rubber because there was significant damage of the rubber surface and a non-rubber surface layer was formed (mainly due to oxidized, chlorinating agent residues and cyanuric acid), which contributed to the formation of WBL. To avoid the creation of WBL, a postchlorination treatment of rubber with a solution of 25 wt% ethanol in water followed by a vacuum-drying process produced excellent results. The effectiveness of this treatment relied on combining an adequate degree of chlorination with no external surface deterioration of the rubber by the excess of chlorination agent.     

Weak Boundary Layers in Styrene-Butadiene Rubber

In this paper two kinds of weak boundary layers (WBL) in synthetic vulcanized styrene-butadiene rubber are described.

i) WBL produced by the presence of antiadhesion compounds of the rubber formulation (zinc stearate, microcrystalline paraffin wax). These WBL cannot be effectively removed by solvent wiping, whether followed by washing with an ethanol/water mix or not. Although this treatment allowed a significant removal of zinc stearate, the paraffin wax concentration on the surface was not greatly reduced, thus, poor adhesion of rubber was obtained. Chlorination with small amounts of ethyl acetate (EA) solutions of trichloro isocyanuric acid (0.5–5 wt% TCI/EA) and/or an extended halogenation treatment increased the adhesion strength and effectively eliminated the zinc stearate from the rubber surface. If an additional heat treatment (50°C/24h) of the chlorinated rubber was also carried out, the WBL was more effectively eliminated and the resulting adhesion was independent of the amount of chlorination agent applied to the rubber surface. Furthermore, this heat treatment favoured the elimination of WBL in the untreated rubber and also contributed to the removal of WBL produced by an excess of halogenation agent.

ii) WBL created by an excess of chlorination agent applied to the rubber surface. The excess of chlorination agent produced lack of adhesion in the rubber because there was significant damage of the rubber surface and a non-rubber surface layer was formed (mainly due to oxidized, chlorinating agent residues and cyanuric acid), which contributed to the formation of WBL. To avoid the creation of WBL, a postchlorination treatment of rubber with a solution of 25 wt% ethanol in water followed by a vacuum-drying process produced excellent results. The effectiveness of this treatment relied on combining an adequate degree of chlorination with no external surface deterioration of the rubber by the excess of chlorination agent.