基于废弃地沟油制备双酯基季铵盐型阳离子表面活性剂

为了减少地沟油对生物体的危害,实现地沟油的综合利用,以地沟油为原料,经过酸解制备地沟油酸。地沟油酸进而与环氧氯丙烷发生开环酯化反应获得氯化单地沟油酸酯,然后与地沟油酸在对甲苯磺酸的催化作用下发生脱水酯化反应制备氯化双地沟油酸酯,进一步与三甲胺发生季铵化反应获得一种基于地沟油的双酯基三甲基氯化铵季铵盐型阳离子表面活性剂。使用傅里叶变换红外光谱表征中间体与产物的特征基团,确定产物的分子结构,使用表面张力仪和电导率仪测试产物的临界胶束浓度。     

基于废弃地沟油制备双酯基季铵盐型阳离子表面活性剂

为了减少地沟油对生物体的危害,实现地沟油的综合利用,以地沟油为原料,经过酸解制备地沟油酸。地沟油酸进而与环氧氯丙烷发生开环酯化反应获得氯化单地沟油酸酯,然后与地沟油酸在对甲苯磺酸的催化作用下发生脱水酯化反应制备氯化双地沟油酸酯,进一步与三甲胺发生季铵化反应获得一种基于地沟油的双酯基三甲基氯化铵季铵盐型阳离子表面活性剂。使用傅里叶变换红外光谱表征中间体与产物的特征基团,确定产物的分子结构,使用表面张力仪和电导率仪测试产物的临界胶束浓度。     

基于地沟油的Gemini型阳离子表面活性剂及对纸张的柔软效果

将废弃地沟油进行酸解获得混合脂肪酸。以混合脂肪酸、二甲基乙醇胺、环氧氯丙烷等为基本原料制备了一种新型的基于地沟油的Gemini阳离子表面活性剂。使用傅里叶变换红外光谱对制备化合物的特征基团进行表征。利用表面张力法测定制备表面活性剂的临界胶束浓度为5.07×10~(-3)mol/L,利用电导率法测定临界胶束浓度为5.02×10~(-3)mol/L,此时对应的表面张力y_(cmc)为35.26 mN/m。最后,使用手感式柔软度测试仪测试制备表面活性剂对纸张的柔软效果,结果表明当表面活性剂浓度达到9.1×10-4 mol/L时,即可以取得较好的柔软效果。     

Gemini型磺基琥珀酸酯盐表面活性剂的合成与性能

采用非外加相转移催化剂的方法合成了Gemini型磺基琥珀酸酯盐表面活性剂,得到较佳工艺条件为:n(顺酐):n(乙二醇)=2.05∶1、于70℃下单酯化反应2.0h,可得到酯化率约95%的单酯化产物;n(顺酐)∶n(己醇)=1.15∶1,160℃条件下双酯化反应40min,可得到酯化率约95%的双酯化产物:n(NaHSO3):n(顺酐)=1.05∶1,反应温度110℃下反应2.5h,可得到磺化率96%的目标产物。测定了Gemini型表面活性剂的表面性能,并与十二烷基硫酸钠和十二烷基苯磺酸钠的性能进行了比较,结果显示:其临界胶束浓度为0.8mmol/L、表面张力为25.7mN/m,渗透性能、去污力较佳,是一种较为理想的表面活性剂。     

溴化1-乙氨基-3-癸基咪唑的合成研究

利用离子液体合成了C_(10)的阳离子型表面活性剂,并使用红外光谱仪对其结构进行表征,确定合成的产物为目标产物。使用表面张力仪对合成的产物进行表面性能的测定,测定结果理想。     

地沟油生产无磷洗衣粉的研究

研究对脱色后地沟油皂化产物用于生产无磷洗衣粉的工艺做了探索。以地沟油脱色后的皂化产物、对环境无害的新型无磷复配洗涤助剂和表面活性剂为原料,制成无磷洗衣粉。经正交实验优选出适用于宾馆、饭店洗涤棉织物为主的重垢型无磷洗衣粉的最佳配方。测试结果表明,优选配方的性能和市售洗衣粉的性能相当,主要技术指标符合国家标准。本研究以脱色后地沟油的皂化产物为原料,降低了产品的成本,又缓解了地沟油对环境保护带来的压力。     

表面活性剂包衣酶在有机溶剂中拆分对映异构体

天然酶经表面活性剂包衣后在有机溶剂中的活性和对映选择性有显著提高 ,稳定性也大为改善。目前研究涉及的大多为酯化或酯交换反应 ,使用最多的为脂肪酶 ,底物的分子结构对包衣酶的对映选择性有显著影响。指出可以借助膜反应器来实现包衣酶的截留和反复利用及产物的分离 ,通过改良表面活性剂或改进包衣酶的制备过程可望进一步提高包衣酶的收率和活性 ,包衣酶催化反应的机理及动力学也有待深入研究。     

一种新型双子表面活性剂的合成与性能

以丙酮为溶剂的条件下,顺丁烯二酸酐、乙二醇、己醇酯化后经磺化合成新型的gemini型磺基琥珀酸盐表面活性剂。反应的较佳工艺条件为:催化剂用量为顺酐质量的1%,n(顺酐)∶n(乙二醇)=2.05∶1,于70℃下单酯化反应2.0 h,得到酯化率约94.6%的单酯化产物;n(己醇)∶n(顺酐)=1.15∶1,160℃下双酯化反应40 min,可得到酯化率约95%的双酯化产物;n(NaHSO3)∶n(顺酐)=1.05∶1,110℃下反应2.5 h,可得到磺化率99.5%的目标产物。合成的样品显示出优良的表面活性和较好的乳化、润湿、渗透、去污等应用性能,是一种较为理想的表面活性剂。     

地沟油脱色及皂化工艺的研究进展

综述了地沟油的脱色及皂化工艺,介绍了活性炭、活性白土、吊白块及双氧水的脱色方法和反应原理,详细阐述了利用餐饮业废油脂的皂化反应产物制造羟基脂肪酸、洗衣粉、表面活性剂和肥皂等方面的应用工艺研究情况,为地沟油的回收利用指明了新的途径。     

聚乙二醇型含硼表面活性剂的合成

含硼特种表面活性剂具有碳氢表面活性剂无法替代的长处,具有广阔的应用前景。因此,合成含硼表面活性剂意义重大。本论文采用聚乙二醇、三乙醇胺、硼酸为原料,应用潜溶剂法（以甲苯为溶剂,通过回流带出酯化反应所生成的水）制备了含硼表面活性剂。设计正交实验确定最佳的酯化条件。实验结果表明,最佳的酯化条件为：温度（90±2）℃,硼酸、三乙醇胺、PEG（400）的摩尔比为2：1：2。最佳酯化条件下合成的聚乙二醇型三乙醇酰胺硼酸酯表面活性剂的电导率为0．36mS·cm^-1,表面张力为67．00mN·m^-1,pH值为8～9,水溶液为均一透明溶液。所合成的硼酸酯表面活性剂可以很好地应用于金属切削加工液中。     

环丙甲酰氯合成改进

环丙甲酰氯是一种重要的中间体。以γ-丁内酯为起始原料,通过与固体光气、异丙醇等原料反应,经过酯化、环合、水解等步骤,合成出含量大于98.5%的环丙甲酰氯。新工艺用固体光气代替传统的卤化剂,值得推广应用。     

Membrane reactors in chemical production processes and the application to the pervaporation-assisted esterification

When appropriate membrane was used for the assistance of chemical and biochemical equilibrium reactions, it is possible to enhance the yield and the purity of the reaction product by selectively adding educts or selectively removing products and to a lower the energy input and the reaction time compared to conventional process. In this paper a review on membrane reactors with special emphasis on membrane-assistance of esterification reactions and a continuous tube membrane reactor for the pervaporation-assistance of the esterification are presented. The heterogeneously catalyzed esterification of ethanol and acetic acid to ethyl acetate and water was investigated as a typical chemical equilibrium reaction. The selective and simultaneous water separation from the reaction mixture of the esterification with polyvinyl alcohol pervaporation membranes is considered to be an interesting process alternative to the conventional distillation process. Compared to the distillation process, for the pervaporation-assisted process a decrease of the energy input of over 75% and of the investment and operating coasts of over 50% each was calculated.     

单乙醇胺磷酸酯的合成

以乙醇胺、磷酸为原料,经酯化反应合成了单乙醇胺磷酸酯。研究了影响反应的因素,优化了反应条件。酯化反应的最优条件为:n(乙醇胺)∶n(磷酸)=1.0∶1.4,回流反应5 h。经减压蒸馏除去溶剂癸烷得粗产品,收率达94.0%。再用90%乙醇纯化得目标产品。回收率95.0%。对目标产品进行熔点测定、元素分析和红外光谱表征,可确认该产品为标题化合物。该产品长期依赖进口,该方法已扩大试验,有待实现工业化。     

Green approach for the preparation of biodegradable lubricant base stock from epoxidized vegetable oil

A novel process for the production of biodegradable lubricant-based stocks from epoxidized vegetable oil with a lower pour point via cationic ion-exchange resins as catalysts was developed. This involves two steps, first, ring-opening reactions by alcoholysis followed by esterification of the resultant hydroxy group in the first step.

The ring-opening reaction of epoxidized soybean oil with different alcohols such as n-butanol, iso-amyl alcohol and 2-ethylhexanol was carried out in presence of Amberlyst 15 (Dry) as a catalyst; identity of products was confirmed by IR and NMR. Pour points of the products were observed in the range of −5 to −15 °C. The hydroxy group of ring-opening product of n-butanol was further reacted with acetic anhydride in presence of catalyst Amberlyst 15 (Dry), which was previously used to carry out ring-opening reaction by alcoholysis and identity of the resulting product was confirmed by IR. Pour point of the resulting product was observed to be −5 °C.     

Thermal properties and chemical changes in blend melt spinning of cellulose acetate butyrate and a novel cationic dyeable copolyester

A novel cationic dyeable copolyester (MCDP) containing purified terephthalate acid (PTA), ethylene glycol (EG), 2‐methyl‐1,3‐propanediol (MPD), and sodium‐5‐sulfo‐isophthalate (SIP) was synthesized via direct esterification method. The chemical structure of modified cationic dyeable polyester (MCPD) was confirmed by FTIR and ¹H‐NMR. The thermal properties of MCDP and cellulose acetate butyrate (CAB) blends with different blend ratios were investigated by DSC. The results revealed that MCDP and CAB were immiscible polymer blends, and the glass transition temperature of CAB in blend fibers was higher than that of CAB in blend chips because of the strengthening hydrogen bonding. The chemical changes of MCDP and CAB in blend melt spinning were analyzed. It was found that the thermal hydrolysis reaction of ester side groups of CAB occurred in blend melt spinning, which resulted in that the acid gas was produced and the hydroxyl group content of CAB was increased. Furthermore, the moisture absorption of blend fibers was improved about three times than pure MCDP fiber even after washing 30 times. © 2010 Wiley Periodicals, Inc. J Appl Polym Sci, 2010     

Acidic activation of cellulose and its esterification by long‐chain fatty acid

Cellulose‐enriched residues from wheat bran can be transformed in bioplastics after esterification of the cellulose by lauroyl chloride. Before the esterification reaction, an activation step with a swelling of the sample in dilute acid and subsequent drying was required. This activation had a marked influence on the amount of esterified product and its degree of substitution. Using pure cellulose as well as cellulose‐enriched agricultural residues, we have shown that the cellulose was totally recovered after this pretreatment and that partial hydrolysis of cellulose chains occurred during the drying step, which probably improved the accessibility to chemical reagents. The possible role of sulfuric acid as catalyst for the esterification reaction of the cellulose by lauroyl chloride was discussed. © 1999 John Wiley & Sons, Inc. J Appl Polym Sci 74: 1933–1940, 1999     

壳聚糖的性能及在电化学生物传感器中的应用

壳聚糖又称脱乙酰甲壳素,是由自然界广泛存在的几丁质（chitin）经过脱乙酰作用得到的,化学名称为聚葡萄糖胺（1-4）-2-氨基-B-D葡萄糖,属带阳离子性质的碱性多糖。壳聚糖作为资源富足、作用普遍的高分子化合物,兼有生物相容性和可生物降解等特点,被广泛运用于医药、食品、化工、化妆品等领域。利用壳聚糖成膜性较好及其特有的表面基团,采用吸附法、共价交联法等方法,壳聚糖可以与其它活性材料形成复合膜作为固定基质修饰电极。本文介绍了壳聚糖的结构、物理化学性质、常见的制备方法,综述了基于壳聚糖的电化学生物传感器在医学领域、环境监测和食品安全中的应用.     

新型缓释氮肥草酰胺

介绍了草酰胺作为一种优质的缓释氮肥,其市场前景,合成方法以及国内外的研究进展。目前最有发展前景的合成方案是以合成气或者煤制气为原料,经过一系列的气体分离净化,再经过酯化,偶联,氨化得到草酰胺,该路线具有原料简单易得,资源利用合理,能源消耗较省,污染小,是循环经济产业同时也是C1化工的重要发展方向。     

Facile Synthesis of Dodecatungstophosphoric Acid @ TiO<Subscript>2</Subscript> Pillared Montmorillonite and Its Effectual Exploitation Towards Solvent Free Esterification of Acetic Acid with <Emphasis Type="Italic">n</Emphasis>-Butanol

Abstract  

An acid activated montmorillonite, treated with organic cationic surfactant, i.e. cetyltrimethylammonium bromide (CTAB), was used as a template to prepare TiO₂ pillared montmorillonite taking titanium ethoxide as titania precursor in hydrochloric acid environment. The pillared montmorillonite was further promoted by dodecatungstophosphoric acid impregnation. The as prepared materials were characterized by various spectroscopic and analytical characterization techniques. The catalyst was employed towards a solvent free esterification of acetic acid with n-butanol. The catalyst showed excellent results with 88% conversion and 100% butyl acetate selectivity. It can be recovered and reused readily, making product isolation and catalyst reuse simple.     

活性炭负载硅钨酸催化合成双三羟甲基丙烷丙烯酸酯

采用直接酯化法,以活性炭负载硅钨酸为催化剂合成双三羟甲基丙烷丙烯酸酯,考察了影响酯化率的主要因素。结果表明,活性炭负载硅钨酸具有良好的催化活性,当酸醇物质的量的比为4.0∶1,负载催化剂用量为反应物质量的0.6%,反应时间为4 h时,酯化率可达96.5%。产物用红外光谱定性检测。