二烷基乙氧基硫酸钠阴离子双子表面活性剂的合成及其表面活性

为研究阴离子双子表面活性剂结构与表面活性的关系,以不同碳链的脂肪醇、环氧氯丙烷、不同的二醇等为原料,通过三步反应合成出一种间隔基为乙氧基的阴离子双子表面活性剂二烷基硫酸钠,得到不同长度碳链和间隔基的4种双子表面活性剂,同时对部分合成条件进行了优化,确定了烷基单缩水甘油醚所用催化剂为苄基三乙基氯化铵以及烷基低聚二醇的最佳反应温度为80℃。核磁共振氢谱和傅立叶变换红外光谱证实了它们及其中间产品的结构。部分产品最小表面张力低于30 mN/m,临界胶束浓度低于0.1 mmol/L,具有良好的表面活性。实验表明,随着碳链的增长和间隔基长度的增加,其CMC降低,间隔基长度的增加使am in变大,但其γCMC变化不大。     

Low-Temperature Synthesis and Characterization of Mixed Sodium Cerium(III) Hexa-Aluminate

Two forms of sodium cerium(III) mixed hexa-aluminate were prepared at temperature as low as 1270°C, i.e., 300°C lower than those reported previously, and characterized by X-ray diffraction techniques. These compounds are formed by thermal treatment, under argon, of an amorphous organometallic precursor obtained by the "citric acid method". During the synthesis, the 3+ oxidation state of cerium is retained at all temperatures.     

槲皮素苯甲酸酯的合成与表征

以槲皮素为原料、浓硫酸作催化剂,85℃与苯甲酰氯反应,TLC板监测反应完毕,过滤、氯仿/甲醇重结晶合成标题化合物。UV表征显示,槲皮素的两个特征吸收峰均发生蓝移,这是形成新化合物共轭体系引起的。IR中ν—OH峰明显减弱,说明槲皮素的5个羟基中有的羟基发生了反应;νCO位于1 745.32 cm-1,酯羰基峰明显增强;νC—O位于1 259.66cm-1,峰变宽增强。1HNMR中3-OH、3'-OH、4'-OH上面的氢消失,说明与苯甲酰氯发生了酯化反应;同时,在δ6.7~8.4处有苯甲酰基的多重峰。MS中m/z 615.2为槲皮素三苯甲酸酯的分子离子峰。因此,槲皮素与苯甲酰氯反应可以得到标题化合物。     

Synthesis and Characterization of Novel Aryl Alkyl Sulfonates Based on Nonylphenol

A series of nonylphenol-substituted alkyl sulfonates (C _x NPAS, x = 8, 10, 12, 14, 16) with two hydrocarbon chains and two different hydrophilic groups has been synthesized from α-olefins and nonylphenol. The respective products have a “pseudo-gemini” surfactant structure. The structures of the C _x NPAS have been characterized by IR, UV, ¹H nuclear magnetic resonance, electrospray ionization mass spectrometry, and elemental analysis. The effects of carbon chain length of the obtained surfactants on properties such as the critical micelle concentrations (CMC) in aqueous solutions, surface tension at the CMC (γ _CMC), and efficiency of adsorption at the water/air interface (pC ₂₀) have been determined. The γ _CMC of the surfactants first decreased and then increased with increasing length of the carbon chain x, and reached a minimum of 29.25 mN/m at x = 10, which is much lower than that of α-olefin sulfonate (AOS) (33.52 mN/m). The CMC decreased and pC ₂₀ increased with increasing x. The introduction of the hydroxyl group is responsible for multiple molecular conformations at the water/air interface and leads to a greater molecular area A _min and smaller Γ_max than those of AOS.     

二巯基丙磺酸钠的合成和表征

以丙烯磺酸钠为原料,经溴化、巯基化、成汞盐络合物、用硫化氢对络合物脱汞四个步骤合成二巯基丙磺酸钠,并对结构进行表征。     

Synthesis and Characterization of 9(10)-Bromo-9-octadecenoic Acids

9(10)-Bromo-cis-9-octadecenoic acid, m. p. 36.7° C, was prepared by dehydrobromination of threo-9,10-dibromo-stearic acid with bases and by polar addition of hydrogen bromide to stearolic acid. The trans isomer, m. p. 6°–8° C, was obtained from the corresponding erythro-dibromide. Both compounds were characterized by IR and NMR spectroscopies and a reaction scheme for their formation by dehydrobromination is suggested.     

糖基化三氮唑香草酸白杨素酯的合成与结构表征

以叠氮糖、炔丙基溴、香草醛和白杨素为原料,通过醚化、Click chemistry氧化、酯化4步反应得到4个糖基化三氮唑香草酸白杨素酯,反应路线简单,条件温和,收率较高,总收率为51%~62%(以香草醛计),产物结构通过1H NMR、IR、ESI-MS和元素分析确认。     

Synthesis and Characterization of Two Potential Energetic Azido Esters

Two new energetic azido esters named 1,3‐bis(azidoacetoxy)‐2‐azidoacetoxymethyl‐2‐ethylpropane ( I ) and 1,3‐bis(azidoacetoxy)‐2,2‐bis(azidomethyl)propane ( II ), have been synthesized and characterized by IR, NMR and Elemental Analysis. Thermal studies revealed that azido esters I and II are stable up to 180 °C and their glass transition temperatures are −47 °C and −52 °C, respectively.     

Synthesis and Characterization of Novel Betti Type Cyanate Esters

Several aromatic diols bearing amino benzyl linkage in the main chain have been synthesized through high yield Betti reaction, which involves the reaction of an aldehyde with p-amino phenol and 8-hydroxy quinoline. Five different aldehydes have been used to prepare five new bisphenols. These bisphenols were converted to their corresponding cyanate esters by the treatment of cyanogen bromide in the presence of triethyl amine. The structures of the diols and dicyanate esters were confirmed by FT-IR, ¹H-NMR, ¹³C-NMR spectral studies and elemental analysis. The cyclotrimerization reactions of cyanate esters have been studied by differential scanning calorimetry (DSC). The maximum curing temperatures of these cyanate esters are in the range of 186-201^oC. T_gvalues of the polycyanurate networks are above 270^oC. Thermogravimetric analysis (TGA) shows that the 10% weight loss of all the cured cyanate esters is above 400^oC in N₂ atmosphere. The char yield is in the range of 66-73%. The flame retardancy of the cyanate ester resins have been studied using Limiting Oxygen Index (LOI) value which is in the range of 43.9-46.7% at 700^oC.     

壬基酚聚氧乙烯（7）醚磷酸酯的合成研究及单,双酯含量的测定

本文合成了壬基酚聚氧乙烯（７）醚磷酸酯（ＮＥＰ－７），研究了合成条件对单、双酯含量的影响，并介绍了一种测量单、双酯含量的新方法。     

芳维A酸糖酯的合成与结构表征

在碳酸钠和四丁基溴化铵催化下,将芳维A酸分别与O-乙酰基溴代葡萄糖、O-乙酰基溴代木糖、O-乙酰基溴代乳糖、O-乙酰基溴代麦芽糖作用,制得相应的芳维A酸乙酰基糖酯。并以IR、MS1、HNMR确认了4个糖酯的结构。     

一水硫酸氢钠催化合成混合二元酸二辛酯

在一水硫酸氢钠催化剂作用下,以异辛醇及生产环己酮的副产混合二元酸为原料,考察了混合二元酸二辛酯合成的工艺条件。结果表明,最佳酯化反应条件为混合二元酸粗品14.6 g,异辛醇40 mL,以15 mL二甲苯作带水剂,催化剂一水硫酸氢钠0.30 g,110～156℃回流反应1.5 h。在该优化条件下,混合二元酸的酯化率达99.64%。催化剂经重结晶后可重复使用。     

壬基酚硫代物低聚体的研制

以壬基酚为主要原料,合成壬基酚硫代物低聚体。研究了反应温度、反应时间和物料比等因素对合成反应的影响。结果表明,合成壬基酚硫代物低聚体的最佳工艺条件为:在常压下,壬基酚与一氯化硫的物料比为2/1(摩尔比),反应时间为2h,反应温度为30℃。     

Itaconic Acid Based Surfactants: I. Synthesis and Characterization of Sodium <Emphasis Type="Italic">n</Emphasis>-Octyl Sulfoitaconate Diester Anionic Surfactant

A novel itaconate-based surfactant, namely sodium n-octyl sulfoitaconate diester (SOSID), has been synthesized from itaconic acid (IA) and n-octanol by sulfonation and esterification reaction processes. The effects of reaction temperature, reaction time, molar ratios of n-octanol to IA and the catalyst dosage on the esterification were investigated. The chemical structure of the surfactants SOSID was characterized by means of LC–MS and confirmed by FT-IR and ¹H NMR spectroscopy. The surface tension γ and the critical micelle concentration (CMC) were determined as 25.02 mN/m and 4.0 × 10^?4 mol/L by using surface tensiometer at 20 °C. Further investigations showed that SOSID possess excellent wetting, emulsifying and lime soap dispersing properties.     

壬基酚聚氧乙烯醚丙基磺酸钠的表面活性及应用性能

研究了硬水和油田水中壬基酚聚氧乙烯醚丙基磺酸钠(NPSO-5)水溶液的表面活性及应用性能,并与常用表面活性剂LAS、AOS和AES进行比较;考察了添加脂肪醇对NPSO-5体系泡沫性能的影响和NPSO-5在NaOH水溶液中的润湿性能及硬水溶液中的润湿乳化性能。结果表明,水硬度从0 mmol/L增加到80 mmol/L,NPSO-5的临界胶束浓度(CMC)从2.06×10-4 mol/L降低到7.8×10-5 mol/L;NPSO-5相对于LAS和AOS具有较强的抗硬水能力,且在硬水中具有较高的起泡能力和稳泡性能,添加脂肪醇在一定程度上改变了液膜吸附层的结构,进一步提高了体系的泡沫性能;在NaOH质量分数达12%时,NPSO-5仍然具有良好的润湿性能。     

Synthesis and Characterization of Estolide Esters Containing Epoxy and Cyclic Carbonate Groups

The unsaturated sites in oleic 2‐ethylhexyl estolide esters (containing 35 % monoenic fatty acids) were converted into epoxide and five‐membered cyclic carbonate groups and the products characterized by Fourier transform infrared spectra (FTIR), ¹H, and ¹³C nuclear magnetic resonance (NMR) spectroscopies. Epoxidation of the alkene bonds was accomplished using performic acid generated in situ from formic acid and hydrogen peroxide. Greater than 90 % alkenes were converted into their corresponding epoxide groups as determined by oxirane values and the epoxide ring structure was confirmed by ¹H and ¹³C NMR. The estolide ester epoxide material was subsequently reacted with supercritical carbon dioxide in the presence of tetrabutylammonium bromide catalyst to produce the corresponding estolide ester containing the cyclic carbonate group. The signals at 1,807 cm^?1 and δ 82 ppm in the FTIR and ¹³C‐NMR spectra, respectively, confirmed the desired cyclic carbonate was produced. The carbonated estolide ester exhibited a dynamic viscosity, at 25 °C, of 172 mPa·s as compared to 155 mPa·s for the estolide ester starting material. The estolide ester structure of these new derivatives was shown to be consistent throughout their synthesis.     

丙烯酸钠-丙烯酰胺高吸水树脂的合成与性能

以过硫酸钾为引发剂、N,N-亚甲基双丙烯酰胺(NNMBA)为交联剂,采用水溶液聚合法制备聚丙烯酸钠-丙烯酰胺高吸水性树脂,研究了丙烯酸与丙烯酰胺比例、单体浓度、引发剂用量、交联剂用量以及聚合温度对树脂吸水性能的影响。制备的高吸水性树脂吸蒸馏水为593g·g-1,吸自来水为260g·g-1,吸0.9%Na Cl溶液为66.7g·g-1。     

左旋泮托拉唑钠的合成工艺研究

以2-氯甲基-3,4-二甲氧基吡啶盐酸盐与5-二氟甲氧基-2-巯基-1H-苯并咪唑为起始原料在氢氧化钠水溶液条件下缩合得到中间体5-二氟甲氧基-2-[[(3,4-二甲氧基-2-吡啶基)甲基]硫基]-1H-苯并咪唑,经过Sharpless不对称氧化得到粗品左旋泮托拉唑钠,再用丙酮重结晶,即可制得高纯度左旋泮托拉唑钠,总收率约65.5%,纯度99.90%。     

左旋泮托拉唑钠、镁的合成

探讨了左旋泮托拉唑钠、镁的合成。以麦芽酚(2-甲基-3-羟基-4-吡喃酮)为起始原料,经过甲基化、氨化、氯化、氧化、甲氧基化、重排、水解、氯化反应合成得到2-氯甲基-3,4-二甲氧基吡啶盐酸盐;以扑热息痛(对乙酰氨基酚)为原料经过醚化、硝化、还原、环合反应合成5-二氟甲氧基-2-巯基-1H-苯并咪唑;二者缩合制得5-二氟甲氧基-2-{[(3,4-二甲氧基-2-吡啶基)甲基]硫}-1H-苯并咪唑;以D-(-)-酒石酸二乙酯为手性试剂,过氧化异丙苯为氧化剂,不对称氧化制得S-(-)-5-二氟甲氧基-2-[(3,4-二甲氧基-2-吡啶基)甲基]亚硫酰基-1H-苯并咪唑;然后与氢氧化钠、氯化镁成盐制得左旋泮托拉唑钠和左旋泮托拉唑镁。通过该法得到了目标产物左旋泮托拉唑钠和左旋泮托拉唑镁,且该合成方法操作简便。