对甲苯磺酸催化合成二乙氧基甲烷

对甲苯磺酸催化合成二乙氧基甲烷;二乙氧基甲烷;对甲苯磺酸;催化合成;乙醇;甲醛     

二乙氧基甲烷的制备和应用

综述了二乙氧基甲烷的制法和用途，参考文献２５篇。     

2,2-二乙氧基乙醇的合成

以40％乙二醛水溶液为原料,经缩醛化、氯代、碱性水解,再经硼氢化钠还原生成2,2-二乙氧基乙醇,总收率36％。其结构经IR,^1H NMR和MS确证。     

糠醛水溶液的液-液萃取分离

糠醛是重要的化工溶剂和中间体,传统生产过程流程复杂[1],能耗高。近年已提出用不同溶剂萃取分离糠醛和水[2]。本文在前文基础上[3]选择醋酸丁酯为萃取剂测定糖醛-水-醋酸丁酯体系的LLE数据,由二组二元体系和三元体系液液平衡数据确定UNIQUAC模型中三对模型参数,并采用UNIQUAC模型模拟计算糖醛水溶液萃取分离结果,以便为错流和逆流萃取试验提供依据。1　实验部分糠醛水溶液和醋酸丁酯加入液液平衡釜[4],磁力搅拌器搅拌30分钟,待温度稳定后,静置40分钟,取上相和下相分析。平衡釜采用CS501型超级恒温水浴控温,平衡结果由SP-6800…     

硫酸铵-碘化钾-乙醇体系萃取分离铋

1　引言利用高聚物水溶液在无机盐存在下可以分成两相的非有机溶剂萃取分离方法已引起人们的重视[1 ,2 ] 。本文研究发现 ,在硫酸铵存在下 ,乙醇与水分相过程中 ,Ｂｉ(Ⅲ )与Ｉ- 形成的ＢｉＩ3-6 络阴离子能被乙醇相定量萃取 ,控制一定的酸度 ,可以实现Ｂｉ(Ⅲ )与Ｆｅ(Ⅲ )、Ｃｏ(Ⅱ )、Ｍｎ(Ⅱ )、Ｃｕ(Ⅱ )、Ｎｉ(Ⅱ )、Ｍｏ(Ⅵ )之间的分离。该萃取体系与传统的有机溶剂萃取分离方法相比 ,具有平衡时间短 ,相分离速度快 ,无三相乳化 ,不使用有毒害有机溶剂 ,操作简单 ,快速均相萃取 异相分离等优点 ,既能萃取离子缔合物 ,又能萃取络阴…     

乙醇水溶液析相萃取分离和富集TlCl4-

研究了乙醇-(NH4)2SO4-罗丹明B体系析相萃取和富集Tl(Ⅲ)的行为及与一些金属离子分离的条件。(NH4)2SO4能使乙醇的水溶液分成两相,在分相过程中,TlCl4-与罗丹明B(RhB)生成的[TlCl4-][RhB+]能被乙醇相完全萃取。当溶液中罗丹明B,(NH4)2SO4和乙醇分别为0.28 mg/mL,0.30 g/mL和质量分数30%时,Tl(Ⅲ)的萃取率达到97.9%以上,Co(Ⅱ),Pb(Ⅱ),Fe(Ⅲ),Mg(Ⅱ),Ru(Ⅲ),Ni(Ⅱ),Cr(Ⅲ),Ag(Ⅰ)和Cu(Ⅱ)基本不萃取,实现了Tl(Ⅲ)与上述金属离子的分离。方法已应用于合成水样中Tl(Ⅲ)的分离和测定。     

硫酸铵-碘化钾-乙醇体系萃取分离钯

传统的萃取分离法主要是采用与水互不相溶的有机溶剂作萃取溶剂,有的反应速度慢,传质速率低,分配比较小而需要在振荡器上进行较长时间振荡或多次萃取才能达到定量萃取的目的。均相萃取、异相分离萃取体系可以克服异相萃取分离技术中的一些缺点而受到重视[1,2]。本文以乙醇为萃取溶剂,均相萃取、异相分离Pd(Ⅱ)。试验表明硫酸铵存在下乙醇与水分相过程中,Pd(Ⅱ)与I-开成的PdI42-与质子化乙醇(C2H5OH2+)形成电中性的缔合物(C2H5OH2+)2·PdI42-被乙醇相萃取,能使Pd(Ⅱ)从Fe(Ⅲ)、Al(Ⅲ)、Zn(Ⅱ)、Mn(Ⅱ)、Ni(Ⅱ)、Cr(Ⅲ)、Co(Ⅱ)…     

硫酸铵-溴化钾-乙醇体系萃取分离金

研究了(NH4)2SO4存在下,KBr-乙醇体系萃取分离Au(Ⅲ）的行为。实验表明,Br^-与Au(Ⅲ）形成的AuBr4^-很容易被萃取到乙醇相中。当溶液中KBr、(NH4)2SO4和无水乙醇浓度分别为0．04g／mL、0．30g／mL、30％(V／V),pH=2—4时能使Au(Ⅲ）的萃取率达到100％,Al（Ⅲ）、Ni(Ⅱ)、Mn(Ⅱ)、Cr（Ⅲ）、Co(Ⅱ)、Fe（Ⅲ）、Zn(Ⅱ)、Cu(Ⅱ)、Mo（Ⅵ)、U(Ⅳ)基本不被萃取,实现了Au（Ⅲ）与上述离子的分离。     

硫酸铵-硫氰酸铵-乙醇体系萃取分离铂

从pH 3.0的水溶液中,在较大量的硫酸铵存在下,Pt(Ⅳ)以Pt(SCN)62-形式定量萃取入乙醇中。萃取体系中各试剂的适宜用量为硫氰酸铵溶液20 g.L-1,硫酸铵溶液300 g.L-1,乙醇0.30 mL.mL-1,按此条件可达到Pt(Ⅳ)与适量的Ni(Ⅱ),Cr(Ⅲ),Co(Ⅱ),Fe(Ⅱ),Mn(Ⅱ),Al(Ⅲ),Rh(Ⅲ)等离子分离。此方法已用于催化剂Ni-Pt/Al2O3试样分析中作为分离手段。对一件上述催化剂试样进行5次测定,测得铂的平均结果为w(Pt)0.104%,RSD为1.7%。     

硫酸铵存在下碘化钾-乙醇体系萃取分离镉

传统萃取分离法由于采用与水互不相溶的有机溶剂 ,对那些萃取反应速度慢、传质速率低、分配比小的体系需在振荡器上进行较长时间振荡或多次萃取才能达到定量萃取 .均相萃取、异相分离萃取体系由于可以克服异相萃取分离技术中一些缺点而受到重视[1,2 ].本文以乙醇为溶剂 ,均相萃取、异相分离镉 .试验表明 ,硫酸铵存在下 ,乙醇与水分相过程中 ,Ｃｄ(Ⅱ )与Ｉ- 形成的ＣｄＩ2 - 4 与质子化乙醇 (Ｃ2 Ｈ5ＯＨ 2 )形成电中性缔合物 (Ｃ2 Ｈ5ＯＨ 2 ) 2 ＣｄＩ2 - 4 被乙醇相完全萃取 .能使Ｃｄ(Ⅱ )从Ｆｅ(Ⅲ )、Ｃｏ(Ⅱ )、Ｎｉ(Ⅱ )、Ｍｎ(Ⅱ )…     

聚乙二醇双水相萃取光度法测定锌

A novel method of extraction spectrophotometric determination of Zn~(2+) in aqueous two-phase system formed by polyethylene glycol-2000,sodium sulfate and zincon has been established.Amounts of PEG solution,zincon solution,sodium sulfate added and the acidity of the system were optimized.The interference effects of various coexistent ions and the method to remove the interference were investigated.The Zn-zincon complex that had been formed in the presence of H_2BO_3-Na_2B_4O_7 buffer solution at pH 7.4 was extracted into the upper PEG-rich phase,and the absorbance of the extracted complex in the upper PEG-rich phase was measured at 630 nm.The apparent molar absorptivity was 7.3 × 10~4 L / (mol·cm).Beer's law was obeyed over the range of 0～2.0 μg / mL Zn~(2+).The analytical results obtained for Zn~(2+) in water samples were in good agreement with values measured by atomic absorption spectrometry.     

溶出温度对乙醇木质素超临界解聚特性影响研究

通过控制溶出温度(160、180和200℃),制备了三种毛竹乙醇木质素EOL(EOL-160、EOL-180和EOL-200),并采用红外光谱仪(FT-IR)、凝胶渗透色谱(GPC)和热重分析(TG)分别对乙醇木质素的官能团、分子量分布及热稳定性进行了分析;采用微型高温高压反应釜,在超临界乙醇体系,进行三种乙醇木质素的解聚实验,通过气相色谱/质谱联用仪(GC/MS)及FT-IR对解聚产物进行分析,探讨乙醇木质素特性对其超临界乙醇环境解聚产物组成的影响规律。结果表明,随着溶出温度的升高,乙醇木质素溶出率呈上升趋势。EOL-160、EOL-180和EOL-200三种乙醇木质素在超临界条件解聚液相产物主要成分分别为对乙基苯酚、2,6-二甲氧基苯酚和4-羟基-3-甲氧基-苯甲酸酯。     

Liquid-vapor equilibrium of dilute aqueous solutions of ethanol and 2-propanol

An automated vapor pressure apparatus has been used to obtain highly precise values of the total pressure and composition of aqueous solutions of ethanol and of 2-propanol in the water-rich region at 25 and 35°C. From these results, values of the partial pressures and fugacities of the components and osmotic coefficients have been inferred. Interaction virial coefficients derived from the present results are compared with interaction parameters previously reported for alcohol molecules in dilute aqueous solution. A discussion is given of the relative importance of hydrophobic effects and hydrogen-bonding in producing the unusual thermodynamic properties of aqueous alcohol solutions.     

两次双水相萃取结合高效液相色谱法选择性分离唾液蛋白质的初步研究（英文）

双水相萃取是一种新型的液-液萃取技术,具有方法简单,易操作,成本低,易放大,条件温和,可保持蛋白质活性等明显优势,特别适用于生物样品的前处理和组分分离。本文建立了15% PEG-4000/8% NaH₂PO₄双水相体系,通过两次双水相萃取结合高效液相色谱法（HPLC）分离了唾液中的多种蛋白质。经过双水相萃取,对上、下两相中的蛋白质进行色谱的梯度洗脱分析。50 min内蛋白质的色谱峰可分为10组,根据其在上、下两相的分配规律还可划分为6个组分区。结果表明,两次双水相萃取结合HPLC可以实现唾液中的蛋白质的选择性分离。该法为复杂生物样品中的蛋白质多维度、选择性分离和分析提供了新的思路。     

Downstream processing of antibodies: Single-stage versus multi-stage aqueous two-phase extraction

Single-stage and multi-stage strategies have been evaluated and compared for the purification of human antibodies using liquid–liquid extraction in aqueous two-phase systems (ATPSs) composed of polyethylene glycol 3350 (PEG 3350), dextran, and triethylene glycol diglutaric acid (TEG-COOH). The performance of single-stage extraction systems was firstly investigated by studying the effect of pH, TEG-COOH concentration and volume ratio on the partitioning of the different components of a Chinese hamster ovary (CHO) cells supernatant. It was observed that lower pH values and high TEG-COOH concentrations favoured the selective extraction of human immunoglobulin G (IgG) to the PEG-rich phase. Higher recovery yields, purities and percentage of contaminants removal were always achieved in the presence of the ligand, TEG-COOH. The extraction of IgG could be enhanced using higher volume ratios, however with a significant decrease in both purity and percentage of contaminants removal. The best single-stage extraction conditions were achieved for an ATPS containing 1.3% (w/w) TEG-COOH with a volume ratio of 2.2, which allowed the recovery of 96% of IgG in the PEG-rich phase with a final IgG concentration of 0.21 mg/mL, a protein purity of 87% and a total purity of 43%. In order to enhance simultaneously both recovery yield and purity, a four stage cross-current operation was simulated and the corresponding liquid–liquid equilibrium (LLE) data determined. A predicted optimised scheme of a counter-current multi-stage aqueous two-phase extraction was hence described. IgG can be purified in the PEG-rich top phase with a final recovery yield of 95%, a final concentration of 1.04 mg/mL and a protein purity of 93%, if a PEG/dextran ATPS containing 1.3% (w/w) TEG-COOH, 5 stages and volume ratio of 0.4 are used. Moreover, according to the LLE data of all CHO cells supernatant components, it was possible to observe that most of the cells supernatant contaminants can be removed during this extraction step leading to a final total purity of about 85%.     

Focused microwave aqueous extraction of chlorophenols from solid matrices and their analysis by chromatographic techniques

Open-vessel focused microwave (FMW) extraction with a purely aqueous carbonate solution was used for the extraction of chlorophenols from various solid matrices. After SPE on C18-bonded silica, the analytes were determined as such by LC-UV or, as their acetyl derivatives, by GC-ECD. The FMW aqueous extraction is efficient and rapid and no organic solvents are used. PCP was detected in several solid samples, with recoveries of 101-115% (RSD, 2-4%) relative to Soxhlet extraction. Similar recoveries were obtained for the other chlorophenols for spiked samples.     

Catalysis of heteropoly acidic salts for synthesis of diethylene glycol ethyl ether with diethylene glycol and ethanol

Ag₃PW₁₂O₄₀ and Ag₄SiW₁₂O₄₀ showed high activity and stability in the synthesis of diethylene glycol ethyl ether with diethylene glycol and ethanol, on which the conversion is 80.2% and 78.4%, respectively, and the selectivity of diethylene glycol ether is 75.4% and 80.6%, respectively. After the third reaction cycle, Ag₃PW₁₂O₄₀ and Ag₄SiW₁₂O₄₀) still showed higher activity and selectivity, on which the conversion is 72. 6% and 77.5% respectively. But the activity of Ag₃PMo₁₂O₄₀ is lower, the conversion is only 21.0%. IR, XRD, TG and n‐butylamine titrimetry showed that the catalysis may be connected with two kinds of acidic centers owned by heteropoly acidic salt.     

Selective separation and enrichment of proteins in aqueous two-phase extraction system

A simple aqueous two-phase extraction system(ATPS) of PEG/phosphate was proposed for selective separation and enrichment of proteins.The combination of ATPE with HPLC was applied to identify the partition of proteins in two phases.Five proteins (bovine serum albumin,Cytochrome C,lysozyme,myoglobin,and trypsin) were used as model proteins to study the effect of phosphate concentration and pH on proteins partition.The PEG/phosphate system was firstly applied to real human saliva and plasma samples,some pro...     

Integration of carboxyl modified magnetic particles and aqueous two-phase extraction for selective separation of proteins

Both of the magnetic particle adsorption and aqueous two-phase extraction (ATPE) were simple, fast and low-cost method for protein separation. Selective proteins adsorption by carboxyl modified magnetic particles was investigated according to protein isoelectric point, solution pH and ionic strength. Aqueous two-phase system of PEG/sulphate exhibited selective separation and extraction for proteins before and after magnetic adsorption. The two combination ways, magnetic adsorption followed by ATPE and ATPE followed by magnetic adsorption, for the separation of proteins mixture of lysozyme, bovine serum albumin, trypsin, cytochrome C and myloglobin were discussed and compared. The way of magnetic adsorption followed by ATPE was also applied to human serum separation.     

A hollow-fiber membrane extraction process for recovery and separation of lactic acid from aqueous solution

An energy-efficient hollow-fiber membrane extraction process was successfully developed to separate and recover lactic acid produced in fermentation. Although many fermentation processes have been developed for lactic acid production, and economical method for lactic acid recovery from the fermentation broth is still needed. Continuous extraction of lactic acid from a simulated aqueous stream was achieved by using Alamine 336 in 2-octanol contained in a hollow-fiber membrane extractor. In this process, the extractant was simultaneously regenerated by stripping with NaOH in a second membrane extractor, and the final product is a concentrated lactate salt solution. The extraction rate increased linearly with an increase in the Alamine 336 content in the solvent (from 5 to 40%). Increasing the concentration of the undissociated lactic acid in the feed solution by either increasing the lactate concentration (from 5 to 40 g/L) or decreasing the solution pH (from 5.0 to 4.0) also increased the extraction rate. Based on these observations, a reactive extraction model with a first-order reaction mechanism for both lactic acid and amine concentrations was proposed. The extraction rate also increased with an increase in the feed flow rate, but not the flow rates of solvent and the stripping solution, suggesting that the process was not limited by diffusion in the liquid films or membrane pores. A mathematical model considering both diffusion and chemical reaction in the extractor and back extractor was developed to simulate the process. The model fits the experimental data well and can be used in scale up design of the process.