乙二醇精制工艺的研究

通过对两种国产树脂催化剂的评价,选出一种性能良好的乙二醇(MEG)精制催化剂,并考察了MEG精制工艺条件。研究结果表明:在装有强酸性阳离子交换树脂催化剂的固定床反应器中,当反应温度为35~55℃、空速小于7.0h-1时,MEG中醛基含量小于3.010-6,达到国外同类催化剂的水平,具有良好的工业化前景。     

氢氧化钙脱除湿法磷酸中砷的研究

采用氢氧化钙作为沉淀剂,研究了搅拌速度、沉淀剂用量、反应时间、反应温度等因素对湿法磷酸中砷的脱除率及P2O5收率的影响,并通过正交实验,得出了适宜的工艺条件。在适宜的工艺条件下可得到较纯净的湿法磷酸。     

工业碳酸钠提纯过程的杂质驻留与去除研究

因原料即工业级碳酸钠来源不同,其中含有杂质类别、含量差异较大,因此,采取不同的物理、化学方法以及一定顺序流程,形成了工业级碳酸钠提纯的各种方法。以华峰副产工业碳酸钠为提纯研究对象,通过一系列物理处理方法,制备纯度较高的试剂级碳酸钠,并对所得中间产品中杂质含量进行分析,从而对工业碳酸钠提纯过程的杂质驻留与去除进行研究。实验结果表明,可溶性离子铁、Pb2+、 Ca2+、Al3+、氯化物和硫酸盐等杂质在碳酸钠晶体表面粘附引起吸藏; K+、Mg2+生成混晶引起共沉,需要经过碳酸钠晶体熔融后才能使杂质降到分析纯级;碳酸钠结晶过程中形成晶簇,包藏母液,晶间包藏磷酸及硅酸盐。     

高压法三聚氰胺产品OAT含量高的原因分析

OAT是对高压法三聚氰胺生产过程中产生的一种副产品的统称,正常生产中三聚氰胺产品中OAT含量一般在200×10-6,若含量过高会引起三聚氰胺产品浊度超标。本文简单概述了意大利欧技公司高压法三聚氰胺生产工艺基本工艺流程,详细阐述了该工艺 OAT 产生和去除的过程,对正常生产中造成高压法三聚氰胺产品 OAT 含量升高的原因进行了分析,通过分析,总结了高压法三聚氰胺生产工艺中防止产品浊度超标操作注意事项。     

Isolation of Non-methylene Interrupted or Acetylenic Fatty Acids from Seed Oils Using Semi-preparative Supercritical Chromatography

Preparative scale supercritical fluid chromatography was used for isolating and purifying uncommon non-methylene interrupted or acetylenic polyunsaturated fatty acids ethyl esters from seed oils. Fractionation of Biota orientalis seed oil ethyl esters was performed by supercritical fluid chromatography to obtain juniperonic acid [(5Z,11Z,14Z,17Z)-eicosa-5,11,14,17-tetraenoic acid], a non-methylene interrupted polyunsaturated fatty acid. Fractionation of sandalwood seed oil ethyl esters yielded ximenynic acid [(E)-octadec-11-en-9-ynoic acid], an acetylenic polyunsaturated fatty acid. The effects of CO₂ flow rate, column stationary phase and particle size were explored to optimize ximenynic and juniperonic ethyl ester recovery and purity from ethyl ester mixtures using online UV/Vis detection. Particle size, followed by the stationary phase, were found to be the most important parameters to achieving good separation. Under optimized conditions, ximenynic and juniperonic ethyl ester purities greater than 99 and 95%, respectively, were achieved in a one step process without co-solvent. The isolation and recovery of juniperonic acid from biota seed oil free fatty acids was also attempted. Using free fatty acids as the feed material, the non-methylene interrupted polyunsaturated sciadonic acid was also able to be separated from other compounds including juniperonic acid under some conditions, and gave an increase in concentration of more than 17 times.     

牛Ⅱ型链球菌van B2蛋白的原核表达及纯化

目的原核表达并纯化牛Ⅱ型链球菌(Streptococcus bovis biotypeⅡ)van B2蛋白。方法采用PCR法从牛Ⅱ型链球菌基因组DNA中扩增van B2基因,克隆至原核表达载体pET-28a(+)中,构建重组表达质粒pET-28a-van B2,转化大肠杆菌Rossata(DE3),IPTG诱导表达。表达的重组蛋白经Ni柱亲和层析纯化后,进行SDS-PAGE及Westernblot分析。结果 PCR扩增获得597 bp的van B2基因片段;重组表达质粒pET-28a-van B2经双酶切及测序证明构建正确;表达的重组van B2蛋白相对分子质量约为29 000,主要以可溶性形式表达;纯化的重组蛋白纯度为70%,可被小鼠抗牛链球菌血清Ⅱ型多克隆抗体特异性识别。结论原核表达并纯化了牛Ⅱ型链球菌van B2蛋白,为van B2基因的耐药性研究奠定了物质基础。     

人胎盘泌乳素的原核表达及纯化

目的原核表达并纯化人胎盘泌乳素(Human placenta lactogen,hPL)。方法从正常产妇新鲜胎盘组织中提取组织总RNA,PCR扩增hPL基因,将其亚克隆至pQE-30载体,构建重组表达质粒,转化感受态大肠杆菌M15(pREP4),经IPTG诱导表达。表达产物经Sephacryl S-200层析柱纯化,纯化产物经SDS-PAGE和western blot鉴定其纯度和特异性。结果重组菌pQE-hPL/M15(pREP4)经双酶切及测序证实构建正确;表达的重组蛋白相对分子质量约23 000,主要以包涵体形式表达,表达量占菌体总蛋白的67%;纯化后目的蛋白纯度可达90%以上;纯化蛋白和hPL包涵体均可与羊抗hPL多克隆抗体特异性结合,具有较强的特异性和抗原性。结论已成功制备了纯度较高的hPL蛋白,为基因工程制备抗体提供了抗原。     

赤子爱胜蚓核酸酶样蛋白的纯化及其活性

目的纯化赤子爱胜蚓核酸酶样蛋白,并鉴定其活性。方法将制备的赤子爱胜蚓核酸酶样蛋白粗提液透析后,经Bio-CAD CM柱层析系统非连续梯度洗脱,收集洗脱峰,对有活性的梯度洗脱峰样品进行单向聚丙烯酰胺凝胶电泳(1D-PAGE)及切胶纯化,将切胶回收纯化的蛋白样品进行双向聚丙烯酰胺凝胶电泳(2D-PAGE),回收蛋白,进行活性和浓度检测。结果透析后的蛋白粗提液经Bio-CAD CM柱层析分离,得到3个不同洗脱梯度的可降解DNA的活性峰,3个梯度蛋白的PAGE带型基本一致,经PAGE分离获得3个核酸酶样蛋白纯品EWD1、EWD2和EWD3,得率和纯化倍数分别为:27.9%,11.6;16.7%,11.2;16.7%,18.6。结论成功纯化了赤子爱胜蚓核酸酶样蛋白,并保持了其良好的生物活性。该纯化方法简单、快速、经济、实用,为该蛋白结构及功能的进一步研究奠定了基础。     

金黄色葡萄球菌肠毒素B的原核表达及纯化

目的原核表达并纯化金黄色葡萄球菌肠毒素B(staphylococcal entertoxin B,SEB)。方法以合成的SEB全基因序列为模板,PCR扩增SEB基因片段,插入原核表达载体pET-28a中,构建重组表达质粒pET-28a-SEB,转化E.coil BL21(DE3),IPTG诱导表达。表达的重组蛋白经硫酸铵盐析、SP阳离子层析柱、Chelating金属鳌合层析铜(Cu2+)柱纯化后,用Thrombin切除组氨酸标签,再经Chelating金属鳌合层析铜(Cu2+)柱和DEAE阴离子层析柱纯化。结果重组原核表达质粒pET-28a-SEB经双酶切及测序证明构建正确;表达的重组蛋白相对分子质量约为31 000,主要以可溶性形式表达,表达量约占菌体总蛋白的30%。最终纯化后的重组SEB蛋白纯度可达90%以上。结论成功构建了SEB基因重组原核表达质粒,在大肠杆菌中表达并纯化了重组SEB蛋白,为进一步研究其致病机理及防控方法奠定了基础。     

Removal of Arsenic(III), Chromium(III) and Iron(III) Traces from Hydrofluoric Acid Solutions by Specialty Anion Exchangers

The removal of As(III), Fe(III), and Cr(III) at trace levels from HF solutions by means of specialty ion exchange resins has been investigated. These impurities are usually found in technical‐grade HF, and they need to be removed to prepare metal‐free HF for the semiconductor industry. It was assumed that Fe(III) and As(III) species in dilute HF were present in anionic form, while Cr(III) was probably in neutral form, CrF₃. First, a selection of specialty ion exchangers was performed. Then, fixed‐bed experiments were carried out to check the ability of selected resins to reach the impurity levels required in SEMI C29 for 5 wt.% HF (5 ppb of As, and 10 ppb of Cr and Fe). The effect of the flow rate and the HF concentration on the metal removal was studied with Purolite D‐3777 and Fuji PEI‐CS‐07 resins respectively. Fuji PEI‐CS‐07 showed the best performance for Fe(III) removal, even at high HF concentration (25 wt.%). A strong decrease in the Cr(III) and As(III) removal capacity with increasing concentration of HF was observed.