一种从生产环已酮副产物废碱液中提取正丁酸等的方法

正本发明涉及一种从生产环己酮副产物废碱液中提取正丁酸、正戊酸、正己酸的方法。通过废水混合,废碱液蒸发,高浓度废碱液中和与分离,硫酸钠制备,粗正丁酸、粗正戊酸、粗正己酸制备,粗正丁酸、粗正戊酸、粗正己酸精制,尾油酯化,酯化尾油分离等步骤处理环己酮生产产生的废碱液,回收其中的有机物和硫酸钠。发明中在粗正丁酸、粗正戊酸、粗正己酸精制时加入NaOH进行皂化除去酸中的杂质提高了产品     

皂化废碱液双效蒸发设计

以10万t/a环己酮生产装置操作数据为基础,结合化工模拟软件计算,开发出高效的双效皂化废碱液蒸发工艺。与单效皂化废碱液蒸发工艺相比,采用双效蒸发工艺处理皂化废碱液,扣除初期建设投资费用,每年可节省费用855.6万元。     

皂化废碱液蒸发浓缩技术的改进

分析了环己酮生产环己烷皂化废碱液焚烧排放烟气时有臭味及蒸发器列管严重结垢的原因和机理.对皂化废碱液蒸发浓缩技术进行了改进:将外加热式管内沸腾升膜蒸发器改造为外加热式管外沸腾强制循环蒸发器,并在皂化废碱液中添加蒸发助剂.实施后明显抑制了蒸发器列管结垢趋势,焚烧炉烟气臭气消除,运行周期达到1个月以上;清洗蒸发器时,只需用稀碱液和水循环清洗,避免了频繁打开蒸发器机械清洗.     

辛醇废碱液无害化处理技术的工业化应用

简述了辛醇废碱液处理方法,介绍了辛醇废碱液作为油气化原料的工业化应用,得出辛醇废碱液可作为油气化原料进入气化炉,参与燃烧反应。辛醇废碱液作为油气化原料,不仅实现了辛醇废碱液无害化处理,还可提高合成气产品收率、减少炭黑的生成和减缓设备腐蚀,具有较好的经济效益和社会效益。     

氯乙烯合成废碱液的循环利用研究

电石乙炔法PVC生产过程中,氯乙烯碱洗塔循环碱液中氯化钠和碳酸钠含量达到一定值时,须及时将循环废碱液排至污水装置进行处理。为降低碱洗过程的运行成本及污水处理成本,减轻污水处理压力,研究开发废碱液收集、蒸发浓缩、结晶分离、过滤处理、浓碱液回用等工艺处理装置,实现废碱液的循环利用,减排增效。     

造纸废液碱回收治污系统的液-固旋流分离器

用新型中小型液—固旋流分离器，使造纸黑液中的有机物、杂质、渣等固形物同碱液分离，较干净的稀碱液进入黑液蒸发器组，蒸发浓缩后回收烧碱。造纸绿液或白液和渣进入中小型新型液—固旋流分离器，快速连续运作，除去绿泥和白泥渣后成干净的澄清液，代替大型的缓慢速度重力沉降的绿液和白液澄清器、稀白液澄清器，废液经处理后达排放水标准。     

湿式氧化处理乙烯裂解废碱液

文章研究了WAO处理乙烯裂解废碱液的方法。在2L高压釜中进行了乙烯废碱液的湿式氧化实验研究，重点考察了反应温度、停留时间对乙烯废碱液中COD、S^2-,酚的含量的影响。结果表明，湿式氧化处理乙烯裂解废碱液是可行的，处理后污水中COD、S^2-,酚的去除率分别达到40％、98％和30％，达到了排放标准。     

一种己内酰胺的制备方法

<正>申请号:201610270888.X申请日:2016-04-27申请人:中国石油化工股份有限公司;中国石油化工股份有限公司巴陵分公司本发明公开了一种己内酰胺的制备方法,该方法是将环己酮肟与发烟硫酸进行贝克曼重排反应,得到己内酰胺硫酸酯溶液;所述己内酰胺硫酸酯溶液与环己酮制备工艺副产的皂化废碱液进行中和反应,中和反应混合产物经过离心分离,得到硫酸钠晶体和粗己内酰胺水溶液;所述粗己内酰胺水溶液经过有机溶剂萃取分离,从萃取水相中回收有机酸,     

固相萃取-高效液相色谱法测定婴幼儿乳粉中维生素D_3的含量

建立一种使用高效液相色谱紫外检测器测定婴幼儿乳粉中维生素D_3含量的方法。样品经高温皂化反应后,将皂化液通过固相萃取柱,对目皂化液中的维生素D_3进行提取,提取液经浓缩后,再经过正相硅胶柱净化,氮吹复溶,通过Zorbax C18色谱柱分离,以外标法定量。维生素D_3标准溶液,在曲线范围内呈良好的线性关系,相关系数r~2均大于0.999;样品3水平加标回收率分别为97%~102%,6次重复测定RSD小于2.0%;检出限为1.0μg/100g,定量限为3.0μg/100g。     

乙烯废碱液的苛化法再生工艺研究

采用苛化法对乙烯裂解废碱液进行处理，Na2CO3的苛化转化率在80％以上(平衡反应液的苛化率在90％以上)；废碱液的反复再生和利用对碱液的吸收性能无显著影响，再生碱液可满足吸收裂解气中CO2等酸性气的要求。     

无渣皂化生产环氧丙烷新技术的开发

针对环氧丙烷生产中产生的皂化废液的回用进行了一系列实验,包括皂化废液用于氯醇化反应的小试、工业化模拟实验,用电解液作皂化剂的工业化模拟实验,皂化废液的淡化与浓缩实验,浓缩的皂化废液电解模拟实验等,提出了无渣皂化生产环氧丙烷的工业化设计方案：采用氯化钠电解液代替石灰乳液进行无渣皂化生产环氧丙烷,部分皂化废液直接返回氯醇化工序,另一部分皂化废液经过多效减压蒸发分离成浓盐水和淡水;浓盐水经重饱和后送到隔膜电解装置进行电解,产生含NaOH的电解液、Cl2和H2,Cl2返回氯醇化工序作为氯醇化反应原料;淡水返回氯醇化工序代替工业水。由此,环氧丙烷生产装置和隔膜法烧碱生产装置形成一个完整的闭路循环体系,解决了传统的氯醇法环氧丙烷生产中废渣及废水污染的问题。     

高纯度烟碱的制备

介绍了以废弃烟草为原料,经皂化、蒸馏、酸化、浓缩、碱化及有机溶剂萃取制备高纯度烟碱的新方法。确定了制备高纯度烟碱的最优工艺为:取1 000 g废弃烟草,加入3 L 0.1 mol/L的NaOH水溶液于60℃皂化4 h,蒸馏皂化液得到烟碱馏出液,酸化、浓缩、氯仿萃取,氯仿液用无水硫酸钠脱水后,减压浓缩得到高纯度烟碱,制得的烟碱纯度达到了99.23%,整个过程的收率为82.7%。     

超声辅助皂化提取黑曲霉中辅酶Q_(10)的研究

通过高效液相色谱鉴定证实黑曲霉菌体中含有辅酶Q10。采用正交实验设计法,研究了超声辅助皂化提取黑曲霉中辅酶Q10的最佳工艺条件。实验表明,焦性没食子酸添加量、皂化温度、超声时间为影响皂化提取效果的显著因子。在75%乙醇溶剂下,最佳提取工艺条件为:焦性没食子酸加入量为培养物的8%,皂化温度40℃,皂化时间45 min,醇碱浓度7.5 g NaOH/75 mL乙醇,超声功率280 W。最优条件下辅酶Q10提取率为0.421 mg/g干培养基,明显优于常规皂化提取。     

二氯丙醇的萃取分离

采用萃取法分离出氯丙烯氯醇化反应得到的溶液中的二氯丙醇,并对萃取工艺进行优化:选择磷酸三辛酯为萃取剂,萃取剂与二氯丙醇溶液的质量比为0.6∶1,萃取剂分成5份萃取5次,萃取率达到99.8%。萃取得到的油层与质量分数为10%的NaOH溶液在负压下进行皂化反应,皂化收率可以达到93%以上。萃取剂和萃余水可以循环使用。     

撞击流-旋转填料床乳状液膜法处理含酚废水的研究(Ⅱ)

研究了利用撞击流-旋转填料床乳状液膜法处理含酚废水的实验过程中几个主要参数对制乳率以及最终提取率的影响。讨论了几种膜添加剂对膜稳定性的影响以及床层填料、不同的水油比、水乳比对制乳率和提取率的影响并得出较优条件。     

动态皂化萃取法提取茄尼醇的研究

建立了以废次烟叶粗提物为原料,采用乙醇和溶剂油动态皂化方法萃取茄尼醇的工艺。讨论了影响动态皂化反应的主要因素,确定了优化的工艺参数:氢氧化钠为皂化试剂,6号溶剂油为烟叶粗提物的溶剂,体积分数为80%乙醇为氢氧化钠的溶剂,氢氧化钠与烟叶粗提物浸膏的质量比为1∶4,皂化反应时间为2.5 h。结果表明,在优化的条件下,经过动态皂化处理,茄尼醇收率119.4%,比经常规的先皂化后萃取处理收率增加9.3%;烟叶粗提物中的茄尼醇质量分数达到19.6%,比常规皂化处理增加2.94%。此外,采用动态皂化减少了工序,节省了萃取溶剂消耗量,因此该法是一种高效快速萃取茄尼醇的方法。     

用油脚脂肪酸制取粘胶短纤油剂

介绍了以油脚脂肪酸为主要原料制取粘胶短纤油剂的制备原理，实验方法和生产应用。     

Biodegradable hot melt adhesive based on partially saponified polyvinyl acetate/cellulose diacetate blend

Recycling the polymer material from the waste has a great advantage in reducing the cost of the biodegradable hot melt adhesive and solving environmental problems. Cellulose diacetate obtained from the acid hydrolysis of discarded cellulose triacetate-based cinematographic films was blended with low molecular weight partially saponified polyvinyl acetate. The degree of substitution of cellulose diacetate and the degree of saponification of partially saponified polyvinyl acetate to obtain the binary blends having excellent compatibility were determined by FTIR and DSC. TGA showed that these blends have sufficient thermal stability for hot melt adhesive applications. The viscoelastic properties of the blends were evaluated by DMA and melt viscosity. The shear strength and the biodegradability of the final hot melt adhesive were examined according to the amount of cellulose diacetate in the blends. The results indicate that adding 20% of cellulose diacetate can reduce the cost of partially saponified polyvinyl acetate -based hot melt adhesive while improving the adhesive strength.     

Extracting hydrocarbons from Huadian oil shale by sub-critical water

The possibility of extracting hydrocarbons from Huadian oil shale by sub-critical water was found in a stainless steel vessel. The effects of temperature and pressure on the extraction of hydrocarbons were studied. After extraction experiments, the residual solid, liquid and gas phase samples were collected and characterized, respectively. The extract yield could reach 7 wt.% (ad) when the extraction of oil shale was conducted at 260 °C for 2.5 h with the pressure of 15 MPa. The results of thermogravimetry (TG) showed that the weight loss of residual solid samples was much smaller than that of the original oil shale. It indicated that kerogen components had been decomposed partly by treatment with sub-critical water. Gas chromatography-mass spectrometry (GC-MS) analysis showed that there were more than 300 recognizable peaks in the extracting solution following processing at 330 °C and 18 MPa. Large amounts of high molecular weight hydrocarbons were gradually decompounded by the increase in types and levels of low molecular weight hydrocarbons, and polycyclic and heterocyclic compounds with the rising of pressure and temperature. These indicated that sub-critical water is capable of cracking kerogen into smaller hydrocarbon compounds at relatively low temperatures.     

Preparation of monodisperse poly(vinyl alcohol) microspheres by heterogeneous surface saponification and iodine complex formation

Monodisperse poly(vinyl acetate) (PVAc) microspheres with high molecular weight obtained by suspension polymerization of vinyl acetate were saponified in alkaline aqueous solution to keep their spherical structure. The saponification was restricted on the surface of the PVAc microspheres and obtained particles had skin/core structure. Various poly(vinyl alcohol) (PVA) microspheres with different diameters and degrees of saponification (DSs) were obtained. The conversion of PVAc to PVA during the heterogeneous surface saponification time were examined by nuclear magnetic resonance spectroscopy and after 72 h hydrogel type PVA microspheres completely saponified were obtained. The crystal melting temperatures of the microspheres obtained by the saponification were measured a constant value of 238°C irrespective of varying DS, and the peaks became enlarged as reaction time. Iodine complexes were formed in saponified microspheres with DS of 41% and 99% by immersing them in I₂/KI aqueous solution and decomposed by the reduction of I₂ in the complexes to 2I^? using sodium sulfite to confirm whether the skin formed through the saponification was composed of PVA with high VA content. Obviously, characteristic blue color developments owing to I₅^?‐PVA complexes were observed in both saponified regions and a red in the PVAc core. Consequently, it was concluded that the PVA skins formed by heterogeneous surface saponification had high DSs. Such complexes endowed polymeric microspheres a good radiopacity which would be useful in clinical treatment of vascular diseases and were examined by X‐ray irradiation image. © 2007 Wiley Periodicals, Inc. J Appl Polym Sci, 2008