Solubility of Dagang vacuum residue and molecular composition of the soluble fractions in different solvents

Dagang vacuum residue (DVR) was ultrasonically extracted with fifteen organic solvents, respectively, and the soluble fractions (SFs) were analyzed with GC/MS. The results show that DVR tends to dissolve in non-polar solvent and that most of GC/MS-detectable components in the SFs are saturated hydrocarbons.     

大港减压渣油超临界萃取物气质联用色谱分析

大港减压渣油被超临界萃取技术分馏成F1~F16个级分。用商品级的石蜡作为外标,用GC/MS对这些级分进行定性和定量分析,分析结果显示,用GC/MS检测的主要成分为C15到C43的直链烷烃、包含藿烷、萜烯和含氧有机化合物等,这些化合物的浓度从F1到F16明显减少。HPLC/MS将被用来分析级分中分子量大、极性大的物种的分子组成。     

从糠醛渣中提取纤维素的工艺

以甲酸和过氧化氢作溶剂,采用Milox三段法提取糠醛渣中的纤维素,将蒸煮与碱性过氧化氢漂白过程相结合,实现了木质素和纤维素分离的无氯漂白工艺,考察了甲酸用量、过氧化氢用量、提取温度和提取时间对糠醛渣中纤维素提取效果的影响。实验结果表明：当甲酸用量为80 mL,过氧化氢用量为14 mL,三段反应温度和时间分别为80 ℃反应2.5 h、95 ℃反应2.5h以及抽滤后加入新鲜溶剂在80 ℃再反应2.5 h,糠醛渣纤维素的得率是41.92%,纤维素的含量为85.09%,木质素含量为3.22%。由此可见该工艺优于其它工艺结果,能够更好地提高糠醛渣的应用价值。     

减压渣油超临界流体萃取馏分在多孔有机膜中的扩散规律

利用超临界流体萃取分馏技术将大港减渣分离成16个窄馏分和1个萃余残渣,选择第3#、6#、9#、12#、15#窄馏分和残渣作为研究对象,运用隔膜池分别测定了308 K下各个油样通过额定孔径为15、50、80和1000 nm 4种聚碳酸酯膜有效扩散系数和平均有效扩散系数。结果显示,大港减渣窄馏分及萃余残渣在膜孔中的有效扩散系数随着实验的进行逐渐降低,表明它们是由一定尺寸分布的组分构成的复杂混合物。随着馏分变重和膜孔直径的降低,各馏分的有效扩散系数均逐渐降低。受阻扩散因子的计算结果表明窄馏分和萃余残渣在15、50和80 nm 3种膜片中的扩散均受到不同程度的阻碍。窄馏分在50和80 nm膜孔中的受阻程度较小,而在15 nm膜孔中的受阻程度相对较大。萃余残渣在这3种膜孔中均存在较为明显的扩散阻力,在15 nm膜孔中的受阻程度尤其严重。受阻扩散因子关联结果表明,在重油分子尺寸和孔径比值相同的条件下,窄馏分和萃余残渣的扩散受阻程度并不相同,分析认为这可能是两者分子构型的差异造成的。     

微波提取苹果渣中总黄酮的工艺研究

采用微波辐射技术,以乙醇提取苹果渣中黄酮类化合物。考察了乙醇浓度、微波功率、处理时间、料液比和浸泡时间对总黄酮提取率的影响。结果表明,最佳工艺条件为:70%乙醇,微波萃取2 min,微波功率为350 W,料液比1∶30(g/mL),总黄酮1次提取率0.683 7%。     

甲壳素制备壳聚糖脱乙酰度可控性的研究

介绍了甲壳素（ehintin）和壳聚糖（ehitosan）的性质、用途及发展前景;分析了国内外对壳聚糖的研究状况及取得的成果;描述了制备壳聚糖的实验原理;初步研究了在保证能获得大分子量的情况下提高壳聚糖的脱乙酰度的实验方法;介绍了测定壳聚糖脱乙酰基的实验方法;分析了影响壳聚糖脱乙酰度（Degree　of　 Deacetylation缩写：D．D．）的主要因素。     

Determination of the heat change in solvent extraction of metals. The extraction of zinc (II) from hydrochloric acid solutions by high molecular weight amines in various organic solvents

The heat change associated with the uptake of zinc (II) has been examined by using a twin type isoperibol calorimeter in the extraction of zinc (II) from hydrochloric acid solutions by trioctylamine hydrochloride (TOAHCl) and trioctylmethyl-ammonium chloride (TOMAC) in various organic solvents such as benzene, chlorobenzene, o-dichlorobenzene, toluene, m-xylene, nitrobenzene, carbon tetrachloride and 1, 2-dichloroethane. It was found that the dependence of apparent molar heat change (the value of the heat change detected with regard to the concentration of zinc (II) reacted) on the aqueous chloride concentration could be attributed to the change in the distribution of zinc (II) chloride species in the aqueous phase. Taking account of this fact, variable Y, which constitutes the sum of the change in enthalpies for the relevant steps in the extraction of zinc (II), except the transformation of ZnCl_j^(2-j)+ to ZnCl₄^2-, in the aqueous phase, is introduced. From the values of Y obtained, it is concluded that in the extraction by TOMAC, Y correlates with the solubility parameter of diluent, suggesting that the organic phases may be regarded as regular solutions, while in the extraction by TOAHCl, no clear-cut relation holds between Y and the physico-chemical constants of the diluent such as dipole moment, dielectric constant and solubility parameters.     

从含铜废渣废液中提取硫酸铜的方法研究

研究从含铜废渣、废液中提取硫酸铜的方法,以减少污染、回收资源。利用含铜废渣、废液生产海绵铜,再通过置换、氧化、酸化、结晶以及重结晶等步骤制备五水硫酸铜晶体。通过上述方法由含铜废渣、废液制备出硫酸铜晶体。该方法所用设备简单,操作简便,铜的回收率高,硫酸铜产品质量达到化学纯（CP）等级。     

碱法回收湿法磷酸萃余渣中五氧化二磷的研究

磷酸是一种重要的化工原料。目前,生产磷酸及磷酸盐的方法主要采用湿法,但湿法磷酸中含有大量的杂质,在利用溶剂萃取法净化湿法磷酸的过程中,大量金属离子杂质以不溶性磷酸盐的形式沉淀出来,其中不溶性五氧化二磷的回收利用问题受到广泛关注。采用碱解工艺设计单因素实验,考察了液固比、n（Na₂O）/n（P₂O₅）、反应温度、反应时间对氢氧化钠分解湿法磷酸萃余渣（难溶性金属磷酸盐）效果的影响,并选出适宜的反应条件范围,在此基础上通过二次回归正交实验得到最佳的反应条件。结果表明,最佳反应条件为：液固比为30 mL/g、n（Na₂O）/n（P₂O₅）为3.31、反应温度为82 ℃、反应时间为4.05 h。在最佳的工艺条件下,五氧化二磷的回收率可达到92.48%,反应碱液可进一步作为生产磷酸三钠的原料而加以利用。该研究得到了一种利用湿法磷酸萃余渣的合理方案,并给出了相关参数,为该方案的实际应用提供指导,对萃余渣的利用和环境保护具有重要意义。     

二甲基亚砜工业废盐中亚硝酸钠的脱除研究

利用二甲基硫醚氧化法制备二甲基亚砜的企业在生产过程中会副产一定量的工业废盐,其主要成分为硝酸钠并含有较大量的亚硝酸钠,需要脱除其中含有的亚硝酸钠使其达到国家排放标准要求。研究了二甲基亚砜工业废盐中亚硝酸钠的氧化脱除工艺,分别采用热空气、双氧水、臭氧3种不同的氧化剂,对废盐中亚硝酸钠的氧化脱除效果进行了研究,并比较了其处理成本。研究结果表明臭氧对亚硝酸钠的脱除效果最好,可将废盐中亚硝酸钠质量分数由2.48%降至0.000 14%,脱除率近100%,其处理成本低,约60元/t。     

Simple separation method of Zn(Ⅱ) and Cd(Ⅱ) from brine solution of zinc plant residue and synthetic chloride media using solvent extraction

In this work, the possibility of separation of Zn~(2+) and Cd~(2+) metal ions from chloride(brine) solutions was examined. For this purpose, simple solvent extraction(SX) experiments by di-2-ethylhexyl phosphoric acid(D2EHPA)in kerosene as a diluent was performed on synthetic and industrial chloride solution obtained from brine leaching of zinc filter cakes(by-product of zinc hydrometallurgical processing). The optimal conditions for separation were determined. The zinc extraction efficiency was 99% with negligible co-extraction of cadmium.Therefore, a high ΔpH_(0.5) value for Zn(Ⅱ) and Cd(Ⅱ) was achieved. FT-IR and slope analysis indicated that ZnClA·3HA and CdClA·3HA species were probably extracted.     

Characterization of liquid products from the co-cracking of ternary and quaternary mixture of petroleum vacuum residue, polypropylene, Samla coal and Calotropis Procera

The co-cracking of the petroleum vacuum residue (XVR) with polypropylene (PP), Samla coal (SC) and Calotropis procera (CL) has been carried out in a batch reactor under isothermal conditions at atmospheric pressure. The liquids obtained by co-cracking have been characterized by Fourier transform infrared spectroscopy, high performance liquid chromatography, ¹H nuclear magnetic resonance (NMR), ¹³C NMR, gel permeation chromatography (GPC), and inductively coupled argon plasma analyses. It was found that the liquid products obtained from the co-cracking of ternary and quaternary mixtures of the petroleum vacuum residue with polypropylene, coal and C. procera contained less than 1 ppm of Ni and V. The HPLC analyses indicates that the liquids obtained from the cracking of ternary mixture of XVR+PP+CL were mainly aliphatic in nature (saturates content 87.4%). NMR analyses showed that the aromatic carbon contents decreased (15.0%) in the liquid products derived from the co-cracking of quaternary mixtures of XVR+PP+SC+CL compared to their theoretical averages (taking the averages of aromatic carbon contents of the liquids from XVR, PP, SC and CL individually). The overall results indicated that there exists a definite interaction of reactive species when XVR, PP, SC and CL were co-cracked together.     

固态发酵植物药提取残渣生产饲料蛋白工艺条件

以某制药厂双黄连制剂生产过程中产生的废弃药渣作为研究对象,在对药渣成份进行了全分析的基础上,利用正交实验法研究了混菌固态发酵植物药提取残渣生产饲料蛋白工艺参数的不同,对发酵产物蛋白含量的影响。结果表明:以40g药渣,35g玉米浆,8g玉米面,15g麸皮,2g尿素组成固态发酵培养基,产朊假丝酵母与扣囊拟内孢霉的菌种配比为2∶1时,最佳发酵条件为:发酵温度30℃,接种量15%,含水量65%,培养时间60h。在最佳发酵条件下,发酵产物的粗蛋白含量可达29.98%。以废弃药渣为主要原料发酵生产蛋白饲料是切实可行的。     

Transformer oils prepared from the vacuum distillates of Egyptian crude paraffinic petroleum

Vacuum gas oil and spindle oil obtained from the vacuum distillation of paraffinic crude oil from the Western Desert region of Egypt were utilized for transformer oils production. The vacuum gas oil, spindle oil and blends therefrom containing different percentages of these oils and were subjected to aromatic extraction, dewaxing catalytic hydrogenation processes. The aromatic extraction process used N-methyl-2-pyrrolidone as solvent, for a feed ratio of 0.7:1 (wt/wt) at an extraction temperature of 55 °C, while in the dewaxing process the wax is removed by chilling the raffinate at − 42 °C using MEK-toluene (60:40,vol/vol). The hydrofinishing process was achieved in a pilot plant using NiO–MoO₃/Al₂O₃ catalyst. These refining processes improved the viscosity indices and the pour points of the resulting oils and removed most of the polar impurities. It was found that, the transformer oil formulated from 7:3 b.w. vacuum gas oil:spindle oil respectively meets the IEC 60296-2003 standard specifications requirements. Its sulfur content is very low and non-corrosive. The gassing tendency is also low due to its low aromatic content. Further, the electrical properties which are significant for transformer oils fulfill the standard specifications as a result of the low water content and polar contaminants. Moreover, addition of 2,4-dimethyl-6-tertiary butyl phenol increases the oxidation stability of the produced oil, by acting as a free radical inhibitor.     

新型溢流器高效回收钛白酸解尾渣中的钛

中国是世界上最大的硫酸法钛白生产国,目前已累计堆积超过千万吨副产品酸解尾渣。酸解尾渣中含有大量未反应的粒径大于25 μm的钛铁精矿,酸解尾渣堆积而不利用就造成了严重的环境污染和资源浪费。根据酸解尾渣颗粒沉降实验分析,发现酸解尾渣料浆具有良好的沉降和易分层特性。通过建立干扰沉降末速度计算式,得出酸解尾渣中颗粒切割粒度25 μm的沉降速度为0.60 mm·s^-1。基于流动、分选机理和沉降特性分析,设计了适用于酸解尾渣分离工艺的新型DTB（draft tube babbled）溢流分离器,并进行了结构参数优化,获得了溢流器最优结构参数和最佳分离效果。结果表明,外排溢流含有极少量大于25 μm的钛铁精矿颗粒,回收的钛品位达27%,回收率为73%。这些结果为大规模回收酸解尾渣中钛资源提供了基础数据。     

Characterization of eluted metal components from coal during pretreatment and solvent extraction

Eluted metals from Enshu (a Chinese) and Stratford (an Australian) coal during pretreatments with methanol/water and dilute acetic acid solutions were characterized and quantitatively analyzed by solid-state ²³Na NMR, cation chromatography, X-ray fluorescence (XRF), and Inductively Coupled Plasma Atomic Emission Spectroscopy (ICP-AES) measurements. To achieve the requirements of solvent extracted coal (namely Hyper-Coal: HPC) for its direct utilization to gas turbine system, alkali and alkali-earth metals such as Na, K, and Ca should be removed from coals. A quantitative analytical method of alkali metals with ICP-AES in combination with flow injection system is established for the evaluation of remaining alkali metal contents, especially for the quantitative analysis of Na concentration in the original coal and its HPC. Microwave irradiation acidic digestion pretreatment under controlled high pressure and temperature is very essential to the prompt and quantitative analyses of all the metals in coals and their derived HPC. Combination of ICP-AES with XRF and/or cation chromatography is also effective for the respective analyses of the residue and the extract or filtrate. Solid-state ²³Na NMR spectra of the coals before and after solvent soaking pretreatment or acetic acid treatment revealed that ion-exchangeable Na species might be rather selectively eluted by these treatments. It is also suggested that the remaining Na species could not be removed by dilute acetic acid solutions.     

植物药提取废渣中再次提取有效成分的研究

利用微波萃取技术针对某中药厂双黄连制剂生产过程中产生的废弃黄芩提取药渣进行了有效成分的再次提取并同传统水提工艺进行了对比。以有效成分(黄芩苷)收率做为考察指标,用正交设计结合单因素分析方法考察微波提取黄芩苷的最佳提取条件,旨在探讨植物药提取废渣的再利用价值、探寻植物药提取废渣资源化的有效途径。结果表明:各因素对黄芩苷收率的影响依次为:乙醇浓度粒径功率提取时间,其中乙醇浓度为显著性影响因素,最佳工艺为:以30%乙醇作为提取溶剂,黄芩药渣粒径80目,微波功率选择500W,微波提取2min。与水提工艺相比,在最佳工艺条件下,微波提取工艺能够获得较高收率的黄芩苷。     

High performance cellulose fibers regenerated from 1-butyl-3-methylimidazolium chloride solution: Effects of viscosity and molecular weight

In the present study, we focused on several factors affecting the utility of 1-butyl-3-methylimidazolium chloride (BMIMCl) for obtaining higher performance fibers. The dependence of the spinnability and tensile strength of the fibers on the zero-shear viscosity of the spinning solutions was investigated based on differences in the molecular weight of the cellulose, pulp concentration, and the pH of BMIMCl. We demonstrated an appropriate viscosity range of 2000–4000 Pa s⁻¹ (100 °C) for spinning dopes to obtain good spinnability and high tensile strength. The pH of the BMIMCl and the molecular weight of the cellulose clearly impacted tensile strength. The high molecular weight of cellulose contributed to high mechanical properties of the regenerated cellulose fibers. Optimizing the molecular weight and concentration of the cellulose based on the appropriate viscosity allowed us to prepare high performance cellulose fibers with a tensile strength of 1.15 GPa and a Young's modulus of 42.9 GPa. © 2019 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2019 , 137, 48681.