Leaching behavior of heavy metals with hydrochloric acid fromfly ash generated in municipal waste incineration plants

The extraction behavior of heavy metals from municipal waste incineration （MWI） fly ash was investigated systematically. The extraction process includes two steps, namely, fly ash was firstly washed with water, and then subjected to hydrochloric acid leaching. The main parameters for water washing process were tested, and under the optimal conditions, about 86% Na, 70% K and 12% Ca were removed from fly ash, respectively. Hydrochloric acid was used for the extraction of valuable elements from the water-washed fly ash, and the optimal extraction was achieved for each heavy metal as follows： 86% for Pb, 98% for Zn, 82% for Fe, 96% for Cd, 62% for Cu, 80% for Al, respectively. And the main compositions of the finally obtained solid residue are Ca2PbO4, CaSi2Os, PbsSiO7, Ca3A12Si3012 and SiO2.

Recovery of waste rare earth fluorescent powders by two steps acid leaching

The effects of the acid leaching and alkali fusion on the leaching efficiency of Y,Eu,Ce,and Tb from the waste rare earth fluorescent powders were investigated in this paper.The results show that hydrochloric acid is better than sulfuric acid in the first acid leaching,and NaOH is better than Na2CO3in the alkali fusion.In the first acid leaching,the Wloss is 20.94%when the waste rare earth fluorescent powders are acid leached in H?concentration 3 mol L-1and S/L ratio 1:3 for 4 h due to red powders dissolved.The better results of the alkali fusion can be got at 800℃ for 2 h when the NaOH is used.The blue powders and the green powders can be dissolved into NaAlO2and oxides such as rare earth oxide(REO).The REO can be dissolved in H?concentration 5 mol L-1,S/L1:10 for 3 h in the second acid leaching.The leaching rates of the Y,Eu,Ce,and Tb are 99.06%,97.38%,98.22%,and 98.15%,respectively.The leaching rate of the total rare earth is 98.60%.

Recycling of waste carbon residue from spent lithium-ion batteries via constant-pressure acid leaching

Waste carbon residue(WCR)was efficiently detoxicated and regenerated to high-purity graphite(PGC)used in lithium-ion batteries through the constant-pressure acid leaching technique.The leaching conditions were optimized by the combination of orthogonal and single-factor experiments.Results show that PGC with 99.5%purity is regenerated at temperature of 60℃,initial acid concentration of 12%,leaching time of 180 min,and liquid-to-solid ratio of 25:1,satisfying the requirements of commercial graphite.Meanwhile,the sodium hydroxide precipitation process was designed to recover valuable components from leachate efficiently.Ni,Co,Mn,and Al recoveries reach 96.92%,87.5%,97.83%,and 92.17%,respectively,at pH=11.Moreover,the co-product NaF can be recovered with purity over 99%via evaporative crystallization.The loss rate of fluorine is less than 0.5%,thereby eliminating the pollution risk of fluorine to the environment.The proposed process shows considerable environmental and economic benefits.

Factors Research on the Influence of Leaching Rate of Nickel and Cobalt from Waste Superalloys with Sulfuric Acid

Unlike the reported leaching technologies of waste superalloys, the process of the “atomized spray-sulfuric acid leaching nickel and cobalt” technology was put forward in the present work according to the compositions of waste superalloys. The effects of sulfuric acid temperature, concentration, leaching time, stirring speed and size of superalloys on leaching of Ni and Co from waste superalloys have been mainly investigated, and the optimum leaching conditions were determined and reported. The leaching rates for nickel and cobalt were 96.68% and 96.63%, respectively, and the contents of nickel and cobalt in leaching slag were 6.77% and 0.96%, respectively. The obtained leaching solution containing Ni and Co could be used for production of Ni and Co products after removal.

Recovery of vanadium and tungsten from waste selective catalytic reduction catalysts by K_(2)CO_(3) roasting and water leaching followed by CaCl_(2) precipitation

Waste selective catalytic reduction(SCR)catalysts are potential environmental hazards.In this study,the recovery of vanadium and tungsten from waste SCR catalysts by K_(2)CO_(3)roasting and water leaching was investigated.The roasting and leaching conditions were optimized:the leaching efficiencies of vanadium and tungsten were 91.19%and 85.36%,respectively,when 18 equivalents of K_(2)CO_(3)were added to perform the roasting at 900℃ for 2 h,followed by leaching at 90°C for 1 h.Notably,in the described conditions,the leaching rate of silicon was only 28.55%.Titanates,including K_(2)Ti_(6)O_(13)and KTi8017,were also produced.Si removal was achieved in 85%efficiency adjusting the pH to 9.5,and the Si impurity thus isolated was composed of amorphous Si.Tungsten and vanadium were precipitated using CaCl_(2).At pH 10 and following the addition of 0.10 mol of H_(2)O_(2)and 16 equivalents of CaCl_(2),the precipitating efficiencies of tungsten and vanadium were 96.89%and 99.65%,respectively.The overall yield of tungsten and vanadium was 82.71%and 90.87%,respectively.

Novel efficient procedure for biodiesel synthesis from waste oils with high acid value using 1-sulfobutyl-3-methylimidazolium hydrosulfate ionic liquid as the catalyst

Preparation of biodiesel from waste oils containing 72% of free fatty acids catalyzed by a novel Br?nsted acidic ionic liquid 1-sulfobutyl-3-methylimidazolium hydrosulfate([BHSO_3MIM][HSO_4]) was systematically investigated.The optimum molar ratio of methanol to waste oils,catalyst amount,reaction temperature and reaction time were 8/1,10%(based on the mass of waste oils),140°C and 6 h,respectively,under which the obtained yield of biodiesel reached 94.9%.Also,[BHSO_3MIM][HSO_4] as a catalyst still retained around 97% of its original catalytic activity after successive re-use of 5 batches(6 h per batch),showing the excellent operational stability.Moreover,the acidic IL [BHSO_3MIM][HSO_4] was able to ef ficiently catalyze conversions of waste oils with different amounts of FFAs(free fatty acids) into biodiesel,and showed tremendous application potential.Therefore,an ef ficient and environmentally friendly catalyst is provided for the synthesis of biodiesel from waste oils with high acid value.

Recycling of Electronic Waste, Using Basic and Acid Leaching

This recycling of printed circuit board (TCI) for the production of metals, given the environmental degradation that can cause toxic substances of these, is the reuse of valuable materials recovered from the TCI, this being an economic engine that promotes the recycling of this waste. This paper presents a methodology for evaluating the reaction kinetics and leaching of metals that form the metal substrate, which have environmental and energy advantages, so the generation of new recovery techniques metals from the TCI low environmental and energy impact is increasingly necessary, for it is essential to establish the parameters affecting the reaction rate and identify design alternatives to determine whether or not sustainable, economically viable and that does not pollute. The method adopted was a leaching acid samples, where the full factorial method employed two experimental levels to evaluate the influence of: leaching time, temperature of the aqueous leach solution, reaction kinetics and solid/liquid, on the percentage of metal extraction. Subsequently, the metals are obtained by calcining and smelting the resulting salts by addition of acid liquor.

A low-cost green approach for synthesis of lead oxide from waste lead ash for use in new lead-acid batteries

This paper proposes a novel method relating to the recycling of waste lead ash originated from procedure of lead alloy production.The spent lead ash was first disposed by acetic acid leaching system,where lead ash structure wrapping impurities would be destroyed.The synthesis of lead oxide products was conducted at a lower temperature of 90℃.The effect of molar ratio of CH3 COOH to lead content of the ash on leaching efficiency was studied through the acetic acid leaching system.The results demonstrate that 84.6%of lead could be obtained in the leaching solution,while merely 0.7%of Fe blend in solution within a leaching time of 120 min.In the stage of lead oxide synthesis from leaching solution,the yield of lead oxide products could reach up to 94.4%when the molar ratio of NaOH to lead in filtrate was 2.5.This novel green method could shed light on the reuse of lead from exhausted ash with a much more convenient and environmentally friendly procedure.

Kinetics of nickel leaching from roasting-dissolving residue of spent catalyst with sulfuric acid

Sulfuric acid leaching process was applied to extract nickel from roasting-dissolving residue of a spent catalyst, the effect of different parameters on nickel extraction was investigated by leaching experiments, and the leaching kinetics of nickel was analyzed. The experimental results indicate that the effects of particle size and sulfuric acid concentration on the nickel extraction are remarkable; the effect of reaction temperature is mild; while the effect of stirring speed in the range of 400-1 200 r/min is negligible. Decreasing particle size or increasing sulfuric acid concentration and reaction temperature, the nickel extraction efficiency is improved. 93.5% of nickel in residue is extracted under suitable leaching conditions, including particle size （0.074-0.100） mm, sulfuric acid concentration 30% （mass fraction）, temperature 80 ~C, reaction time 180 min, mass ratio of liquid to solid 10 and stirring speed 800 r/min. The leaching kinetics analyses shows that the reaction rate of leaching process is controlled by diffusion through the product layer, and the calculated activation energy of 15.8 kJ/mol is characteristic for a diffusion controlled process.

Research on Catalytic Cracking Performance Improvement of Waste FCC Catalyst by Magnesium Modification

In this study,the deactivation mechanism caused by high accessibility of strong acid sites for the waste FCC catalyst was proposed and verified for the first time.Based on the proposed deactivation mechanism,magnesium modification through magnesium chloride impregnation was employed for the regeneration of waste FCC catalyst.The regenerated waste FCC catalyst was characterized,with its heavy oil catalytic cracking performance tested.The characterization results indicated that,in comparison with the unmodified waste FCC catalyst,the acid sites strength of the regenerated waste FCC catalyst was weakened,with no prominent alterations of the total acid sites quantity and textural properties.The heavy oil catalytic cracking results suggested that the catalytic cracking performance of the regenerated waste FCC catalyst was greatly improved due to the suitable surface acidity of the sample.In contrast with the unmodified waste FCC catalyst,the gasoline yield over the regenerated waste FCC catalyst significantly increased by 3.04 percentage points,meanwhile the yield of dry gas,LPG,coke and bottoms obviously decreased by 0.36,0.81,1.28 and 0.87 percentage points,respectively,making the regenerated waste FCC catalyst serve as a partial substitute for the fresh FCC catalyst.Finally,the acid property change mechanism was discussed.

Study on the Leaching of Pt, Pd and Rh from Spent Auto-catalysts in Various Acidities

Auto-catalysts were the largest consumers of platinum group metals and the most important secondary resources, recovery of PGMs from spent auto-catalysts by leaching with various acidities were investigated. The leaching thermodynamics of PGMs at 363 K was first discussed. At 363 K the higher the acidities of HCl, the higher the leaching recoveries of PGMs, and the sequence of leaching recovery was Pd>Pt>Rh. When H2SO4 used alone, the leaching recoveries of PGMs was low, when the acidity of H2SO4 increasing, the leaching recovery of Rh kept stable.

Cobalt Recovery from Waste Catalysts (Petroleum Refining Industry from Gujarat)

A hydrometallurgical process has been developed for cobalt recovery from a waste catalyst (petroleum refining industry). This waste catalyst containing about 2.18 weight % of Co, is highly contaminated by Mg, Al, Si, Ca, Fe, Ni, Cu, Zn, Mo. The major steps are: (I) The spent catalyst is roasted with flux material in an electrical furnace at very high temperature (700?C) for a specific duration. (II) The roasted sample is leached with sulphuric acid to bring the metal contents into solution form. (III) For separating cobalt values from the leach solution, the solution pH is raised by NaOH addition, where all cobalt content is precipitated at a pH of about 12. (IV) This cobalt hydroxide precipitate is filtered and dissolved in minimum amount of sulphuric acid to get cobalt sulphate solution which is used as the electrolyte for the electrolytic recovery of cobalt. For optimizing various parameters like (1) H2SO4 concentration;(2) Duration;(3) Cobalt concentration;(4) Current density;(5) Temperature;(6) Stirring etc., The particle surface morphology and deposited layers have been characterized by scanning electron microscopy (SEM). A compact metallic deposit containing 70% cobalt was obtained.

Pressure acid leaching of black shale for extraction of vanadium

Extraction of vanadium from black shale was attempted in pressure acid leaching.The chemical components of the sample obtained from Guizhou Province of China show that it contains 3.258%V2O5,52.880%SiO2 and 16.140%Al2O3.Phase analyses of vanadium indicates vanadium mainly exists in the free oxide and mica.Vanadium contents in the two phases are 18%and 53%, respectively.The contents of V3 +,V 4+and V 5+are almost equal.Under the optimum parameters of one-step leaching(reaction time of 3 h,sulfuric addition of 25%,temperature of 150℃,liquid to solid ratio of 1.2 mL/g,catalyst(FeSO4)addition of 5%and size of 85%particle 0.074 mm),about 77%of vanadium is recovered.After two-step countercurrent leaching,the leach recovery of vanadium can reach above 90%.Air replacing oxygen is completely feasible.The impurity metals can dissolve into solution in different degrees.

Biodiesel Production from Waste Cooking Oil over Mesoporous SO42-/Zr-SBA-15

Biodiesel production from waste cooking oils over SO42-/Zr-SBA-15 catalyst was successfully carried out and investigated. SO42-/Zr-SBA-15 catalyst was prepared by one-step process using anhydrous zirconium nitrate as zirconium resource, and endowed with the strong Lewis acid sites formed by supporting the zirconium species onto the SBA-15 surface. The asprepared SOt2-/Zr-SBA-15 showed excellent triglyceride conversion efficiency of 92.3% and fatty acid methyl esters （FAME） yield of 91.7% for the transesterification of waste cooking oil with methanol under the optimized reaction conditions： the methanol/oil molar ratio of 30, the reaction temperature of 160 ℃, the reaction time of 12 h and 10wt% of catalyst. It was noticed that the as-prepared SOa2-/Zr-SBA-15 materials with the higher area surface of mesoporous framework and the surface acidity displayed excellent stability and reusability, maintaining high FAME yield of （74±1）% after seven runs of reaction.

废烟气脱硝催化剂中TiO_(2)资源化回收实验研究

采用高温碱浸和酸洗的方法对废选择性催化还原(SCR)脱硝催化剂进行处理,研究碱浸和酸洗对催化剂各组分的浸出效果,考察温度对催化剂浸出行为的影响规律。结果表明,碱浸温度的提高促进V和W的浸出,210℃时V和W的浸出率分别为82.38%和74.92%。经高温碱浸和酸洗处理后,Al、Ca、Na等杂质的最高浸出率均可达98%以上,回收TiO_(2)的纯度较高,可用于生产新催化剂。高温碱浸会破坏催化剂的结构,有利于后续HCl处理对杂质的去除,除杂效果优于直接酸洗处理。高温碱浸过程中会生成Na_(2)TiO_(3),经HCl反应并水解后会形成新的TiO_(2)颗粒,形成更多的小孔,比表面积增大。

废电解液在湿法炼锌渣中回收金、银、锌的应用研究

锌电解过程产出大量的废电解液,废电解液酸性较强并含有多种金属离子,如直接排放会对环境造成严重污染。以废电解液和浓硫酸作为浸出介质,研究了采用酸浸—浮选工艺综合回收湿法炼锌渣中金、银、锌。以常规浸出工艺产生的浸出渣(老渣)为主要研究对象,考察了矿浆搅拌速度、废电解液用量、硫酸补加量、酸浸温度对金、银浮选指标的影响。结果表明:酸浸—浮选老渣闭路试验最终获得的精矿中金品位为10.16 g/t,金回收率为78.63%,银品位为1039.64 g/t,银回收率为74.72%,锌品位为40.64%,锌回收率为21.86%,酸浸液中锌回收率为60.15%;采用热酸浸出工艺产生的浸出渣(新渣)和现浸出过程产出的新鲜渣浆进行验证试验可获得较好的闭路试验指标。该方法可实现废电解液的循环利用,使渣中有价金属得到高效综合回收。

氟碳铈矿除Ca、Si制备脱硝催化剂及其脱硝性能的研究

包头混合稀土精矿是氟碳铈矿(CeCO_(3)F)和独居石(CePO_(4))的共生矿物,结构复杂,难以分解,且Ca、Si杂质嵌布在矿物表面,影响了稀土矿物的脱硝活性,因此在使用天然矿物作为催化剂之前,有必要对其进行除杂预处理。采用酸浸固氟焙烧方案将氟碳铈矿制成脱硝催化剂,具体工艺为:第一步,HCl除Ca,HCl浓度为6mol/L,氟碳铈矿与NaCl(固氟剂)质量比为1∶5,混合并搅拌12h后于500℃下焙烧2h;第二步,HF除Si,HF浓度为13mol/L,除Ca后粉末与NaCl质量比为1∶5,混合并搅拌12h后于500°C下焙烧2h。氟碳铈矿除Ca、Si后制备的催化剂中Ca含量降至1.85%,Si含量降至0.17%,稀土元素含量相比原矿提高了约22%。氟碳铈矿除Ca、Si后,表面形成了发达的孔结构,比表面积增大,活性元素增多,且部分Ce的价态由+3价转变为+4价,还形成了晶格氧,这些组织结构的变化为催化剂脱硝过程提供了更多的氧化还原中心,使得催化剂脱硝性能显著提高。因此,用除杂后的氟碳铈矿作脱硝催化剂比直接用天然矿物具有更大的优势。

橙皮还原浸出废旧锂电池正极材料有价金属

为了促进废旧锂电池的高效环保浸出,研究了一种利用橙皮作为有机还原剂,高效浸出废旧锂电池正极材料中金属的方法。结果表明:橙皮的添加显著提高了柠檬酸浸出剂的性能,实现了锂、镍、钴和锰的高浸出率,最佳浸出条件为柠檬酸浓度2 mol/L、橙皮用量40 g/L、浸出温度95℃、液固比20∶1、搅拌速度300 r/min、浸出时间120 min。利用Design Expert 10推导出了一个浸出模型,能精确预测金属的浸出率。动力学研究表明,锂、镍、钴和锰的表观活化能分别为64.95、67.71、66.65和72.8 kJ/mol,说明正极材料浸出过程主要受化学反应控制。通过对比OP浸出前后的SEM像,验证了橙皮还原能力可用还原糖理论进行解释。

砷锑烟尘与冶炼污酸的联合处置

基于砷、锑在酸性溶液中的溶解差异性,结合砷锑烟尘和冶炼污酸的成分特征,提出氧化酸浸分砷—湿法还原固砷的砷锑烟尘与冶炼污酸的联合处置工艺。结果表明,在过氧化氢加料系数1、过氧化氢质量分数30%、液固比5、温度30℃、浸出时间4 h、污酸酸度1 mol/L条件下,砷的浸出率可达99%以上,所得浸出渣锑含量高达90%,砷含量仅为0.2%,实现了高砷锑烟尘中砷和锑的初步分离;采用氯化亚锡二段还原工艺,在酸度12 mol/L、温度90℃、n(NaCl)/n(As)=3、还原剂系数1、反应时间4 h的条件下,砷还原率可达99.75%,反应后液中锑浓度为6.72 g/L,砷浓度仅为0.17 g/L,实现砷和锑的二次分离。

钛石膏中铁浸出动力学及其酸浸循环工艺研究

硫酸法制备钛白粉的过程中产生了钛白废酸及钛石膏,采用以废治废思路,将钛白废酸作为浸取剂循环浸出钛石膏中的铁杂质,以实现资源的有效利用。研究了钛白废酸循环酸浸钛石膏的最优工艺条件,实验结果表明,在反应温度为333.15 K、液固质量比(以下简称液固比)为5∶1、反应时间为60 min、循环酸浸2次的条件下,钛石膏的除铁效率能达到80%以上。结合SEM、XRF、XRD等表征结果对比分析酸浸前后的钛石膏产品,结果发现酸浸条件能降低钛石膏中多种杂质组分含量,且酸浸前后钛石膏的物相组成均为CaSO_(4)·2H_(2)O。在上述研究的基础上形成了完整的钛石膏处理工艺,研究了在钛白废酸体系下,钛石膏中铁元素的浸出特性,并使用浸出动力学模型进行了拟合与计算,结果表明,该浸出过程受内部扩散控制,反应的表观活化能为59.08 kJ/mol。