Phosphate recovery from phosphorus-rich solution obtained from chicken manure incineration ash

The recovery of phosphorus from waste is very important for Japan because Japan has no natural phosphorus resources. In order to recover phosphorus from incineration ash of chicken manure, an acid dissolution–alkali precipitation method was investigated. Phosphorus content in the ash was 8%. The ash was treated with hydrochloric acid to obtain phosphorus-rich solution. Phosphorus could then be recovered as a precipitant by adding sodium hydroxide solution into the phosphorus-rich solution and gradually changing the pH in the solution to 3, 4, and 8. At pH 3, a small amount of phosphorus was precipitated to remove iron, which would cause coloring of subsequent precipitants. At pH 4, 84% of the phosphorus in the original solution could be recovered as CaHPO₄ · 2H₂O with a purity of 92%. At pH 8, 8% of the phosphorus in the phosphorus-rich solution could be recovered as identified hydroxyapatite. A recovery rate of 92% phosphorus as CaHPO₄ · 2H₂O and identified as hydroxyapatite was achieved.     

钼尾矿制备硅微粉

以钼尾矿为原料,采用酸溶—碳酸钾沉淀法制备硅微粉。考察了反应温度、反应时间、K₂CO₃质量分数对产品中SiO₂质量分数和SiO₂产率的影响。得到的优化工艺条件为：钼尾矿粒径小于74 μm,反应温度50 ℃,反应时间60 min,K₂CO₃质量分数50%。在此工艺条件下,SiO₂产率可达98.92%,产品硅微粉的SiO₂质量分数达98.44%,粒径为100~200 nm,超过中华人民共和国黑色冶金行业标准《不定型耐火材料用二氧化硅微粉》（YB/T 115—2004）中SF96指标（SiO₂质量分数≥96.0%）的要求。     

酸渣制备无水硫酸钠

采用炼油厂酸渣经水稀释后,添加含钠化合物进行中和反应,制备无水Na_2SO_4.最佳工艺条件为:将酸渣用水稀释20倍,按n(Na_2CO_3):n(SO_4~(2-))=1.10或n(NaOH):n(SO_4~(2-))=1.20的比例加入Na_2CO_3,溶液或NaOH溶液,油水分离去除油相后蒸发、干燥,在650℃下灼烧后溶解、过滤、蒸发、结晶,得到Na_2SO_4产品.NaCO_3法可将酸渣中约78%的SO_4~(2-)转化到产品Na_2SO_4中;NaOH法可将酸渣中约66%的SO_4~(2-)转化到产品Na_2SO_4中.制备的无水Na_2SO_4产品均达到GB/T6009-2003<工业无水硫酸钠>二类标准.     

乙烯废碱液的再生

开发了除油-苛化-脱硫组合技术处理乙烯废碱液工艺,考察了影响各级处理效果的主要因素.实验结果表明:经石英砂-聚丙烯腈纤维膜-强碱性阴离子交换树脂组合装置除油后,碱液中油类物质质量浓度小于2 mg/L,NaOH,Na_2CO_3,Na_2S等无机组分含量基本不变;经苛化-脱硫处理后碱液中Na_2CO_3和Na_2S质量浓度分别小于4 430 mg/L和4 480 mg/L;再生碱液的流体力学性质及对酸性气体的吸收性能均可满足乙烯裂解气碱洗要求.     

煤气化细渣制备碳硅复合材料吸附去除水中Pb2+

以煤气化细渣为原料制备了高比表面积碳硅复合材料,并利用过硫酸铵对其进行表面改性,用于吸附100.0 mg/L PbCl₂溶液中Pb²⁺。表征结果显示：碳硅复合材料的比表面积为1 347 m²/g,改性后降为474 m²/g;改性后材料表面的羟基、羰基和羧基等含氧基团的含量显著增加。实验结果表明：溶液pH为5时,改性碳硅复合材料对Pb²⁺的平衡吸附量为124 mg/g,Pb²⁺去除率可达98.2%;吸附过程符合准二级动力学模型,以化学吸附为主,伴有物理吸附;吸附过程分为外扩散和内扩散两个阶段,受内扩散控制。     

Ammonium removal from landfill leachate by chemical precipitation

The landfill leachate in Hong Kong usually contains quite high NH₄⁺–N concentration, which is well known to inhibit nitrification in biological treatment processes. A common pre-treatment for reducing high strength of ammonium (NH₄⁺–N) is by an air-stripping process. However, there are some operational problems such as carbonate scaling in the process of stripping. For this reason, some technical alternatives for NH₄⁺–N removal from leachate need to be studied. In this study, a bench-scale experiment was initiated to investigate the feasibility of selectively precipitating NH₄⁺–N in the leachate collected from a local landfill in Hong Kong as magnesium ammonium phosphate (MAP). In the experiment, three combinations of chemicals, MgCl₂·6H₂O+Na₂HPO₄·12H₂O, MgO+85% H₃PO₄, and Ca(H₂PO₄)₂·H₂O+MgSO₄·7H₂O, were used with the different stoichiometric ratios to generate the MAP precipitate effectively. The results indicated that NH₄⁺–N contained in the leachate could be quickly reduced from 5618 to 112 mg/l within 15 min, when MgCl₂·6H₂O and Na₂HPO₄·12H₂O were applied with a Mg²⁺:NH₄⁺:PO₄³⁻ mol ratio of 1:1:1. The pH range of the minimum MAP solubility was discovered to be between 8.5 and 9.0. Attention should be given to the high salinity formed in the treated leachate by using MgCl₂·6H₂O and Na₂HPO₄·12H₂O, which may affect microbial activity in the following biological treatment processes. The other two combinations of chemicals [MgO+85% H₃PO₄ and Ca(H₂PO₄)2·H₂O+MgSO₄·7H₂O] could minimise salinity after precipitation, but they were less efficient for NH₄⁺–N removal, compared with MgCl₂·6H₂O and Na₂HPO₄·12H₂O. COD had no significant reduction during this precipitation. It was found that the sludge of MAP generated was easily settled within 10 min to reach its solids content up to 27%. The other characteristics including capillary suction time (CST) and dry density (DD) of the MAP sludge were also tested. The experimental results indicate that the settled sludge is quite solid and can be directly dumped at a landfill site even without any further dewatering treatment.     

Synthesis of chromium-containing pigments from chromium recovered from leather waste

Cobalt-chromite green and chrome-tin pink pigments have been prepared from chromium extracted from leather shavings produced as a waste product of the leather-tanning industry. The alkaline agent (NaOH, CaO, MgO, NH4OH) used in the extraction process influences the nature of the final product. The effect of the NH4OH:CaO ratio on the final product in the case of cobalt-chromite green was examined. The pigments obtained were characterized by FT-IR and X-ray diffraction (XRD). Colour measurements were compared with those recorded from materials prepared from pure Cr2O3. The leaching of Cr(VI) from the materials was examined by UV spectroscopy.     

电镀废水中镍的回收和利用

采用化学沉淀法回收电镀含镍废水中的Ni~(2+),研究了各工艺因素对回收效果的影响.实验结果表明,回收电镀含镍废水中Ni~(2+)的最佳工艺条件为:反应温度30 ℃,废水pH 12～13,0.1 mol/L的NaOH溶液加入量70 mL,以聚丙烯酸钠为絮凝剂,搅拌转速1 250 r/min,搅拌时间2 min.将回收产物Ni(OH)_2用作润滑油添加剂可有效改善润滑油的摩擦磨损性能.     

氧化剂对土壤中石油污染物去除率的影响

以FeSO_4-柠檬酸为催化剂,探讨了不同氧化剂的类型、浓度、与催化剂的比例等因素对土壤中石油污染物去除率的影响。实验结果表明:各氧化剂体系的石油去除率大小顺序为KMnO_4CaO_2≥H_2O_2K_2S_2O_8;随着反应时间的延长,各体系的石油去除率均呈现出先快速增涨、再缓慢增加后略有降低的趋势;在氧化剂浓度相同条件下,H_2O_2体系和Na_2S_2O_8体系的石油去除率分别比对照增加了145.5%~238.7%和112.6%~167.5%;在催化剂用量相同条件下,H_2O_2体系和Na_2S_2O_8体系达到最高石油去除率时的n(氧化剂)∶n(催化剂)分别为50∶1和100∶1;H_2O_2体系对残油族组分的去除率大小顺序为非烃芳烃饱和烃沥青质。     

含铜废催化剂中铜的回收

采用热解—氨浸工艺处理含铜废催化剂（w（Cu）为23.6%）,优化了工艺条件,并通过蒸氨还原法制备出Cu₂O产品。实验结果表明：热解工段中,控制管式热解炉的空气流量为3.0 m³/min,在升温速率20 ℃/min、热解终温600 ℃、终温保持时间90 min的优化条件下,含铜废催化剂中的有机物热解完全;氨浸工段中,以NH₄Cl-NH₃-H₂O溶液为氨浸液,控制氨浸温度为40 ℃,在烧成料研磨时间90 min（粒径29.43 μm）、氨浸液总氨浓度4 mol/L、氨浸时间80 min的优化条件下,铜浸出率达到98%;经蒸氨还原法制得的Cu₂O产品的质量符合HG/T 2961—2010《工业氧化亚铜》中的一等品标准,产率为24%。     

Determinants of nitrous oxide emission from agricultural drainage waters

Emissions of the powerful greenhouse gas nitrous oxide (N₂O) from agricultural drainage waters are poorly quantified and its determinants are not fully understood. Nitrous oxide formation in agricultural soils is known to increase in response to N fertiliser application, but the response of N₂O in field drainage waters is unknown. This investigation combined an intensive study of the direct flux of N₂O from the surface of a fertilised barley field with measurement of dissolved N₂O and nitrate (NO₃) concentrations in the same field’s drainage waters. Dissolved N₂O in drainage waters showed a clear response to field N fertilisation, following an identical pattern to direct N₂O flux from the field surface. The range in N₂O concentrations between individual field drains sampled on the same day was large, indicating considerable spatial variability exists at the farm scale. A consistent pattern of very rapid outgassing of the dissolved N₂O in open drainage ditches was accentuated at a weir, where increased turbulence led to a clear drop in dissolved N₂O concentration. This study underlines the need for carefully planned sampling campaigns wherever whole farm or catchment N₂O emission budgets are attempted. It adds weight to the argument for the downward revision of the IPCC emission factor (EF₅-g) for NO₃ in drainage waters.     

Recovery of nickel oxide from spent catalyst

This study investigates the possibility of recovering nickel from the spent catalyst (NiO/Al2O3) resulting from the steam reforming process to produce water gas (H2/H2O) in many industries. In the extraction process, nickel is recovered as sulfate using sulfuric acid as a solvent. The considered parameters affecting nickel recovery were acid concentration, temperature and time of digestion solid:liquid ratio, particle size and stirring rate. Nickel was to be directly recovered as a sulfate salt by direct crystallization method. The conversion was 99% at 50% sulfuric acid concentration, solid: liquid ratio (1:12) by weight, particle size less than 500 micron for more than 5 h and 800 rpm at 100 degrees C.     

Determinants of nitrous oxide emission from agricultural drainage waters

Emissions of the powerful greenhouse gas nitrous oxide (N₂O) from agricultural drainage waters are poorly quantified and its determinants are not fully understood. Nitrous oxide formation in agricultural soils is known to increase in response to N fertiliser application, but the response of N₂O in field drainage waters is unknown. This investigation combined an intensive study of the direct flux of N₂O from the surface of a fertilised barley field with measurement of dissolved N₂O and nitrate (NO₃) concentrations in the same fields drainage waters. Dissolved N₂O in drainage waters showed a clear response to field N fertilisation, following an identical pattern to direct N₂O flux from the field surface. The range in N₂O concentrations between individual field drains sampled on the same day was large, indicating considerable spatial variability exists at the farm scale. A consistent pattern of very rapid outgassing of the dissolved N₂O in open drainage ditches was accentuated at a weir, where increased turbulence led to a clear drop in dissolved N₂O concentration. This study underlines the need for carefully planned sampling campaigns wherever whole farm or catchment N₂O emission budgets are attempted. It adds weight to the argument for the downward revision of the IPCC emission factor (EF₅-g) for NO₃ in drainage waters.     

湿法烟气脱硫石膏制备硫酸铵

采用湿法烟气脱硫石膏为原料,与( NH4)2CO3反应,制备(NH4)2SO4.通过X射线衍射仪表征可知:脱硫石膏的主要成分为CaSO4,反应后CaSO4中的Ca2+大部分以CaCO3形式存在于固体沉淀物中,CaCO3粉末平均粒径为80 nm;而原先CaSO4中的不溶性SO2-4则与NH+4结合生成(NH4)2SO4,...     

从含铬铝泥中回收铝的新工艺

采用"打浆水洗除Cr(Ⅵ)—电渗析除Cr(Ⅵ)—碱浸提铝—碳酸化分解法精制Al_2O_3"的新工艺处理含铬铝泥(以下简称铝泥),并回收Al_2O_3。实验结果表明:铝泥在70℃下经3次打浆水洗后,w(Na_2CrO_4)(以干铝泥计)降至5.0%;采用电渗析除Cr(Ⅵ)工艺可有效去除铝泥中以结合态和结晶态形式存在的Na_2CrO_4,在55 V直流电压下电渗析6h后铝泥中的w(Na_2CrO_4)降至0.98%;在碱浸温度为100℃、碱浸时间为3 h、NaOH质量浓度为150 g/L的优化碱浸条件下,铝浸出率(以Al_2O_3计)高达90.0%;经3次碳酸化分解处理后,Al_2O_3产品的纯度达98.65%,满足GB/T 24487-2009《氧化铝》中的一级标准,Al_2O_3回收率为96.37%。     

汞矿区汞污染土壤的淋洗修复

以贵州省铜仁市汞矿区汞污染土壤为研究对象,分别采用KI、Na_2S_2O_3、乙二胺四乙酸、柠檬酸、酒石酸、十二烷基硫酸钠溶液对其进行淋洗修复,筛选出合适的淋洗剂,优化了淋洗条件,并探索了淋洗液的处理方法。实验结果表明:对该土壤淋洗效果最好的淋洗剂为Na_2S_2O_3,最佳淋洗条件为Na_2S_2O_3浓度0.01 mol/L、固液比(g/m L)1∶5、淋洗时间4 h、淋洗次数1次,在此条件下土壤中总汞的淋洗率为13.41%,有效态汞含量可降至原来的61.54%;Na2S对淋洗液中的汞具有较好的去除效果,每升淋洗液加入0.6 g Na_2S处理后,即可满足GB8978—1996《污水综合排放标准》。     

旋转填充床分离沼气中的CO_2

以水为吸收液,采用旋转填充床分离微生物厌氧发酵沼气中的CO_2,考察了工艺条件对CO_2吸收效果的影响。实验结果表明:进液量越大、气液比越小、进口CO_2体积分数越小、操作压力越大、进液温度越低则CO_2的吸收效果越好,而床转速以适中为宜;在进液量60 L/h、气液比3.3、床转速1 000 r/min、进口CO_2体积分数40%、操作压力1.2 MPa、进液温度5℃的条件下,CO_2吸收率为57.4%,提纯后气体的CO_2体积分数为17%。     

利用含铬废水和含铅废水制备铬黄

利用净化后的含铬废水和含铅废水制备铬黄.采用沉淀法对废水进行净化预处理,最佳工艺条件:100mL含铬废水中加入20 g Na_2CO_3,及10 mL H_2O_2,用NaOH调节含铬废水pH为10.00;用NaOH调节含铅废水pH为2.65.将净化后的10 mL含铬废水和25 mL含铅废水混合,在55-60℃条件下反应10 min,合成的铬黄达到GB/T 3184-2008<铬酸铅颜料和钼铬酸铅颜料>的质量标准.经重金属吸附剂处理Pb~(2+)后铬黄合成滤液中的Cr~(6+)和Pb~(2+)质量浓度均达到GB8978-1996<污水综合排放标准>的指标.     

Hydrometallurgical recycling of cobalt from zinc plants residue

A large amount of hot filter cake (HFC) is annually generated in Iranian zinc plants. It contains 1% zinc, 16–30% manganese, 5–25% calcium and 1–4.5% cobalt. Usually, zinc is selectively leached by an alkaline medium and its residue is known as alkaline leached HFC (ALHFC). In the present study, the possibility of cobalt extraction from ALHFC was investigated using a creative hydrometallurgical process. At the first stage, zinc and cadmium were selectively removed with sulfuric acid. At the second stage, it was deeply focused on the possibility of selective reductive leaching of cobalt by H₂O₂ as a reductant in the presence of manganese. As results, several differences were found between the mechanism of cobalt and manganese leaching. Accordingly, cobalt leaching was more affected by acid concentration and manganese leaching was more affected by reductant concentration. Consequently, with manipulating these important parameters, it was made possible to selectively separate cobalt from manganese. Based on the obtained results, 90.9% of cobalt and only 10.04% of manganese were leached with 1% of H₂O₂. At the third stage, pregnant cobalt solution was successfully purified through a solvent extraction process with D2EHPA. Finally, cobalt hydroxide as our final product with a purity of more than 99% was precipitated from the pure pregnant solution at 70 °C.     

用含硫化砷废渣制备砷酸铜

以湖北省某化工企业含砷废水处理过程中产生的含硫化砷废渣为研究对象,采用氧化碱浸—沉淀工艺制备砷酸铜。考察了沉淀反应液pH、沉淀反应温度、搅拌转速对砷沉淀效果的影响。采用XRD和SEM技术对砷酸铜的物相及形貌进行了表征。实验结果表明：废渣在氧化碱浸过程的砷浸出率为96.53%;沉淀反应时间为30 min时,沉淀步骤的最佳工艺条件为沉淀反应液pH 5.0、搅拌转速500 r/min、沉淀反应温度50 ℃。验证实验结果表明,在该工艺条件下,砷沉淀率均达93.96%以上。SEM表征结果显示,砷酸铜产品为颗粒状,粒径约为500 nm。XRD表征结果显示,砷酸铜产品中主要含有Cu₃As₂O₈,Cu₄O（AsO₄）₂,Cu₄（As₂O₇）O₂。该方法工艺简单、无二次污染,为废渣的综合利用提供了一种新的技术路线。