CN106423045B - A kind of modified montmorillonoid sorbent preparation method of Treatment of Zinc-containing Wastewater - Google Patents
A kind of modified montmorillonoid sorbent preparation method of Treatment of Zinc-containing Wastewater Download PDFInfo
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- 238000002360 preparation method Methods 0.000 title claims abstract description 25
- 239000002351 wastewater Substances 0.000 title claims abstract description 25
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 title claims abstract description 22
- 229910052725 zinc Inorganic materials 0.000 title claims abstract description 22
- 239000011701 zinc Substances 0.000 title claims abstract description 22
- 238000011282 treatment Methods 0.000 title claims description 15
- 239000002594 sorbent Substances 0.000 title 1
- GUJOJGAPFQRJSV-UHFFFAOYSA-N dialuminum;dioxosilane;oxygen(2-);hydrate Chemical class O.[O-2].[O-2].[O-2].[Al+3].[Al+3].O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O GUJOJGAPFQRJSV-UHFFFAOYSA-N 0.000 claims abstract description 104
- 229910052901 montmorillonite Inorganic materials 0.000 claims abstract description 72
- 239000000725 suspension Substances 0.000 claims abstract description 43
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 34
- 239000003463 adsorbent Substances 0.000 claims abstract description 28
- 239000000138 intercalating agent Substances 0.000 claims abstract description 28
- 239000012153 distilled water Substances 0.000 claims abstract description 24
- 239000000843 powder Substances 0.000 claims abstract description 21
- 238000000034 method Methods 0.000 claims abstract description 15
- 238000000746 purification Methods 0.000 claims abstract description 12
- 239000008367 deionised water Substances 0.000 claims abstract description 7
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 7
- 238000001914 filtration Methods 0.000 claims abstract description 5
- 238000000703 high-speed centrifugation Methods 0.000 claims abstract 2
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 30
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 22
- 229910017604 nitric acid Inorganic materials 0.000 claims description 22
- 229920002401 polyacrylamide Polymers 0.000 claims description 22
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 16
- 239000007788 liquid Substances 0.000 claims description 16
- 238000005119 centrifugation Methods 0.000 claims description 11
- 238000001035 drying Methods 0.000 claims description 10
- 239000000463 material Substances 0.000 claims description 7
- 238000004140 cleaning Methods 0.000 claims description 3
- 230000008569 process Effects 0.000 claims description 3
- 238000007873 sieving Methods 0.000 claims description 3
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims 7
- 229910052938 sodium sulfate Inorganic materials 0.000 claims 7
- 235000011152 sodium sulphate Nutrition 0.000 claims 7
- RCEAADKTGXTDOA-UHFFFAOYSA-N OS(O)(=O)=O.CCCCCCCCCCCC[Na] Chemical compound OS(O)(=O)=O.CCCCCCCCCCCC[Na] RCEAADKTGXTDOA-UHFFFAOYSA-N 0.000 claims 3
- 238000002156 mixing Methods 0.000 claims 3
- 229960000935 dehydrated alcohol Drugs 0.000 claims 2
- MVFCKEFYUDZOCX-UHFFFAOYSA-N iron(2+);dinitrate Chemical compound [Fe+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O MVFCKEFYUDZOCX-UHFFFAOYSA-N 0.000 claims 2
- 238000011010 flushing procedure Methods 0.000 claims 1
- 230000001376 precipitating effect Effects 0.000 claims 1
- 239000007787 solid Substances 0.000 claims 1
- 238000012986 modification Methods 0.000 abstract description 19
- 230000004048 modification Effects 0.000 abstract description 19
- 238000009830 intercalation Methods 0.000 abstract description 9
- 238000001354 calcination Methods 0.000 abstract description 5
- 230000002687 intercalation Effects 0.000 abstract description 5
- 238000003756 stirring Methods 0.000 abstract description 4
- 239000003795 chemical substances by application Substances 0.000 abstract description 2
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 description 28
- 239000000243 solution Substances 0.000 description 28
- VCJMYUPGQJHHFU-UHFFFAOYSA-N iron(3+);trinitrate Chemical compound [Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O VCJMYUPGQJHHFU-UHFFFAOYSA-N 0.000 description 16
- PTFCDOFLOPIGGS-UHFFFAOYSA-N Zinc dication Chemical compound [Zn+2] PTFCDOFLOPIGGS-UHFFFAOYSA-N 0.000 description 13
- NWONKYPBYAMBJT-UHFFFAOYSA-L zinc sulfate Chemical compound [Zn+2].[O-]S([O-])(=O)=O NWONKYPBYAMBJT-UHFFFAOYSA-L 0.000 description 9
- 229960001763 zinc sulfate Drugs 0.000 description 9
- 229910000368 zinc sulfate Inorganic materials 0.000 description 9
- 238000001556 precipitation Methods 0.000 description 8
- 238000005406 washing Methods 0.000 description 8
- 238000001179 sorption measurement Methods 0.000 description 7
- 239000000203 mixture Substances 0.000 description 6
- 239000010865 sewage Substances 0.000 description 6
- 230000000694 effects Effects 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 5
- 230000008901 benefit Effects 0.000 description 3
- 239000003344 environmental pollutant Substances 0.000 description 3
- 229910052500 inorganic mineral Inorganic materials 0.000 description 3
- 239000011707 mineral Substances 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 231100000719 pollutant Toxicity 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 241000282414 Homo sapiens Species 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 229910001385 heavy metal Inorganic materials 0.000 description 2
- 239000011259 mixed solution Substances 0.000 description 2
- 230000007935 neutral effect Effects 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000009388 chemical precipitation Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000005189 flocculation Methods 0.000 description 1
- 230000016615 flocculation Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000000750 progressive effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000004083 survival effect Effects 0.000 description 1
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
- B01J20/12—Naturally occurring clays or bleaching earth
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/281—Treatment of water, waste water, or sewage by sorption using inorganic sorbents
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- Dispersion Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Hydrology & Water Resources (AREA)
- Engineering & Computer Science (AREA)
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Abstract
一种处理含锌废水的改性蒙脱土吸附剂制备方法，其步骤为：（1）蒙脱土悬浊液的制备：通过预处理措施将蒙脱土提纯为细粉状材料，并与蒸馏水配制成蒙脱土悬浊液；（2）FN插层剂的制备，（3）FN插层剂的无机改性，（4）FN插层蒙脱土的提纯，（5）SDS插层剂的制备，（6）SDS插层剂的有机改性，（7）PAM絮凝剂的制备，（8）SDS插层蒙脱土的提纯，在步骤（6）中得到的二次改性蒙脱土悬浊液中滴加PAM絮凝剂，快速搅拌均匀后进行高速离心、过滤，将滤渣用去离子水清洗至中性，进行低温干燥，得到纯净的SDS插层蒙脱土粉末；（9）将步骤（8）制得的SDS插层蒙脱土粉末高温焙烧，制得改性蒙脱土吸附剂。A method for preparing a modified montmorillonite adsorbent for treating zinc-containing wastewater. Distilled water was prepared into montmorillonite suspension; (2) preparation of FN intercalating agent, (3) inorganic modification of FN intercalating agent, (4) purification of FN intercalated montmorillonite, (5) SDS intercalation preparation of the agent, (6) organic modification of SDS intercalating agent, (7) preparation of PAM flocculant, (8) purification of SDS intercalated montmorillonite, the secondary modified montmorillonite obtained in step (6) Add PAM flocculant dropwise to the de-soiled suspension, stir evenly, then perform high-speed centrifugation and filtration, wash the filter residue with deionized water to neutrality, and dry at low temperature to obtain pure SDS intercalated montmorillonite powder; (9 ) calcining the SDS intercalated montmorillonite powder obtained in step (8) at high temperature to obtain a modified montmorillonite adsorbent.
Description
技术领域technical field
本发明涉及工业污水治理领域，尤其涉及处理含锌废水的改性蒙脱土吸附剂制备技术。The invention relates to the field of industrial sewage treatment, in particular to the preparation technology of a modified montmorillonite adsorbent for treating zinc-containing wastewater.
背景技术Background technique
近年来，随着工业领域发展，人们对于水资源的需求量逐渐增加，同时全球性的水环境污染问题也变得愈加突出。人类工业活动引起污水大量排放，导致地球表面水体中重金属污染物浓度逐渐增大，严重威胁到人类的生存与生活环境。尤其是某些活性较高的重金属离子污水，例如含锌废水的处理问题，由于其治理难度大、效果差、成本高，引起了社会民众及众多专家的高度关注，已经成为工业污水治理领域必须攻克的一大技术难题。In recent years, with the development of the industrial field, people's demand for water resources has gradually increased, and the global water environment pollution problem has become more and more prominent. The massive discharge of sewage caused by human industrial activities leads to the gradual increase in the concentration of heavy metal pollutants in the water bodies on the earth's surface, which seriously threatens the survival and living environment of human beings. In particular, the treatment of some highly active heavy metal ion sewage, such as zinc-containing wastewater, has attracted great attention from the public and many experts due to its difficult treatment, poor effect and high cost, and has become a must in the field of industrial sewage treatment. A major technical problem to overcome.
目前含锌废水的锌离子浓度已经处在一个较低的水平，常用的去除锌离子措施有化学沉淀法、离子交换法、活性炭吸附等方法，但这些技术存在处理效率低、经济效益低等缺点。经过数十年的技术沉淀，矿物材料的污染物吸附性能逐渐被人们发现，矿物吸附剂因为其储量丰富、成本低廉、对环境影响小等优点备受关注，有关矿物吸附剂用于含锌污水处理控制的研究也逐渐成为热点。其中，蒙脱土因为其较高的比表面积、较大的孔隙率以及性质稳定、成本低廉等特性，被作为一种优良的吸附材料而得到广泛的研究。蒙脱土本身的锌离子吸附性能并不高，但是对其进行特定的改性之后，其锌离子吸附性能可大幅增加。目前有关蒙脱土的无机、有机改性来增加其对特定污染物吸附性能的研究已经非常广泛，但是对于通过改性来实现其对含锌废水的处理能力提升，还未有太多研究，因此将蒙脱土应用于含锌废水处理，往往不能达到好的处理效果。采用新技术将蒙脱土进行适当的改性，来提高其锌离子吸附性能，对于含锌废水的处理可发挥重要作用。At present, the concentration of zinc ions in zinc-containing wastewater is already at a relatively low level. Commonly used measures to remove zinc ions include chemical precipitation, ion exchange, and activated carbon adsorption. However, these technologies have disadvantages such as low treatment efficiency and low economic benefits. . After decades of technical precipitation, people have gradually discovered the pollutant adsorption properties of mineral materials. Mineral adsorbents have attracted much attention because of their abundant reserves, low cost, and low environmental impact. The use of mineral adsorbents in zinc-containing wastewater The research on processing control has gradually become a hot spot. Among them, montmorillonite has been widely studied as an excellent adsorbent because of its high specific surface area, large porosity, stable properties, and low cost. The zinc ion adsorption performance of montmorillonite itself is not high, but after specific modification, its zinc ion adsorption performance can be greatly increased. At present, the research on inorganic and organic modification of montmorillonite to increase its adsorption performance for specific pollutants has been very extensive, but there is not much research on the improvement of its treatment capacity for zinc-containing wastewater through modification. Therefore, the application of montmorillonite in the treatment of zinc-containing wastewater often fails to achieve a good treatment effect. The new technology is used to properly modify montmorillonite to improve its zinc ion adsorption performance, which can play an important role in the treatment of zinc-containing wastewater.
发明内容SUMMARY OF THE INVENTION
本发明的目的是提供一种处理含锌废水的改性蒙脱土吸附剂制备方法。The object of the present invention is to provide a method for preparing a modified montmorillonite adsorbent for treating zinc-containing wastewater.
本发明是一种处理含锌废水的改性蒙脱土吸附剂制备方法，包括以下操作步骤：The present invention is a method for preparing a modified montmorillonite adsorbent for treating zinc-containing wastewater, comprising the following operation steps:
（1）蒙脱土悬浊液的制备：通过冲洗、烘干、粉碎、过筛等预处理措施将蒙脱土提纯为100～150目的细粉状材料，并与蒸馏水按固液质量比为0.1～0.2配制成蒙脱土悬浊液；(1) Preparation of montmorillonite suspension: Purify montmorillonite into 100-150 mesh fine powder materials through pretreatment measures such as washing, drying, crushing, and sieving, and the solid-liquid mass ratio with distilled water is: 0.1～0.2 is formulated into montmorillonite suspension;
（2）FN插层剂的制备：将1mol/L硝酸铁溶液、1mol/L氢氧化钠溶液按以下比例混合均匀：1mol/L硝酸铁溶液10～12mL、1mol/L氢氧化钠溶液20～25mL；(2) Preparation of FN intercalating agent: Mix 1 mol/L ferric nitrate solution and 1 mol/L sodium hydroxide solution uniformly in the following proportions: 10-12 mL of 1 mol/L ferric nitrate solution, 20-12 mL of 1 mol/L sodium hydroxide solution 25mL;
（3）FN插层剂的无机改性：在60～80℃恒温条件下，将步骤（1）中配制的蒙脱土悬浊液及步骤（2）中配制的FN插层剂，按5:1～3:1的比例混合均匀，充分搅拌并超声分散15～20分钟，使蒙脱土悬浊液充分改性；(3) Inorganic modification of FN intercalating agent: under the constant temperature condition of 60-80 °C, the montmorillonite suspension prepared in step (1) and the FN intercalating agent prepared in step (2) were prepared according to 5. The ratio of :1～3:1 is evenly mixed, fully stirred and ultrasonically dispersed for 15～20 minutes, so that the montmorillonite suspension is fully modified;
（4）FN插层蒙脱土的提纯：将步骤（3）中得到的FN插层改性蒙脱土悬浊液经离心、沉淀后，采用无水乙醇清洗，多次重复离心、沉淀、清洗过程直至溶液PH值低于8.0，之后于60～80℃下进行低温干燥，得到纯净的FN插层蒙脱土粉末；(4) Purification of FN intercalated montmorillonite: After centrifugation and precipitation, the FN intercalated modified montmorillonite suspension obtained in step (3) was washed with absolute ethanol, and the centrifugation, precipitation, The cleaning process is carried out until the pH value of the solution is lower than 8.0, and then low-temperature drying is carried out at 60 to 80 ° C to obtain pure FN intercalated montmorillonite powder;
（5）SDS插层剂的制备：在常温条件下，将十二烷基硫酸钠（SDS）、1mol/L硝酸和无水乙醇，按以下比例混合均匀：十二烷基硫酸钠20～25g，1mol/L硝酸10～12mL，无水乙醇10～12mL；(5) Preparation of SDS intercalating agent: Under normal temperature conditions, mix sodium dodecyl sulfate (SDS), 1mol/L nitric acid and absolute ethanol in the following proportions: 20-25g sodium dodecyl sulfate , 1mol/L nitric acid 10～12mL, absolute ethanol 10～12mL;
（6）SDS插层剂的有机改性：将步骤（4）中提纯得到的FN插层蒙脱土粉末与蒸馏水按固液质量比为0.1～0.2配制成FN插层蒙脱土悬浊液，并与步骤（5）中制备的SDS插层剂按8:1～5:1的比例混合均匀，充分搅拌并超声分散15～20分钟，使FN插层蒙脱土悬浊液二次改性；(6) Organic modification of SDS intercalating agent: the FN intercalating montmorillonite powder purified in step (4) and distilled water are prepared into FN intercalating montmorillonite suspension liquid according to the solid-liquid mass ratio of 0.1-0.2 , and evenly mixed with the SDS intercalating agent prepared in step (5) at a ratio of 8:1 to 5:1, fully stirred and ultrasonically dispersed for 15 to 20 minutes, so that the FN intercalated montmorillonite suspension was reformed twice. sex;
（7）PAM絮凝剂的制备：将聚丙烯酰胺、1mol/L硝酸和蒸馏水在常温条件下，按以下比例混合均匀：聚丙烯酰胺5～10g，1mol/L硝酸10～12mL，蒸馏水100～120mL；(7) Preparation of PAM flocculant: Mix polyacrylamide, 1mol/L nitric acid and distilled water at room temperature in the following proportions: polyacrylamide 5-10g, 1mol/L nitric acid 10-12mL, distilled water 100-120mL ;
（8）SDS插层蒙脱土的提纯：在步骤（6）中得到的SDS插层改性蒙脱土悬浊液中滴加0.5%～0.8%的PAM絮凝剂，快速搅拌均匀后进行高速离心、过滤，将过滤的滤渣用去离子水清洗至中性，之后于60～80℃下进行低温干燥，得到纯净的SDS插层蒙脱土粉末；(8) Purification of SDS-intercalated montmorillonite: add 0.5% to 0.8% of PAM flocculant dropwise to the SDS-intercalated modified montmorillonite suspension obtained in step (6), stir quickly and evenly, then carry out high-speed Centrifuge and filter, wash the filtered residue with deionized water until neutral, and then dry at low temperature at 60-80°C to obtain pure SDS intercalated montmorillonite powder;
（9）将步骤（8）制得的SDS插层蒙脱土粉末在450～550℃下高温焙烧30～45分钟，制得改性蒙脱土吸附剂。(9) calcining the SDS intercalated montmorillonite powder obtained in step (8) at a high temperature of 450-550° C. for 30-45 minutes to obtain a modified montmorillonite adsorbent.
本发明可达到相当的技术进步性及实用性，并具有产业上的广泛利用价值，其至少具有下列优点：The present invention can achieve considerable technical progress and practicability, and has extensive industrial value, and at least has the following advantages:
（1）本发明提供了一种处理含锌废水的改性蒙脱土吸附剂制备方法，以蒙脱土为基础吸附剂经过两次改性处理，得到改性蒙脱土吸附剂，对工业废水中含锌废水的锌离子具有较高的吸附性。(1) The present invention provides a method for preparing a modified montmorillonite adsorbent for treating zinc-containing wastewater. The modified montmorillonite adsorbent is obtained by taking montmorillonite as a basic adsorbent through two modification treatments, which is suitable for industrial use. Zinc ions in wastewater containing zinc have high adsorption.
（2）本发明原料广泛、环保性好、成本低廉，且制备工艺简单，能够明显降低工业成本，符合污水治理产业发展要求，具有较高的产业利用价值。(2) The present invention has a wide range of raw materials, good environmental protection, low cost, and simple preparation process, which can significantly reduce industrial costs, meet the development requirements of the sewage treatment industry, and have high industrial utilization value.
具体实施方式Detailed ways
本发明提供了一种处理含锌废水的改性蒙脱土吸附剂制备方法，在技术上有明显的进步性，并具有显著的有益效果，是一种新颖、进步、有效的新技术。有关本发明的前述及其他技术内容、特点及功效，将在以下具体进行说明。通过具体实施方式的说明，当可对本发明为达成预定目的所采取的技术手段及功效得以更加深入且具体的了解，然而所附实施例仅是提供参考与说明之用，并非用来对本发明加以限制。The invention provides a method for preparing a modified montmorillonite adsorbent for treating zinc-containing wastewater, which has obvious technical progress and significant beneficial effects, and is a novel, advanced and effective new technology. The foregoing and other technical contents, features and effects of the present invention will be described in detail below. Through the description of the specific embodiments, the technical means and effects adopted by the present invention to achieve the predetermined purpose can be more deeply and concretely understood. However, the attached embodiments are only used for reference and description, and are not used to interpret the present invention. limit.
本发明提供了一种处理含锌废水的改性蒙脱土吸附剂制备方法，以蒙脱石为基础吸附剂，先对蒙脱石进行无机改性，得到FN插层蒙脱土，再进行有机改性及絮凝、提纯，得到纯净的SDS插层蒙脱土粉末，经过高温焙烧后，制得改性蒙脱土吸附剂。利用该方法获得的改性蒙脱土吸附剂对含锌废水中锌离子的去除率可达到88.0％以上。The invention provides a method for preparing a modified montmorillonite adsorbent for treating zinc-containing wastewater. The montmorillonite is used as the basic adsorbent, and the montmorillonite is firstly modified inorganically to obtain FN intercalated montmorillonite. After organic modification, flocculation and purification, pure SDS intercalated montmorillonite powder is obtained, and after high temperature roasting, the modified montmorillonite adsorbent is obtained. The modified montmorillonite adsorbent obtained by this method can achieve a removal rate of over 88.0% for zinc ions in zinc-containing wastewater.
本发明一种处理含锌废水的改性蒙脱土吸附剂制备方法，包括以下操作步骤：The present invention is a method for preparing a modified montmorillonite adsorbent for treating zinc-containing wastewater, comprising the following operation steps:
（1）蒙脱土悬浊液的制备：通过冲洗、烘干、粉碎、过筛等预处理措施将蒙脱土提纯为100～150目的细粉状材料，并与蒸馏水按固液质量比为0.1～0.2配制成蒙脱土悬浊液；(1) Preparation of montmorillonite suspension: Purify montmorillonite into 100-150 mesh fine powder materials through pretreatment measures such as washing, drying, crushing, and sieving, and the solid-liquid mass ratio with distilled water is: 0.1～0.2 is formulated into montmorillonite suspension;
（2）FN插层剂的制备：将1mol/L硝酸铁溶液、1mol/L氢氧化钠溶液按以下比例混合均匀：1mol/L硝酸铁溶液10～12mL、1mol/L氢氧化钠溶液20～25mL；(2) Preparation of FN intercalating agent: Mix 1 mol/L ferric nitrate solution and 1 mol/L sodium hydroxide solution uniformly in the following proportions: 10-12 mL of 1 mol/L ferric nitrate solution, 20-12 mL of 1 mol/L sodium hydroxide solution 25mL;
（3）FN插层剂的无机改性：在60～80℃恒温条件下，将步骤（1）中配制的蒙脱土悬浊液及步骤（2）中配制的FN插层剂，按5:1～3:1的比例混合均匀，充分搅拌并超声分散15～20分钟，使蒙脱土悬浊液充分改性；(3) Inorganic modification of FN intercalating agent: under the constant temperature condition of 60-80 °C, the montmorillonite suspension prepared in step (1) and the FN intercalating agent prepared in step (2) were prepared according to 5. The ratio of :1～3:1 is evenly mixed, fully stirred and ultrasonically dispersed for 15～20 minutes, so that the montmorillonite suspension is fully modified;
（4）FN插层蒙脱土的提纯：将步骤（3）中得到的FN插层改性蒙脱土悬浊液经离心、沉淀后，采用无水乙醇清洗，多次重复离心、沉淀、清洗过程直至溶液PH值低于8.0，之后于60～80℃下进行低温干燥，得到纯净的FN插层蒙脱土粉末；(4) Purification of FN intercalated montmorillonite: After centrifugation and precipitation, the FN intercalated modified montmorillonite suspension obtained in step (3) was washed with absolute ethanol, and the centrifugation, precipitation, The cleaning process is carried out until the pH value of the solution is lower than 8.0, and then low-temperature drying is carried out at 60 to 80 ° C to obtain pure FN intercalated montmorillonite powder;
（5）SDS插层剂的制备：在常温条件下，将十二烷基硫酸钠（SDS）、1mol/L硝酸和无水乙醇，按以下比例混合均匀：十二烷基硫酸钠20～25g，1mol/L硝酸10～12mL，无水乙醇10～12mL；(5) Preparation of SDS intercalating agent: Under normal temperature conditions, mix sodium dodecyl sulfate (SDS), 1mol/L nitric acid and absolute ethanol in the following proportions: 20-25g sodium dodecyl sulfate , 1mol/L nitric acid 10～12mL, absolute ethanol 10～12mL;
（6）SDS插层剂的有机改性：将步骤（4）中提纯得到的FN插层蒙脱土粉末与蒸馏水按固液质量比为0.1～0.2配制成FN插层蒙脱土悬浊液，并与步骤（5）中制备的SDS插层剂按8:1～5:1的比例混合均匀，充分搅拌并超声分散15～20分钟，使FN插层蒙脱土悬浊液二次改性；(6) Organic modification of SDS intercalating agent: the FN intercalating montmorillonite powder purified in step (4) and distilled water are prepared into FN intercalating montmorillonite suspension liquid according to the solid-liquid mass ratio of 0.1-0.2 , and evenly mixed with the SDS intercalating agent prepared in step (5) at a ratio of 8:1 to 5:1, fully stirred and ultrasonically dispersed for 15 to 20 minutes, so that the FN intercalated montmorillonite suspension was reformed twice. sex;
（7）PAM絮凝剂的制备：将聚丙烯酰胺、1mol/L硝酸和蒸馏水在常温条件下，按以下比例混合均匀：聚丙烯酰胺5～10g，1mol/L硝酸10～12mL，蒸馏水100～120mL；(7) Preparation of PAM flocculant: Mix polyacrylamide, 1mol/L nitric acid and distilled water at room temperature in the following proportions: polyacrylamide 5-10g, 1mol/L nitric acid 10-12mL, distilled water 100-120mL ;
（8）SDS插层蒙脱土的提纯：在步骤（6）中得到的SDS插层改性蒙脱土悬浊液中滴加0.5%～0.8%的PAM絮凝剂，快速搅拌均匀后进行高速离心、过滤，将过滤的滤渣用去离子水清洗至中性，之后于60～80℃下进行低温干燥，得到纯净的SDS插层蒙脱土粉末；(8) Purification of SDS-intercalated montmorillonite: add 0.5% to 0.8% of PAM flocculant dropwise to the SDS-intercalated modified montmorillonite suspension obtained in step (6), stir quickly and evenly, then carry out high-speed Centrifuge and filter, wash the filtered residue with deionized water until neutral, and then dry at low temperature at 60-80°C to obtain pure SDS intercalated montmorillonite powder;
（9）将步骤（8）制得的SDS插层蒙脱土粉末在450～550℃下高温焙烧30～45分钟，制得改性蒙脱土吸附剂。(9) calcining the SDS intercalated montmorillonite powder obtained in step (8) at a high temperature of 450-550° C. for 30-45 minutes to obtain a modified montmorillonite adsorbent.
作为优选，步骤（2）中，FN插层剂在制备过程中，将硝酸铁溶液在5分钟内匀速加入到氢氧化钠溶液中，并充分搅拌均匀，控制加入时的温度为60～80℃；Preferably, in step (2), during the preparation process of the FN intercalating agent, the ferric nitrate solution is added to the sodium hydroxide solution at a uniform speed within 5 minutes, and fully stirred evenly, and the temperature during the addition is controlled to be 60-80 ° C ;
作为优选，步骤（5）中，SDS插层剂在制备过程中，将十二烷基硫酸钠缓慢加入到硝酸中，溶解均匀后，将二者的混合溶液在5分钟内匀速加入到无水乙醇中，并充分搅拌均匀，控制加入时的温度为20～25℃；Preferably, in step (5), during the preparation process of the SDS intercalating agent, sodium dodecyl sulfate is slowly added to the nitric acid, and after uniform dissolution, the mixed solution of the two is added to the anhydrous solution at a uniform speed within 5 minutes. ethanol, and fully stir it evenly, and control the temperature during the addition to be 20-25°C;
作为优选，步骤（7）中，PAM絮凝剂在制备过程中，将聚丙烯酰胺缓慢加入到蒸馏水中，溶解均匀后，将二者的混合溶液在5分钟内匀速加入到硝酸中，并控制加入时的温度为20～25℃。Preferably, in step (7), during the preparation process of the PAM flocculant, polyacrylamide is slowly added to distilled water, and after it is uniformly dissolved, the mixed solution of the two is added to nitric acid at a uniform speed within 5 minutes, and the addition of controlled The temperature at that time is 20～25 ℃.
实施例1：Example 1:
对蒙脱土进行清洗、烘干、粉碎、过筛，选择粒径140～150 目的蒙脱石细粉材料，将该蒙脱石用蒸馏水制成固液质量比为0.1～0.2的悬浊液；用硝酸铁溶液、氢氧化钠溶液制备FN插层剂，在60℃恒温条件下，加入到蒙脱土悬浊液中进行无机改性；将FN插层改性蒙脱土悬浊液经离心、沉淀、清洗进行提纯后，与蒸馏水按固液质量比为0.1～0.2配制成FN插层蒙脱土悬浊液；用十二烷基硫酸钠、硝酸和无水乙醇制备SDS插层剂，加入到FN插层蒙脱土悬浊液中进行二次有机改性；用聚丙烯酰胺、硝酸和蒸馏水制备PAM絮凝剂，加入到SDS插层改性蒙脱土悬浊液中，快速搅拌、离心、过滤，并经清洗、干燥后在500℃下高温焙烧45分钟，制得改性蒙脱土吸附剂。The montmorillonite is cleaned, dried, pulverized and sieved, and the montmorillonite fine powder material with a particle size of 140-150 mesh is selected, and the montmorillonite is made into a suspension with a solid-liquid mass ratio of 0.1-0.2 with distilled water ; Prepare FN intercalating agent with ferric nitrate solution and sodium hydroxide solution, add it to montmorillonite suspension under constant temperature of 60 ℃ for inorganic modification; pass FN intercalation modified montmorillonite suspension through After purification by centrifugation, precipitation and washing, it is mixed with distilled water in a solid-liquid mass ratio of 0.1 to 0.2 to prepare a FN intercalated montmorillonite suspension; use sodium dodecyl sulfate, nitric acid and anhydrous ethanol to prepare SDS intercalating agent , added to FN intercalated montmorillonite suspension for secondary organic modification; PAM flocculant was prepared with polyacrylamide, nitric acid and distilled water, added to SDS intercalated modified montmorillonite suspension, stirred rapidly , centrifugation, filtration, and after washing and drying, the modified montmorillonite adsorbent was obtained by calcining at a high temperature of 500 ° C for 45 minutes.
本实施例中的废水采用硫酸锌和去离子水配制而成的硫酸锌溶液，通过检测后，其锌离子含量为465.14 mg·L-1。The wastewater in this example was a zinc sulfate solution prepared from zinc sulfate and deionized water. After testing, the zinc ion content was 465.14 mg·L -1 .
利用该方法得到的改性蒙脱土吸附剂对上述含锌废水（硫酸锌溶液）中锌离子的去除率为88.0％。The removal rate of zinc ions in the above-mentioned zinc-containing wastewater (zinc sulfate solution) by the modified montmorillonite adsorbent obtained by this method is 88.0%.
实施例2：Example 2:
对蒙脱土进行清洗、烘干、粉碎、过筛，选择粒径100～115 目的蒙脱石细粉材料，将该蒙脱石用蒸馏水制成固液质量比为0.1～0.2的悬浊液；用硝酸铁溶液、氢氧化钠溶液制备FN插层剂，在60℃恒温条件下，加入到蒙脱土悬浊液中进行无机改性；将FN插层改性蒙脱土悬浊液经离心、沉淀、清洗进行提纯后，与蒸馏水按固液质量比为0.1～0.2配制成FN插层蒙脱土悬浊液；用十二烷基硫酸钠、硝酸和无水乙醇制备SDS插层剂，加入到FN插层蒙脱土悬浊液中进行二次有机改性；用聚丙烯酰胺、硝酸和蒸馏水制备PAM絮凝剂，加入到SDS插层改性蒙脱土悬浊液中，快速搅拌、离心、过滤，并经清洗、干燥后在500℃下高温焙烧45分钟，制得改性蒙脱土吸附剂。The montmorillonite is cleaned, dried, pulverized and sieved, and the montmorillonite fine powder material with a particle size of 100-115 mesh is selected, and the montmorillonite is made into a suspension with a solid-liquid mass ratio of 0.1-0.2 with distilled water ; Prepare FN intercalating agent with ferric nitrate solution and sodium hydroxide solution, add it to montmorillonite suspension under constant temperature of 60 ℃ for inorganic modification; pass FN intercalation modified montmorillonite suspension through After purification by centrifugation, precipitation and washing, it is mixed with distilled water in a solid-liquid mass ratio of 0.1 to 0.2 to prepare a FN intercalated montmorillonite suspension; use sodium dodecyl sulfate, nitric acid and anhydrous ethanol to prepare SDS intercalating agent , added to FN intercalated montmorillonite suspension for secondary organic modification; PAM flocculant was prepared with polyacrylamide, nitric acid and distilled water, added to SDS intercalated modified montmorillonite suspension, stirred rapidly , centrifugation, filtration, and after washing and drying, the modified montmorillonite adsorbent was obtained by calcining at a high temperature of 500 ° C for 45 minutes.
本实施例中的废水采用硫酸锌和去离子水配制而成的硫酸锌溶液，通过检测后，其锌离子含量为465.14 mg·L-1。The wastewater in this example was a zinc sulfate solution prepared from zinc sulfate and deionized water. After testing, the zinc ion content was 465.14 mg·L -1 .
利用该方法得到的改性蒙脱土吸附剂对上述含锌废水（硫酸锌溶液）中锌离子的去除率为92.5％。The removal rate of zinc ions in the above-mentioned zinc-containing wastewater (zinc sulfate solution) by the modified montmorillonite adsorbent obtained by this method is 92.5%.
实施例3：Example 3:
对蒙脱土进行清洗、烘干、粉碎、过筛，选择粒径100～115 目的蒙脱石细粉材料，将该蒙脱石用蒸馏水制成固液质量比为0.1～0.2的悬浊液；用硝酸铁溶液、氢氧化钠溶液制备FN插层剂，在80℃恒温条件下，加入到蒙脱土悬浊液中进行无机改性；将FN插层改性蒙脱土悬浊液经离心、沉淀、清洗进行提纯后，与蒸馏水按固液质量比为0.1～0.2配制成FN插层蒙脱土悬浊液；用十二烷基硫酸钠、硝酸和无水乙醇制备SDS插层剂，加入到FN插层蒙脱土悬浊液中进行二次有机改性；用聚丙烯酰胺、硝酸和蒸馏水制备PAM絮凝剂，加入到SDS插层改性蒙脱土悬浊液中，快速搅拌、离心、过滤，并经清洗、干燥后在550℃下高温焙烧45分钟，制得改性蒙脱土吸附剂。The montmorillonite is cleaned, dried, pulverized and sieved, and the montmorillonite fine powder material with a particle size of 100-115 mesh is selected, and the montmorillonite is made into a suspension with a solid-liquid mass ratio of 0.1-0.2 with distilled water ; Prepare FN intercalation agent with ferric nitrate solution and sodium hydroxide solution, and add it to montmorillonite suspension under the constant temperature of 80 ℃ for inorganic modification; pass FN intercalation modified montmorillonite suspension through After purification by centrifugation, precipitation and washing, it is mixed with distilled water in a solid-liquid mass ratio of 0.1 to 0.2 to prepare a FN intercalated montmorillonite suspension; use sodium dodecyl sulfate, nitric acid and anhydrous ethanol to prepare SDS intercalating agent , added to FN intercalated montmorillonite suspension for secondary organic modification; PAM flocculant was prepared with polyacrylamide, nitric acid and distilled water, added to SDS intercalated modified montmorillonite suspension, stirred rapidly , centrifugation, filtration, and after washing and drying, the modified montmorillonite adsorbent was obtained by roasting at a high temperature of 550 ° C for 45 minutes.
本实施例中的废水采用硫酸锌和去离子水配制而成的硫酸锌溶液，通过检测后，其锌离子含量为465.14 mg·L-1。The wastewater in this example was a zinc sulfate solution prepared from zinc sulfate and deionized water. After testing, the zinc ion content was 465.14 mg·L -1 .
利用该方法得到的改性蒙脱土吸附剂对上述含锌废水（硫酸锌溶液）中锌离子的去除率为95.3％。The modified montmorillonite adsorbent obtained by this method has a removal rate of 95.3% for zinc ions in the above-mentioned zinc-containing wastewater (zinc sulfate solution).
上述本发明的制备方法，对于现今污水处理行业的技术人员来说具有较多可取之处，是一种技术创新，确实具有技术进步性。The above-mentioned preparation method of the present invention has many advantages for the technical personnel in the sewage treatment industry, and is a kind of technological innovation, which is indeed technologically progressive.
以上所述，仅是披露本发明的较佳实施例，并非对本发明作任何形式上的限制，任何熟悉本专业的技术人员，在不脱离本发明技术方案范围内，当可利用上述揭示的技术内容作出些许变动或修饰等同变化的等效实施例，但凡是未脱离本发明技术方案的内容，依据本发明的技术实质对以上实施例所作的任何简单修改、等同变化与修饰，均仍属于本发明技术方案的范围内。The above only discloses the preferred embodiments of the present invention, and does not limit the present invention in any form. Any person skilled in the art, without departing from the scope of the technical solution of the present invention, can use the technology disclosed above. The content is slightly changed or modified equivalent embodiments of equivalent changes, but all the content that does not depart from the technical solution of the present invention, any simple modifications, equivalent changes and modifications made to the above embodiments according to the technical essence of the present invention still belong to the present invention. within the scope of the technical solution of the invention.
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| 钠基膨润土插层改性的微结构与吸附机理;闫智超等;《环境工程学报》;20160930;第10卷(第9期);第4879-4886页 |
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