CN112221475B - 一种吸附土壤中Ni的材料 - Google Patents
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- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 18
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 15
- 239000000047 product Substances 0.000 claims description 13
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 12
- 239000011324 bead Substances 0.000 claims description 11
- OZAIFHULBGXAKX-UHFFFAOYSA-N 2-(2-cyanopropan-2-yldiazenyl)-2-methylpropanenitrile Chemical compound N#CC(C)(C)N=NC(C)(C)C#N OZAIFHULBGXAKX-UHFFFAOYSA-N 0.000 claims description 9
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 claims description 9
- 239000002245 particle Substances 0.000 claims description 9
- 238000001914 filtration Methods 0.000 claims description 7
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- HGINCPLSRVDWNT-UHFFFAOYSA-N Acrolein Chemical compound C=CC=O HGINCPLSRVDWNT-UHFFFAOYSA-N 0.000 claims description 6
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- AWJUIBRHMBBTKR-UHFFFAOYSA-N isoquinoline Chemical compound C1=NC=CC2=CC=CC=C21 AWJUIBRHMBBTKR-UHFFFAOYSA-N 0.000 claims description 6
- 229910052757 nitrogen Inorganic materials 0.000 claims description 6
- MYRTYDVEIRVNKP-UHFFFAOYSA-N 1,2-Divinylbenzene Chemical compound C=CC1=CC=CC=C1C=C MYRTYDVEIRVNKP-UHFFFAOYSA-N 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
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- CSNNHWWHGAXBCP-UHFFFAOYSA-L Magnesium sulfate Chemical compound [Mg+2].[O-][S+2]([O-])([O-])[O-] CSNNHWWHGAXBCP-UHFFFAOYSA-L 0.000 claims description 3
- 229910002092 carbon dioxide Inorganic materials 0.000 claims description 3
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- CUONGYYJJVDODC-UHFFFAOYSA-N malononitrile Chemical compound N#CCC#N CUONGYYJJVDODC-UHFFFAOYSA-N 0.000 claims description 3
- 239000003208 petroleum Substances 0.000 claims description 3
- 238000002360 preparation method Methods 0.000 claims description 3
- AKHNMLFCWUSKQB-UHFFFAOYSA-L sodium thiosulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=S AKHNMLFCWUSKQB-UHFFFAOYSA-L 0.000 claims description 3
- 235000019345 sodium thiosulphate Nutrition 0.000 claims description 3
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- 238000001035 drying Methods 0.000 claims description 2
- 238000010438 heat treatment Methods 0.000 claims description 2
- 239000004088 foaming agent Substances 0.000 claims 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical class [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims 1
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- 239000003344 environmental pollutant Substances 0.000 abstract description 4
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- 239000000919 ceramic Substances 0.000 abstract description 2
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- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 15
- 229910052759 nickel Inorganic materials 0.000 description 7
- 239000004604 Blowing Agent Substances 0.000 description 4
- 239000000203 mixture Substances 0.000 description 3
- 238000005033 Fourier transform infrared spectroscopy Methods 0.000 description 2
- 229910021586 Nickel(II) chloride Inorganic materials 0.000 description 2
- 238000000921 elemental analysis Methods 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 238000000227 grinding Methods 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 description 2
- HPALAKNZSZLMCH-UHFFFAOYSA-M sodium;chloride;hydrate Chemical class O.[Na+].[Cl-] HPALAKNZSZLMCH-UHFFFAOYSA-M 0.000 description 2
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- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 1
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- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 238000003321 atomic absorption spectrophotometry Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 239000003480 eluent Substances 0.000 description 1
- 239000003112 inhibitor Substances 0.000 description 1
- HPIGCVXMBGOWTF-UHFFFAOYSA-N isomaltol Natural products CC(=O)C=1OC=CC=1O HPIGCVXMBGOWTF-UHFFFAOYSA-N 0.000 description 1
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- 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
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/26—Synthetic macromolecular compounds
- B01J20/262—Synthetic macromolecular compounds obtained otherwise than by reactions only involving carbon to carbon unsaturated bonds, e.g. obtained by polycondensation
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- B—PERFORMING OPERATIONS; TRANSPORTING
- 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
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28014—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their form
- B01J20/28016—Particle form
- B01J20/28019—Spherical, ellipsoidal or cylindrical
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B09—DISPOSAL OF SOLID WASTE; RECLAMATION OF CONTAMINATED SOIL
- B09C—RECLAMATION OF CONTAMINATED SOIL
- B09C1/00—Reclamation of contaminated soil
- B09C1/08—Reclamation of contaminated soil chemically
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- Chemical Kinetics & Catalysis (AREA)
- Life Sciences & Earth Sciences (AREA)
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- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
- Processing Of Solid Wastes (AREA)
Abstract
土壤重金属污染物来源广泛，包括电镀、电池、电解、采矿、冶炼、农药、医药、油漆、颜料、五金、机械、化妆品、陶瓷、化工等众多行业。吸附是常用的去除重金属的方法。然而现有的吸附材料的吸附容量普遍较小。本申请合成了一种新材料，对土壤中的重金属Ni具有较高的吸附容量。
Description
技术领域
本发明属于污染修复/治理领域，公开了一种吸附土壤中重金属Ni2+的聚合物材料及其合成方法。
背景技术
土壤重金属污染物来源广泛，包括电镀、电池、电解、采矿、冶炼、农药、医药、油漆、颜料、五金、机械、化妆品、陶瓷、化工等众多行业。吸附是常用的去除重金属的方法。然而现有的吸附材料的吸附容量普遍较小。因此，需要一种能够大量吸附土壤重金属的新材料。
发明内容
本申请是一种高效吸附土壤中Ni的材料，结构式如下:
其制备方法如下：
1)向溶剂二氯甲烷中加入以下四组分：丙二腈，丙烯醛，异喹啉和异氰环已烷，四组分摩尔比1:1:1:1，室温下搅拌24小时。然后5％硫代硫酸钠水溶液洗涤，然后用饱和食盐水洗涤，然后无水硫酸镁干燥过滤，滤液真空干燥，干燥物通过快速柱层析纯化，淋洗剂为体积比＝1:1的乙酸乙酯/石油醚，得到中间体。
2)玻璃反应器中，加入溶剂乙酸乙酯，然后加入以下组分：对二乙烯基苯、前述中间体，二组分的摩尔比为1:1，搅拌，将溶液以氮气脱气，然后加入0.15g偶氮二异丁腈(AIBN)引发剂，氮气流下，80℃加热搅拌24小时。冷却至室温，然后在乙醚中沉降，过滤，过滤得到的固体微粒使用乙醇洗涤。真空干燥，得到白色微粒。上述100重量份白色微粒经加料口加入单螺杆挤出机中，控制口模温度100℃，压力为11MPa。通过安装在挤出机机筒上的发泡剂注入口注入15重量份发泡剂液态二氧化碳。然后经直径3mm的圆孔口模挤出、切粒、冷却得到产物发泡珠粒，产物用于吸附土壤中重金属Ni，具有较高的吸附容量。
附图说明：
附图1为本申请产物珠粒的FTIR结果。
具体实施方式：
实施例1(制备实验)：
向200mL溶剂二氯甲烷中加入以下四组分：0.05mol丙二腈(99％，常州市弘裕化工有限公司)，然后加入丙烯醛(99％，山东喜玛供应链管理有限公司)，异喹啉(98％，武汉荣灿生物科技有限公司)和异氰环已烷(98％，江苏艾康生物医药研发有限公司)，四组分摩尔比1:1:1:1，室温下搅拌24小时。然后5％硫代硫酸钠水溶液洗涤，然后用饱和食盐水洗涤，然后无水硫酸镁干燥过滤，滤液真空干燥，干燥物通过快速柱层析(淋洗剂为乙酸乙酯/石油醚＝1:1，体积比)纯化得到中间体，收率96.1％，反应式如下：
中间体元素分析(％)计算值：C,77.16；H,6.48；N,16.36。测定值：C,77.09；H,6.50；N,16.41。IR(KBr，cm-1)：728、764、787、921、991、1379、1457、1547、1601、1638(C＝N)、1837乙烯、2244C＝-N、2917、2940、3041、3461。
250ml玻璃反应器中，加入100mL溶剂乙酸乙酯，0.04mol对二乙烯基苯(DVB，98％，郑州杰克斯化工产品有限公司，使用前先用中性氧化铝过滤除去阻聚剂)和0.04mol前述中间体，搅拌，将溶液以氮气脱气5分钟，然后加入0.15g偶氮二异丁腈(AIBN)引发剂，氮气流下，80℃加热搅拌24小时。冷却至室温，然后在乙醚中沉降，过滤，过滤得到的固体微粒使用乙醇洗涤3次。真空干燥，得到白色微粒。
上述100重量份白色微粒经加料口加入单螺杆挤出机中，控制口模温度100℃，压力为11MPa。通过安装在挤出机机筒上的发泡剂注入口注入15重量份发泡剂液态二氧化碳。然后经直径3mm的圆孔口模挤出、切粒、冷却得到产物发泡珠粒，收率96.1％，产物结构式如下。元素分析(％)计算值：C,80.63；H,7.61；N,11.75。测定值：C,80.51；H,7.66；N,11.83。
产物结构式：
附图1为本申请产物珠粒的FTIR结果。
实施例2(Ni2+吸附实验)：
采集野外无污染土壤，为砂壤土，风干碾细后过2mm筛。称取2kg上述过筛的无污染土样，将NiCl2(优级纯)碾磨粉碎，加入土中配得0.5gNi/kg的土样，混合均匀，并按照GB/T17139-1997《土壤质量-镍的测定》测得土中镍含量0.5±0.05gNi/kg土。然后称取1kg上述含镍土样放入3L锥形瓶中，然后加入1L去离子水，最后加入1g本申请产物发泡珠粒，室温下30rpm振荡。60分钟后，停止震荡，手工取出全部发泡珠粒，风干发泡珠粒，然后按照HJ751-2015《固体废物-镍、铜的测定：火焰原子吸收分光光度法》检测风干的发泡珠粒的镍含量即吸附量，测得发泡珠粒对镍的吸附量为0.23 7g镍/g珠粒。
Claims (1)
1.一种高效吸附土壤中Ni的材料，结构式如下:
其制备方法如下：
1)向溶剂二氯甲烷中加入以下四组分：丙二腈，丙烯醛，异喹啉和异氰环已烷，四组分摩尔比1:1:1:1，室温下搅拌24小时；然后使用5％硫代硫酸钠水溶液洗涤，然后用饱和食盐水洗涤，然后无水硫酸镁干燥过滤，滤液真空干燥，干燥物通过快速柱层析纯化，淋洗剂为体积比＝1:1的乙酸乙酯/石油醚，得到中间体；2)玻璃反应器中，加入溶剂乙酸乙酯，然后加入以下组分：对二乙烯基苯、前述中间体，二组分的摩尔比为1:1，搅拌，将溶液以氮气脱气，然后加入0.15g偶氮二异丁腈引发剂，氮气流下，80℃加热搅拌24小时，然后冷却至室温，然后在乙醚中沉降，过滤，过滤得到的固体微粒使用乙醇洗涤；真空干燥，得到白色微粒；上述100重量份白色微粒经加料口加入单螺杆挤出机中，控制口模温度100℃，压力为11MPa；通过安装在挤出机机筒上的发泡剂注入口注入15重量份发泡剂液态二氧化碳；然后经直径3mm的圆孔口模挤出、切粒、冷却得到产物发泡珠粒，产物用于吸附土壤中重金属Ni，具有较高的吸附容量。
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| 不同催化剂条件下芳香醛与丙二睛Knoevenagel固相反应的研究;王海燕;《山东化工》;20131231;第42卷;第32-34页 * |
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