CN112934168A - 一种含镁硅胶复合材料及其制备方法与应用 - Google Patents
一种含镁硅胶复合材料及其制备方法与应用 Download PDFInfo
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- 239000000741 silica gel Substances 0.000 title claims abstract description 58
- 229910002027 silica gel Inorganic materials 0.000 title claims abstract description 58
- 239000011777 magnesium Substances 0.000 title claims abstract description 45
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 title claims abstract description 44
- 229910052749 magnesium Inorganic materials 0.000 title claims abstract description 44
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- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 28
- FPAFDBFIGPHWGO-UHFFFAOYSA-N dioxosilane;oxomagnesium;hydrate Chemical compound O.[Mg]=O.[Mg]=O.[Mg]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O FPAFDBFIGPHWGO-UHFFFAOYSA-N 0.000 claims description 15
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- 229910001862 magnesium hydroxide Inorganic materials 0.000 claims description 8
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- JLVVSXFLKOJNIY-UHFFFAOYSA-N Magnesium ion Chemical compound [Mg+2] JLVVSXFLKOJNIY-UHFFFAOYSA-N 0.000 claims description 7
- 229910001425 magnesium ion Inorganic materials 0.000 claims description 7
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 6
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- QWPPOHNGKGFGJK-UHFFFAOYSA-N hypochlorous acid Chemical compound ClO QWPPOHNGKGFGJK-UHFFFAOYSA-N 0.000 claims description 2
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- B01J20/103—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate comprising silica
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- B01J20/04—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of alkali metals, alkaline earth metals or magnesium
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Abstract
本发明公开了一种含镁硅胶复合材料及其制备方法,以及在重金属吸附中的应用;所述含镁硅胶复合材料的制备方法为:首先将黑滑石酸处理、固液分离,然后通过对固体液体的分别处理得到活化硅胶和含镁溶液,随后进行浸渍,从而实现对矿物材料的综合利用,得到含镁硅胶材料;本发明的优势在于,克服了传统的工艺对废液的浪费问题,同时增强了表面电荷以及提高了比表面积和孔隙率,制备的复合材料在提高吸附性能的同时,使用寿命得到了较好的提升,并且操作简单,耗材少,具有良好的应用前景。
Description
技术领域
本发明涉及一种通过对黑滑石综合利用制备的含镁硅胶复合材料,及其在重金属吸附方面的应用。
背景技术
金属电镀等工业废水处理不当,对环境造成污染,并导致重金属在生物体和人类中的积累。虽然一些重金属是重要的生物元素,但高剂量的重金属对人体有害。例如,高剂量的铜会导致呕吐和抽搐等健康危害,过量摄入铅会发生中毒,可以引起贫血症、神经功能失调及肾损伤,而且在体内不易排出,有蓄积性。因此,在排放到环境中之前,需要从废水中回收重金属。
重金属去除有多种处理方法,如吸附分离法、化学沉积法、溶剂萃取法、离子交换法、膜分离法等。其中,吸附法具有效率高、成本低、操作方便等优点。常用作吸附物的材料是硅胶、活性碳、分子筛、壳聚糖、沸石、粘土、离子交换树脂、活性氧化铝等。
粘土矿物已广泛用作水性介质中的吸附剂,用于去除大量不同的污染物。铜(II)进行阳离子交换是通过与表面羟基络合其中经过微晶带负电荷的表面达到附着在膨润土上的过程。其中MgO可以作为一个稳定缓冲器,最大限度地减少金属溶解度,避免再溶解。
到目前为止,人们已经通过热处理和化学处理等方法来改性粘土。其中,酸活化处理完的粘土与未处理的粘土相比,具有更好的孔隙分布和均匀的粒径,从而使其具有更高的吸附能力。酸活化处理通过溶解去除了表面杂质,以增大吸附容量,就材料表面而言,它在粘土材料的修饰方面表现出优势。为了提高降解性能,将金属物质(如氧化镁、氯化镁等)加入矿物材料中来产生的高表面电荷,改善酸性环境,以调整材料的基本性能。然而,这种复合方法也存在着一定问题,即粘土没有得到综合利用,产生大量废水急需处理等。
近年来,绿色环保的理念深入人心,同时也成为化学研究的理念,如何进一步开发利用矿石就成为一个重要的问题。目前,含镁硅胶材料作为良好的吸附材料,有较大的比表面积和良好的稳定性。以硅胶为中心的无极纳米系列材料因其具有极强的亲水性,不仅可以在水中具有强稳定性,其硅氧键还可以吸附重金属离子。但是,由于黑滑石的尝试研究仍有空白以及目前改性方法的局限性,通过黑滑石制备高性能的含镁硅胶系列的复合材料一直面临很大困难和挑战。
发明内容
本发明针对以上的不足,提供了一种基于黑滑石的复合材料及其制备方法,以及在重金属吸附方面的应用。本发明预先通过酸处理法,进行杂质的过滤以及黑滑石内部硅镁的分离,通过固液分离,将固体酸化、真空干燥得到硅胶,液体经pH的调节得到氯化镁母液,然后进行溶液浸渍、控温脱水,以达到镁基硅胶复合材料的均匀形成。
本发明改善了黑滑石矿石利用率低的问题,在构建含有硅胶材料的同时进行废液的回收利用,防止Mg的流失以及提高电荷,提高使用寿命和性能。
本发明的技术方案如下:
一种含镁硅胶复合材料,按如下方法制备得到:
(1)将黑滑石粉加入酸液中蚀刻20~30h(优选24h),之后离心(转速5000~10000r/min,优选10000r/min)分离,分别收集固体和液体,所得固体经水洗(1~4次,优选3次),干燥(放入烘箱在40~100℃下干燥),得到硅胶;
所述黑滑石粉粒径为300~400nm,由来源于江西广丰区的原料黑滑石,通过球磨机球磨,经粒径分析仪测定粒径后分级筛分获得;
所述酸液的浓度为1~12mol/L,优选6mol/L;酸选自盐酸、硫酸、醋酸、次氯酸中的至少一种;
所述黑滑石粉与酸的质量比为1:0.1~10,优选1:0.5;
(2)在步骤(1)离心分离得到的液体中加入碱性化合物调节pH至5~8(优选7),得到浸渍液,将步骤(1)所得硅胶在真空干燥下活化后,加入所得浸渍液中浸渍12~24h(优选12h),之后烘干(100~200℃,优选150℃),得到所述含镁硅胶复合材料;
所述碱性化合物选自氢氧化镁、氢氧化钠、氢氧化铁、氨水、氢氧化铝、熟石灰中的至少一种,优选氢氧化镁;
所述硅胶真空干燥的温度为100~150℃(优选130℃),时间为6~24h;
活化后硅胶与浸渍液中镁离子的质量比为1:0.005~0.1,优选1:0.008;浸渍液中镁离子的浓度可由原子吸收法测定。
本发明制得的含镁硅胶复合材料可应用于重金属吸附,应用方法例如:
将所述含镁硅胶复合材料加入重金属溶液中进行吸附;
所述含镁硅胶复合材料和重金属的质量比为1:0.1~10,优选1:0.2;
所述重金属为As(III)、As(V)、Cd(II)、Cu(II)、Pb(II)中的至少一种。
与现有技术相比,本发明的有益效果在于:
本发明克服了传统工艺对废液的浪费问题,将黑滑石进一步回收利用,以达到提高性能的目的;通过调控反应的pH,可以调控吸附位点的数目,从而可以间接控制颗粒的大小,以及孔隙率,实现精确控制。制备的含镁硅胶颗粒在提高使用寿命的同时,由于其MgO能分散电子,可以提高分散性能和吸附性能,同时方法简单,易操作,具有广阔的应用前景。
附图说明
图1为实施例1中黑滑石粉末未处理前的扫描电镜图。
图2为实施例1中黑滑石综合利用制备的含镁硅胶材料的扫描电镜图。
图3为实施例1中黑滑石综合利用制备的含镁硅胶材料的扫描电镜图。
具体实施方式
下面通过具体实施例进一步描述本发明,但本发明的保护范围并不仅限于此。
以下实施例中,原料黑滑石来源于江西广丰区,粒径为300~400nm的黑滑石粉通过以下方法制备得到:首先通过球磨机球磨30~60min,再经粒径分析仪测定粒径后分级筛分,最终得到粒径为300~400nm的黑滑石粉。
同时,300~400nm的白滑石(江西广丰)、珍珠岩(江西广丰)、膨润土(江西广丰)均用此法得到。
实施例1制备黑滑石复合吸附材料
A.(Mg-黑滑石)含镁硅胶材料的制备:
(1)取粒径为300-400nm的黑滑石粉50g加入6mol/L的盐酸69.5ml(盐酸的质量分数为36%)蚀刻24h,用离心机离心,转速为10000r/min,用水洗3次,放入烘箱在40-100℃
下干燥,得到黑色颗粒65g。
(2)将通过离心机得到的溶液,加氢氧化镁调节pH至7,取样测试镁离子浓度为40mg/L,取溶液100mL,将步骤1得到的硅胶取0.5g在真空干燥下活化,所用温度为130℃,时间为12h,反应完成后,倒入调节后的溶液中浸渍12h,放入烘箱在150℃下干燥,
得到含镁硅胶氧化物3g。
(3)取步骤(2)所述的含镁硅胶颗粒100mg,溶于100mL的硝酸铜溶液(离子浓度为200mg/L)中,进行吸附性能测试,在两小时内吸附含量为100mg/g。
B.仅含硅胶材料的制备:
(1)取粒径为300-400nm的黑滑石粉50g加入6mol/L的盐酸69.5ml(盐酸的质量分数为36%)蚀刻24h,用离心机离心,转速为10000r/min,用水洗3次,放入烘箱在40-100℃下干燥,得到黑色颗粒63g。
(2)将步骤1得到的硅胶取0.5g在真空干燥下活化,所用温度为130℃,时间为12h,得到硅胶材料0.49g。
(3)取步骤(2)所述的硅胶颗粒100mg,溶于100mL的硝酸铜溶液(离子浓度为200mg/L)中,进行吸附性能测试,在两小时内吸附含量为60mg/g。
C.镁基材料的制备:
(1)取粒径为300-400nm的黑滑石粉50g加入6mol/L的盐酸69.5ml(盐酸的质量分数为36%)蚀刻24h,用离心机离心,转速为10000r/min,得到上层清液65mL。
(2)将通过离心机得到的溶液,加氢氧化镁调节pH至7,取样测试镁离子浓度为40.1mg/L,取溶液3.33mL,溶于100mL的硝酸铜溶液(离子浓度为200mg/L)中,进行吸附性能测试,在两小时内吸附含量为0.1mg/g。
D.(Mg-其他滑石)含镁硅胶材料的制备
(1)取粒径为300-400nm的白滑石粉、珍珠岩粉、膨润土粉50g加入6mol/L的盐酸69.5ml(盐酸的质量分数为36%)蚀刻24h,用离心机离心,转速为10000r/min,用水洗3次,放入烘箱在40-100℃下干燥,得到黑色颗粒63g。
(2)将通过离心机得到的溶液,加氢氧化镁调节pH至7,取样测试镁离子浓度为5mg/L、3mg/L、10mg/L,取溶液100.5mL,将步骤1得到的硅胶取0.5g在真空干燥下活化,所用温度为130℃,时间为12h,反应完成后,倒入调节后的溶液中浸渍12h,放入烘箱在150℃下干燥,得到含镁硅胶氧化物2.3g、2.5g、2.8g。
(3)取步骤(2)所述的含镁硅胶颗粒各100mg,溶于100mL的硝酸铜溶液(离子浓度为200mg/L)中,进行吸附性能测试,在两小时内吸附含量为90mg/g、88mg/g、85mg/g。
实施例2制备不同比例含镁硅胶材料
(1)取粒径为300-400nm的黑滑石粉50g加入6mol/L的盐酸69.5ml(盐酸的质量分数为36%)蚀刻24h,用离心机离心,转速为10000r/min,用水洗3次,放入烘箱在40-100℃下干燥,得到黑色颗粒64g。
(2)将通过离心机得到的溶液,加氢氧化镁调节pH至7,取样测试镁离子浓度为40mg/L,取溶液50mL、100mL、200mL,将步骤1得到的硅胶取0.5g在真空干燥下活化,所用温度为130℃,时间为12h,反应完成后,倒入调节后的溶液中浸渍12h,放入在150℃下干燥,得到含镁硅胶氧化物1.7g、2.9g、4.8g。
(3)取步骤(2)所述的含镁硅胶颗粒各100mg,溶于100mL的硝酸铜溶液(离子浓度为200mg/L)中,进行吸附性能测试,在两小时内吸附含量为60mg/g、106mg/g、85mg/g。
实施例3制备不同pH的硅胶材料
(1)取粒径为300-400nm的黑滑石粉50g加入6mol/L的盐酸69.5ml(盐酸的质量分数为36%)蚀刻24h,用离心机离心,转速为10000r/min,用水洗3次,放入烘箱在40-100℃下干燥,得到黑色颗粒65g。
(2)将通过离心机得到的溶液,加氢氧化镁调节pH至5、6、7,取样镁测试离子浓度为15mg/L、25mg/L、38mg/L,取溶液266.7mL、160mL、105.3mL,将步骤1得到的硅胶取0.5g在真空干燥下活化,所用温度为130℃,时间为12h,反应完成后,倒入调节后的溶液中浸渍12h,放入烘箱在150℃下干燥,得到含镁硅胶氧化物2.7g、2.4g、3.1g。
(3)取步骤(2)所述的含镁硅胶颗粒各100mg,溶于100mL的硝酸铜溶液(离子浓度为200mg/L)中,进行吸附性能测试,在两小时内吸附含量为90mg/g、88mg/g、95mg/g。
Claims (9)
1.一种含镁硅胶复合材料,其特征在于,按如下方法制备得到:
(1)将黑滑石粉加入酸液中蚀刻20~30h,之后离心分离,分别收集固体和液体,所得固体经水洗,干燥,得到硅胶;
(2)在步骤(1)离心分离得到的液体中加入碱性化合物调节pH至5~8,得到浸渍液,将步骤(1)所得硅胶在真空干燥下活化后,加入所得浸渍液中浸渍12~24h,之后烘干,得到所述含镁硅胶复合材料。
2.如权利要求1所述含镁硅胶复合材料,其特征在于,步骤(1)中,所述黑滑石粉粒径为300~400nm。
3.如权利要求1所述含镁硅胶复合材料,其特征在于,步骤(1)中,所述酸液的浓度为1~12mol/L;酸选自盐酸、硫酸、醋酸、次氯酸中的至少一种。
4.如权利要求1所述含镁硅胶复合材料,其特征在于,步骤(1)中,所述黑滑石粉与酸的质量比为1:0.1~10。
5.如权利要求1所述含镁硅胶复合材料,其特征在于,步骤(2)中,所述碱性化合物选自氢氧化镁、氢氧化钠、氢氧化铁、氨水、氢氧化铝、熟石灰中的至少一种。
6.如权利要求1所述含镁硅胶复合材料,其特征在于,步骤(2)中,所述硅胶真空干燥的温度为100~150℃,时间为6~24h。
7.如权利要求1所述含镁硅胶复合材料,其特征在于,步骤(2)中,活化后硅胶与浸渍液中镁离子的质量比为1:0.005~0.1。
8.如权利要求1所述含镁硅胶复合材料在重金属吸附中的应用。
9.如权利要求8所述的应用,其特征在于,应用方法为:
将所述含镁硅胶复合材料加入重金属溶液中进行吸附;
所述含镁硅胶复合材料和重金属的质量比为1:0.1~10;
所述重金属为As(III)、As(V)、Cd(II)、Cu(II)、Pb(II)中的至少一种。
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Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN114288985A (zh) * | 2021-12-29 | 2022-04-08 | 浙江工业大学 | 一种黑滑石吸附材料及其制备方法与应用 |
CN115624951A (zh) * | 2022-10-31 | 2023-01-20 | 苏州北美国际高级中学 | 一种钴离子快速富集材料及制备方法 |
CN115715970A (zh) * | 2022-11-18 | 2023-02-28 | 浙江工业大学 | 一种黑滑石基纳米矿晶及其制备方法 |
Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN102908978A (zh) * | 2012-11-12 | 2013-02-06 | 江西理工大学 | 原位反应制备高效吸附剂 |
CN108854941A (zh) * | 2018-05-25 | 2018-11-23 | 陕西科技大学 | 一种基于海泡石制备的含镁纳米复合材料及其制备方法 |
CN110475608A (zh) * | 2017-03-30 | 2019-11-19 | 水泽化学工业株式会社 | 重金属吸附剂 |
-
2021
- 2021-02-08 CN CN202110172213.2A patent/CN112934168A/zh active Pending
Patent Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN102908978A (zh) * | 2012-11-12 | 2013-02-06 | 江西理工大学 | 原位反应制备高效吸附剂 |
CN110475608A (zh) * | 2017-03-30 | 2019-11-19 | 水泽化学工业株式会社 | 重金属吸附剂 |
CN108854941A (zh) * | 2018-05-25 | 2018-11-23 | 陕西科技大学 | 一种基于海泡石制备的含镁纳米复合材料及其制备方法 |
Non-Patent Citations (1)
Title |
---|
《矿产资源工业要求手册》编委会编: "矿产资源工业要求手册", 《矿产资源工业要求手册》 * |
Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN114288985A (zh) * | 2021-12-29 | 2022-04-08 | 浙江工业大学 | 一种黑滑石吸附材料及其制备方法与应用 |
CN115624951A (zh) * | 2022-10-31 | 2023-01-20 | 苏州北美国际高级中学 | 一种钴离子快速富集材料及制备方法 |
CN115624951B (zh) * | 2022-10-31 | 2024-05-28 | 苏州北美国际高级中学 | 一种钴离子快速富集材料及制备方法 |
CN115715970A (zh) * | 2022-11-18 | 2023-02-28 | 浙江工业大学 | 一种黑滑石基纳米矿晶及其制备方法 |
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