CN112791727A - 一种磁性NixZn(1-x)Fe2O4气凝胶的制备方法 - Google Patents
一种磁性NixZn(1-x)Fe2O4气凝胶的制备方法 Download PDFInfo
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- 235000019441 ethanol Nutrition 0.000 claims description 8
- 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 claims description 8
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- ONDPHDOFVYQSGI-UHFFFAOYSA-N zinc nitrate Chemical compound [Zn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ONDPHDOFVYQSGI-UHFFFAOYSA-N 0.000 claims description 6
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- 239000003795 chemical substances by application Substances 0.000 claims description 4
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims description 4
- KBJMLQFLOWQJNF-UHFFFAOYSA-N nickel(ii) nitrate Chemical compound [Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O KBJMLQFLOWQJNF-UHFFFAOYSA-N 0.000 claims description 4
- 239000011592 zinc chloride Substances 0.000 claims description 4
- 235000005074 zinc chloride Nutrition 0.000 claims description 4
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- 229910021586 Nickel(II) chloride Inorganic materials 0.000 claims description 3
- MQRWBMAEBQOWAF-UHFFFAOYSA-N acetic acid;nickel Chemical compound [Ni].CC(O)=O.CC(O)=O MQRWBMAEBQOWAF-UHFFFAOYSA-N 0.000 claims description 3
- ZOIORXHNWRGPMV-UHFFFAOYSA-N acetic acid;zinc Chemical compound [Zn].CC(O)=O.CC(O)=O ZOIORXHNWRGPMV-UHFFFAOYSA-N 0.000 claims description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 3
- 229940078494 nickel acetate Drugs 0.000 claims description 3
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 claims description 3
- 239000001301 oxygen Substances 0.000 claims description 3
- 229910052760 oxygen Inorganic materials 0.000 claims description 3
- 239000004246 zinc acetate Substances 0.000 claims description 3
- BRLQWZUYTZBJKN-UHFFFAOYSA-N Epichlorohydrin Chemical compound ClCC1CO1 BRLQWZUYTZBJKN-UHFFFAOYSA-N 0.000 claims description 2
- 238000006243 chemical reaction Methods 0.000 claims description 2
- 239000007789 gas Substances 0.000 claims description 2
- PVFSDGKDKFSOTB-UHFFFAOYSA-K iron(3+);triacetate Chemical compound [Fe+3].CC([O-])=O.CC([O-])=O.CC([O-])=O PVFSDGKDKFSOTB-UHFFFAOYSA-K 0.000 claims description 2
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- PYWVYCXTNDRMGF-UHFFFAOYSA-N rhodamine B Chemical compound [Cl-].C=12C=CC(=[N+](CC)CC)C=C2OC2=CC(N(CC)CC)=CC=C2C=1C1=CC=CC=C1C(O)=O PYWVYCXTNDRMGF-UHFFFAOYSA-N 0.000 description 4
- 229940043267 rhodamine b Drugs 0.000 description 4
- 230000005389 magnetism Effects 0.000 description 3
- 229910003264 NiFe2O4 Inorganic materials 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
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- WGEATSXPYVGFCC-UHFFFAOYSA-N zinc ferrite Chemical compound O=[Zn].O=[Fe]O[Fe]=O WGEATSXPYVGFCC-UHFFFAOYSA-N 0.000 description 1
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- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/76—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/80—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with zinc, cadmium or mercury
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Abstract
本发明涉及一种磁性NixZn(1‑x)Fe2O4气凝胶的制备方法,属于复合材料制备工艺技术领域。通过将铁源、锌源、镍源、去离子水和乙醇搅拌至澄清溶液,再向溶液中加入一定量质子去除剂,得到NixZn(1‑x)Fe2O4气凝胶溶胶,一定温度下静置凝胶并老化和溶剂置换。采用乙醇超临界干燥、高温热处理等工艺,最终得到NixZn(1‑x)Fe2O4气凝胶。本发明制备出的NixZn(1‑x)Fe2O4气凝胶不仅能在可见光条件下产生光生电子空穴对从而提高光催化效率,而且镍元素的掺入显著提高了光催化剂的磁化强度,有利于回收再利用,在光催化降解污染物方面将具有很好的应用前景和无限的潜力。
Description
技术领域
本发明属于具有光催化降解污染物无机纳米材料制备的技术领域,具体涉及一种磁性NixZn(1-x)Fe2O4气凝胶的制备方法。
背景技术
随着科学技术的不断进步以及化工产品的过度使用,日益严重的环境污染已经成了人们不得不面对的严峻问题。诸如二氧化钛一类的光催化剂可以将吸收的光能转化为化学能并用于污染物处理和清洁能源生产,被认为是解决环境污染和能源危机最有环保有效的方法之一。但目前商用光催化剂大多只能在紫外光照射下才能起作用,太阳光利用率低进而导致催化效率低,而且,大多数光催化剂降解污染物是分散在含有污染物的溶液中使用的,这也导致催化剂难以回收重复再利用。因此,急需一种能在可见光下产生激发并具有强磁性、易回收的光催化材料来解决以上问题。
发明内容
本发明的目的是为了改善目前商用光催化剂太阳光利用率低以及难以回收等缺点而提供一种具有可见光催化活性和较高磁化强度的磁性NixZn(1-x)Fe2O4气凝胶的制备方法。
本发明的技术方案为:一种磁性NixZn(1-x)Fe2O4气凝胶的制备方法,其具体步骤如下:
(1)按NixZn(1-x)Fe2O4(X为0~1)的化学计量比称取铁源、锌源、镍源,然后将铁源、锌源、镍源、去离子水和无水乙醇按摩尔比例为1:(0~0.5):(0~0.5):(40~60):(15~20)混合搅拌,得到澄清混合溶液;
(2)向澄清混合溶液中加入质子去除剂,混合搅拌后倒入模具,20~50℃下等待凝胶;
(3)将步骤(2)中得到的湿凝胶在20~25℃下静置8~12h;
(4)将步骤(3)中静置后的湿凝胶再在烘箱中老化,期间进行溶剂置换;
(5)将步骤(4)中溶剂置换后的复合湿凝胶进行乙醇超临界干燥处理,其中乙醇超临界干燥法采用N2气体保护,干燥温度为255~275℃,高压反应釜压力控制在10~12MPa,反应时间为2~4h;
(6)将步骤(5)中得到的气凝胶进行高温热处理,热处理温度为300~900℃,升温速率为2~4℃/min,保温时间为2~4h,自然冷却至室温,得到NixZn(1-x)Fe2O4气凝胶。
优选步骤(1)中铁源为氯化铁、硝酸铁或乙酸铁的一种;锌源为氯化锌、硝酸锌或乙酸锌的一种;镍源为氯化镍、硝酸镍或乙酸镍的一种。
优选步骤(1)中混合搅拌的时间为20~30min。
优选步骤(2)中混合搅拌的时间为2~5min。
优选步骤(2)中质子去除剂为环氧丙烷、环氧乙烷或环氧氯丙烷的一种,铁源和质子去除剂按摩尔比例为1:(5~10)。
优选步骤(4)中所述的溶剂置换为无水乙醇进行溶剂置换,每6~9h更换一次,总共置换6~8次。
优选步骤(4)中烘箱的温度为40~60℃。
优选步骤(6)中高温热处理气氛为空气或者氧气的一种。
有益效果:
(1)太阳光利用率高,催化效率高。NixZn(1-x)Fe2O4气凝胶基于铁酸锌光催化剂改性而来,可在可见光下产生光生电子空穴对,极大的提高了太阳光的利用率,进而提高催化效率。
(2)磁性强,可回收再利用。镍元素的掺入显著提高了NixZn(1-x)Fe2O4气凝胶的磁性,可实现高效的回收再利用。
附图说明
图1为实施例1制备的NixZn(1-x)Fe2O4气凝胶材料的实物照片。
图2为不同锌镍配比的NixZn(1-x)Fe2O4气凝胶材料的磁滞回线。
具体实施方式
实例1
将1mol氯化铁、0mol氯化锌、0.5mol氯化镍、40mol去离子水和15mol无水乙醇均匀搅拌20min,然后向混合溶液中加入5mol的环氧乙烷,混合搅拌2min后倒入模具,20℃下等待凝胶。将湿凝胶在20℃下静置8h后放在40℃的烘箱内。期间使用无水乙醇置换湿凝胶中的杂质离子,置换6次,每次6h。再将复合湿凝胶放入高温高压釜中,利用乙醇超临界干燥法对样品进行干燥,其中压力控制在10MPa,控制温度在255℃,超临界干燥时间为2h。然后将样品在氧气气氛下以2℃/min的升温速率加热至300℃,保温时间为2h,冷却至室温后得到NiFe2O4气凝胶。实物照片如图1所示,成功制备了低密度、整体式的气凝胶光催化材料。经过测试发现:制得的NiFe2O4气凝胶的磁化强度为70emu/g,50mg催化剂在可见光下照射10mg/L的100ml罗丹明B溶液,1h的降解率为52.44%。
实例2
将1mol硝酸铁、0.5mol硝酸锌、0mol硝酸镍、60mol去离子水和20mol无水乙醇均匀搅拌30min,然后向混合溶液中加入10mol的环氧丙烷,混合搅拌5min后倒入模具,50℃下等待凝胶。将湿凝胶在25℃下静置12h后放在60℃的烘箱内。期间使用无水乙醇置换湿凝胶中的杂质离子,置换8次,每次9h。再将复合湿凝胶放入高温高压釜中,利用乙醇超临界干燥法对样品进行干燥,其中压力控制在12MPa,控制温度在275℃,超临界干燥时间为4h。然后将样品在空气气氛下以4℃/min的升温速率加热至900℃,保温时间为4h,冷却至室温后得到ZnFe2O4气凝胶。经过测试发现:制得的ZnFe2O4气凝胶的磁化强度为49emu/g,50mg催化剂在可见光下照射10mg/L的100ml罗丹明B溶液,1h的降解率为50.89%。
实例3
将1mol氯化铁、0.1mol乙酸锌、0.4mol硝酸镍、45mol去离子水和16mol无水乙醇均匀搅拌24min,然后向混合溶液中加入7mol的环氧氯丙烷,混合搅拌3min后倒入模具,30℃下等待凝胶。将湿凝胶在22℃下静置9h后放在45℃的烘箱内。期间使用无水乙醇置换湿凝胶中的杂质离子,置换7次,每次7h。再将复合湿凝胶放入高温高压釜中,利用乙醇超临界干燥法对样品进行干燥,其中压力控制在11MPa,控制温度在260℃,超临界干燥时间为2.5h。然后将样品在空气气氛下以3℃/min的升温速率加热至450℃,保温时间为3h,冷却至室温后得到Ni0.8Zn0.2Fe2O4气凝胶。经过测试发现:制得的Ni0.8Zn0.2Fe2O4气凝胶的磁化强度为102emu/g,50mg催化剂在可见光下照射10mg/L的100ml罗丹明B溶液,1h的降解率为55.71%。
实例4
将1mol硝酸铁、0.2mol氯化锌、0.3mol乙酸镍、50mol去离子水和18mol无水乙醇均匀搅拌28min,然后向混合溶液中加入8.5mol的环氧丙烷,混合搅拌4min后倒入模具,40℃下等待凝胶。将湿凝胶在24℃下静置10h后放在50℃的烘箱内。期间使用无水乙醇置换湿凝胶中的杂质离子,置换8次,每次8h。再将复合湿凝胶放入高温高压釜中,利用乙醇超临界干燥法对样品进行干燥,其中压力控制在10MPa,控制温度在270℃,超临界干燥时间为3h。然后将样品在空气气氛下以2.5℃/min的升温速率加热至600℃,保温时间为2.5h,冷却至室温后得到Ni0.6Zn0.4Fe2O4气凝胶。经过测试发现:制得的Ni0.6Zn0.4Fe2O4气凝胶的磁化强度为89emu/g,50mg催化剂在可见光下照射10mg/L的100ml罗丹明B溶液,1h的降解率为58.80%。
实例1-4所制备的NixZn(1-x)Fe2O4气凝胶的磁滞回线如图2所示,镍元素的掺入使得材料的磁化强度有所提高。
Claims (8)
1.一种磁性NixZn(1-x)Fe2O4气凝胶的制备方法,其具体步骤如下:
(1)按NixZn(1-x)Fe2O4(X为0~1)的化学计量比称取铁源、锌源、镍源,然后将铁源、锌源、镍源、去离子水和无水乙醇按摩尔比例为1:(0~0.5):(0~0.5):(40~60):(15~20)混合搅拌,得到澄清混合溶液;
(2)向澄清混合溶液中加入质子去除剂,混合搅拌后倒入模具,20~50℃下等待凝胶;
(3)将步骤(2)中得到的湿凝胶在20~25℃下静置8~12h;
(4)将步骤(3)中静置后的湿凝胶再在烘箱中老化,期间进行溶剂置换;
(5)将步骤(4)中溶剂置换后的复合湿凝胶进行乙醇超临界干燥处理,其中乙醇超临界干燥法采用N2气体保护,干燥温度为255~275℃,高压反应釜压力控制在10~12MPa,反应时间为2~4h;
(6)将步骤(5)中得到的气凝胶进行高温热处理,热处理温度为300~900℃,升温速率为2~4℃/min,保温时间为2~4h,自然冷却至室温,得到NixZn(1-x)Fe2O4气凝胶。
2.根据权利要求1所述的制备方法,其特征在于步骤(1)中铁源为氯化铁、硝酸铁或乙酸铁的一种;锌源为氯化锌、硝酸锌或乙酸锌的一种;镍源为氯化镍、硝酸镍或乙酸镍的一种。
3.根据权利要求1所述的制备方法,其特征在于步骤(1)中混合搅拌的时间为20~30min。
4.根据权利要求1所述的制备方法,其特征在于步骤(2)中混合搅拌的时间为2~5min。
5.根据权利要求1所述的制备方法,其特征在于步骤(2)中质子去除剂为环氧丙烷、环氧乙烷或环氧氯丙烷的一种,铁源和质子去除剂按摩尔比例为1:(5~10)。
6.根据权利要求1所述的制备方法,其特征在于步骤(4)中所述的溶剂置换为无水乙醇进行溶剂置换,每6~9h更换一次,总共置换6~8次。
7.根据权利要求1所述的制备方法,其特征在于步骤(4)中烘箱的温度为40~60℃。
8.根据权利要求1所述的制备方法,其特征在于步骤(6)中高温热处理气氛为空气或者氧气的一种。
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