CN107185514A - 一种制备管状薄层氧化铟‑氧化钛材料的方法 - Google Patents
一种制备管状薄层氧化铟‑氧化钛材料的方法 Download PDFInfo
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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims abstract description 38
- 238000000034 method Methods 0.000 title claims abstract description 18
- PJXISJQVUVHSOJ-UHFFFAOYSA-N indium(iii) oxide Chemical compound [O-2].[O-2].[O-2].[In+3].[In+3] PJXISJQVUVHSOJ-UHFFFAOYSA-N 0.000 title abstract description 4
- 229910003437 indium oxide Inorganic materials 0.000 title abstract 2
- 239000010453 quartz Substances 0.000 claims abstract description 40
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 40
- 239000003708 ampul Substances 0.000 claims abstract description 37
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims abstract description 21
- 239000000463 material Substances 0.000 claims abstract description 20
- YRKCREAYFQTBPV-UHFFFAOYSA-N acetylacetone Chemical compound CC(=O)CC(C)=O YRKCREAYFQTBPV-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000002243 precursor Substances 0.000 claims abstract description 18
- 239000007788 liquid Substances 0.000 claims abstract description 14
- HXCHRJMJMALFHP-UHFFFAOYSA-N azanium;ethanol;hydroxide Chemical compound N.O.CCO HXCHRJMJMALFHP-UHFFFAOYSA-N 0.000 claims abstract description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 9
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- AJPJDKMHJJGVTQ-UHFFFAOYSA-M sodium dihydrogen phosphate Chemical compound [Na+].OP(O)([O-])=O AJPJDKMHJJGVTQ-UHFFFAOYSA-M 0.000 claims abstract description 7
- 239000003381 stabilizer Substances 0.000 claims abstract description 7
- 238000001816 cooling Methods 0.000 claims abstract description 4
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- 125000005909 ethyl alcohol group Chemical group 0.000 claims description 10
- 238000006243 chemical reaction Methods 0.000 claims description 9
- 229910052738 indium Inorganic materials 0.000 claims description 9
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 claims description 9
- 238000003756 stirring Methods 0.000 claims description 8
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- 239000011159 matrix material Substances 0.000 claims description 6
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- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 5
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical class CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 5
- 238000013019 agitation Methods 0.000 claims description 5
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- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims 1
- 230000001476 alcoholic effect Effects 0.000 claims 1
- 238000001354 calcination Methods 0.000 abstract description 9
- 238000005516 engineering process Methods 0.000 abstract description 7
- 230000001699 photocatalysis Effects 0.000 abstract description 6
- KFZMGEQAYNKOFK-UHFFFAOYSA-N isopropyl alcohol Natural products CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 abstract description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 abstract description 3
- RGHLNCFICOYDIO-UHFFFAOYSA-N [In].C(CCC)O Chemical compound [In].C(CCC)O RGHLNCFICOYDIO-UHFFFAOYSA-N 0.000 abstract description 2
- 229910000403 monosodium phosphate Inorganic materials 0.000 abstract description 2
- 239000010865 sewage Substances 0.000 abstract description 2
- 239000000758 substrate Substances 0.000 abstract description 2
- 239000008367 deionised water Substances 0.000 abstract 1
- 229910021641 deionized water Inorganic materials 0.000 abstract 1
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- GLMQLIQWKQLVMB-UHFFFAOYSA-N [O-2].[In+3].[O-2].[Ti+4] Chemical compound [O-2].[In+3].[O-2].[Ti+4] GLMQLIQWKQLVMB-UHFFFAOYSA-N 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
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Abstract
一种制备管状薄层氧化铟‑氧化钛材料的方法,属于材料技术领域,按以下步骤进行:(1)将无水乙醇和乙二醇混合,45±1℃回流;加入钛酸异丙醇酯、四叔丁基氢氧化铵‑乙醇溶液、正丁醇铟和稳定剂AP‑8,回流获得溶液A;将无水乙醇、乙酰丙酮、磷酸二氢钠和去离子水搅拌混合,获得溶液B;将溶液B加入到溶液A中,45±1℃回流,获得前驱体溶液;(2)将石英管一端封闭,将前驱体溶液装满石英管静置后倒出,悬垂至没有液体滴出;80±1℃保温;(3)400~550℃煅烧后随炉冷却。本发明在石英管内壁上制备的薄层In2O3‑TiO2材料结构致密、活性成分分布均匀、光催化活性高、与石英基体结合紧密、使用寿命长,适于大规模连续流动治理污水。
Description
技术领域
本发明属于材料技术领域,特别涉及一种制备管状薄层氧化铟-氧化钛料的方法。
背景技术
环境水污染治理一直是环境工程领域的研究重点,人们始终对新型的水污染治理技术进行不懈的探索。自从半个世纪以前发现了光催化技术对有机污染物的降解作用,人们对于光催化氧化技术在诸多领域的应用寄予了厚望。时至今日,众多的光催化材料和技术已经广泛用于大气和水环境中的污染治理。TiO2是一种研究最为广泛和深入的光催化材料,该类材料具有良好的活性,但其主要缺点是对可见光吸收较弱,因而并不适于利用阳光作为辐射光源以降低使用成本。为了调节TiO2的禁带宽度,通常采用掺杂和复合氧化物形式。
能够应用于大规模工业化水治理的光催化材料是该领域的研究重点,同时对各种特殊应用条件的适应性也是应用该技术的关键之处。由于有关光催化技术的研究主要围绕理论研究过程,缺少对大规模污水治理过程所需特定光催化材料制备的研究。
发明内容
针对现有技术存在的问题,本发明提供一种制备管状薄层氧化铟-氧化钛料的方法,通过调配成分、精确控制前驱体合成、涂覆、凝胶化以及结晶固化过程,制备出以石英管为基体材料的管状薄层In2O3-TiO2材料。
本发明的方法按以下步骤进行:
1、制备In2O3-TiO2前驱体溶液:
1.1、将50~80mL无水乙醇和10~15mL乙二醇混合获得混合溶液,将混合溶液加热至45±1℃,在搅拌条件下回流反应20~30min;然后向混合溶液中加入12~15mL钛酸异丙醇酯、5.5~6.2mL四叔丁基氢氧化铵-乙醇溶液、3.6~4.1mL正丁醇铟和1.6~1.8mL稳定剂AP-8,继续在45±1 ℃和搅拌条件下回流反应30~40 min,获得溶液A;所述的四叔丁基氢氧化铵-乙醇溶液中四叔丁基氢氧化铵的重量浓度为25~30%;
1.2、将23~32mL无水乙醇、2.6~2.7mL乙酰丙酮、0.5~0.8g磷酸二氢钠和5.3~7.1mL去离子水搅拌混合均匀形成透明溶液,获得溶液B;
1.3、在搅拌条件下,将溶液B加入到溶液A中,在45±1℃回流反应30~40min,获得透明的In2O3-TiO2前驱体溶液;
2、液膜涂覆和凝胶化:
2.1、采用石英管作为涂覆基体,将石英管一端封闭,将In2O3-TiO2前驱体溶液装满石英管,静置60s以上,然后将In2O3-TiO2前驱体溶液倒出,开启石英管封闭端,悬垂至没有液体从石英管内滴出,制成内壁涂覆有液膜的石英管;
2.2、将内壁涂覆有液膜的石英管加热至80±1℃保温12~16 h,获得内壁覆盖凝胶膜的石英管;
3、涂层结晶固化:
将内壁覆盖凝胶膜的石英管升温至400~550 ℃,煅烧2~5 h,然后随炉冷却,在石英管内获得管状薄层In2O3-TiO2材料。
上述的石英管内径25 mm。
上述的步骤3中升温是以5±0.1℃/min的速率升温。
上述方法中,将石英管一端封闭是采用胶塞堵塞。
与现有技术相比,本发明的优点在于:
通过合理调配前驱体成分并精确控制前驱体溶液合成、石英管涂覆和凝胶化以及涂层结晶固化过程,制备出以石英管为基体材料的管状薄层In2O3-TiO2材料。石英基体材料能够保证高温煅烧条件下涂层材料的稳定性,并能保证外射光线能充分透过。通过本发明在石英管内壁上制备的薄层In2O3-TiO2材料结构致密、活性成分分布均匀、光催化活性高、与石英基体结合紧密、使用寿命长,适于大规模连续流动治理污水。
具体实施方式:
本发明实施例中采用的无水乙醇、乙二醇、钛酸异丙醇酯、四叔丁基氢氧化铵-乙醇溶液、正丁醇铟、稳定剂AP-8、乙酰丙酮和磷酸二氢钠为市购分析纯试剂。
本发明实施例中的石英管长度100 mm,壁厚1 mm,内径25 mm。
本发明实施例中进行回流反应的装置包括200 mL四口圆底烧瓶、控温电热包、球形冷凝管和测温热电隅。
本发明实施例中制备溶液A采用电动搅拌,制备溶液B采用磁力搅拌,电动搅拌机的搅拌速度为100rpm,磁力搅拌器的转速为200 rpm。
本发明将溶液B加入到溶液A时,采用缓慢滴入的方式,以反应物料不出现激烈反应为准。
本发明实施例中制备内壁覆盖凝胶膜的石英管采用恒温电热干燥箱。
本发明实施例中煅烧采用程控箱式电炉。
本发明实施例中制备的管状薄层In2O3-TiO2材料的厚度0.5~0.6微米,成分为In2O3与TiO2,In2O3与TiO2的摩尔数比为(1.3~1.7):1。
实施例1
安装回流反应装置,包括200 mL四口圆底烧瓶、控温电热包、球形冷凝管、测温热电隅和电动搅拌机;
1、制备In2O3-TiO2前驱体溶液:
在圆底烧瓶中分别加入50 mL无水乙醇和10 mL 乙二醇,开启电动搅拌机;球形冷凝管通入自来水后,开启电热包加热,保持溶液温度45±1℃,在搅拌状态下回流20 min;
继续向烧瓶中加入12 mL钛酸异丙醇酯、5.5 mL 四叔丁基氢氧化铵乙醇溶液、3.6 mL正丁醇铟和1.6 mL稳定剂AP-8,继续45±1℃回流30 min,形成溶液A;
所述的四叔丁基氢氧化铵乙醇溶液中四叔丁基氢氧化铵的重量浓度为25%;
在100 mL烧杯中加入23 mL无水乙醇、2.6mL乙酰丙酮、0.5g磷酸二氢钠和5.3mL去离子水,置于磁力搅拌器上搅拌30 min至形成透明溶液,形成溶液B;
将溶液B加入到放有溶液A的烧瓶中,在45±1℃加热搅拌回流30min,形成透明状In2O3-TiO2前驱体溶液;
2、石英管涂覆和凝胶化:
采用石英管作为涂覆基体,将石英管一端用胶塞堵塞,开口向上垂直放置,将In2O3-TiO2前驱体溶液倒入石英管,使之充满,静置60s,倒出管中溶液,去除胶塞,垂直悬挂至石英管下端不再有液滴流下,在涂覆中要注意不使石英管外壁沾上前驱体溶液;
将内壁涂覆In2O3-TiO2前驱体液膜的石英管放置于恒温电热干燥箱内,在80±1℃保温12 h,获得内壁覆盖凝胶膜的石英管;
3、涂层结晶固化:
将获得内壁覆盖凝胶膜的石英管置于程控箱式电炉内,从室温开始以5±0.1 ℃/min的升温速率升至煅烧温度,所述的煅烧温度为400 ℃,并保持煅烧温度5 h;然后随炉冷却,在石英管内获得管状薄层In2O3-TiO2材料。
实施例2
方法同实施例1,不同点在于:
(1)在烧瓶中分别加入65mL无水乙醇和12 mL 乙二醇,45±1℃回流25min;
(2)加入13 mL钛酸异丙醇酯、5.8 mL 四叔丁基氢氧化铵乙醇溶液、3.9 mL正丁醇铟和1.7 mL稳定剂AP-8,继续回流35min,形成溶液A;
所述的四叔丁基氢氧化铵乙醇溶液中四叔丁基氢氧化铵的重量浓度为28%;
(3)在100mL烧杯中加入27mL无水乙醇、2.6mL乙酰丙酮、0.6g磷酸二氢钠和6.2mL去离子水,搅拌35 min形成溶液B;
(4)将溶液B置于放有溶液A的烧瓶中,在45±1℃回流35min,形成In2O3-TiO2前驱体溶液;
(5)In2O3-TiO2前驱体溶液充满石英管后静置90s;
(6)干燥时在80±1℃保温14 h;
(7)煅烧温度为480℃,煅烧时间3 h。
实施例3
方法同实施例1,不同点在于:
(1)在烧瓶中分别加入80 mL无水乙醇和15 mL 乙二醇,45±1℃回流30min;
(2)加入15 mL钛酸异丙醇酯、6.2mL 四叔丁基氢氧化铵乙醇溶液、4.1mL正丁醇铟和1.8 mL稳定剂AP-8,继续回流40min,形成溶液A;
所述的四叔丁基氢氧化铵乙醇溶液中四叔丁基氢氧化铵的重量浓度为30%;
(3)在100mL烧杯中加入32mL无水乙醇、2.7mL乙酰丙酮、0.8g磷酸二氢钠和7.1mL去离子水,搅拌40 min形成溶液B;
(4)将溶液B置于放有溶液A的烧瓶中,在45±1℃回流40min,形成In2O3-TiO2前驱体溶液;
(5)In2O3-TiO2前驱体溶液充满石英管后静置120s;
(6)干燥时在80±1℃保温16 h;
(7)煅烧温度为550℃,煅烧时间2 h。
以上所述仅为本发明的优选实施例,并非因此限制本发明的专利范围,凡是利用本发明说明书内容所作的等效变换,或直接或间接运用在其他相关的技术领域,均同理包括在本发明的保护范围内。
Claims (4)
1.一种制备管状薄层氧化铟-氧化钛材料的方法,其特征在于按以下步骤进行:
(1)制备In2O3-TiO2前驱体溶液:
(1.1)将50~80mL无水乙醇和10~15mL乙二醇混合获得混合溶液,将混合溶液加热至45±1℃,在搅拌条件下回流反应20~30min;然后向混合溶液中加入12~15mL钛酸异丙醇酯、5.5~6.2mL四叔丁基氢氧化铵-乙醇溶液、3.6~4.1mL正丁醇铟和1.6~1.8mL稳定剂AP-8,继续在45±1 ℃和搅拌条件下回流反应30~40 min,获得溶液A;所述的四叔丁基氢氧化铵-乙醇溶液中四叔丁基氢氧化铵的重量浓度为25~30%;
(1.2)将23~32mL无水乙醇、2.6~2.7mL乙酰丙酮、0.5~0.8g磷酸二氢钠和5.3~7.1mL去离子水搅拌混合均匀形成透明溶液,获得溶液B;
(1.3)在搅拌条件下,将溶液B加入到溶液A中,在45±1℃回流反应30~40min,获得透明的In2O3-TiO2前驱体溶液;
(2)液膜涂覆和凝胶化:
(2.1)采用石英管作为涂覆基体,将石英管一端封闭,将In2O3-TiO2前驱体溶液装满石英管,静置60s以上,然后将In2O3-TiO2前驱体溶液倒出,开启石英管封闭端,悬垂至没有液体从石英管内滴出,制成内壁涂覆有液膜的石英管;
(2.2)将内壁涂覆有液膜的石英管加热至80±1℃保温12~16 h,获得内壁覆盖凝胶膜的石英管;
(3)涂层结晶固化:
将内壁覆盖凝胶膜的石英管升温至400~550 ℃,煅烧2~5 h,然后随炉冷却,在石英管内获得管状薄层In2O3-TiO2材料。
2.根据权利要求1所述的一种制备管状薄层氧化铟-氧化钛材料的方法,其特征在于步骤(3)中升温是以5±0.1℃/min的速率升温。
3.根据权利要求1所述的一种制备管状薄层氧化铟-氧化钛材料的方法,其特征在于步骤(2.1)中将石英管一端封闭是采用胶塞堵塞。
4.根据权利要求1所述的一种制备管状薄层氧化铟-氧化钛材料的方法,其特征在于所述的石英管选用内径25 mm。
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