CN106040225A - 一种薄层状钛酸铋材料及其制备方法 - Google Patents
一种薄层状钛酸铋材料及其制备方法 Download PDFInfo
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- 239000000463 material Substances 0.000 title claims abstract description 51
- 229910002115 bismuth titanate Inorganic materials 0.000 title claims abstract description 45
- 238000002360 preparation method Methods 0.000 title claims abstract description 36
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 76
- 239000010936 titanium Substances 0.000 claims abstract description 76
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 52
- 238000003756 stirring Methods 0.000 claims abstract description 37
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims abstract description 32
- -1 titanium alkoxide Chemical class 0.000 claims abstract description 30
- RXPAJWPEYBDXOG-UHFFFAOYSA-N hydron;methyl 4-methoxypyridine-2-carboxylate;chloride Chemical compound Cl.COC(=O)C1=CC(OC)=CC=N1 RXPAJWPEYBDXOG-UHFFFAOYSA-N 0.000 claims abstract description 27
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 26
- 238000001354 calcination Methods 0.000 claims abstract description 26
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims abstract description 22
- 229960000583 acetic acid Drugs 0.000 claims abstract description 11
- VBIXEXWLHSRNKB-UHFFFAOYSA-N ammonium oxalate Chemical compound [NH4+].[NH4+].[O-]C(=O)C([O-])=O VBIXEXWLHSRNKB-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 11
- 239000012362 glacial acetic acid Substances 0.000 claims abstract description 11
- 239000004094 surface-active agent Substances 0.000 claims abstract description 11
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 claims abstract description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 9
- UIIMBOGNXHQVGW-DEQYMQKBSA-M Sodium bicarbonate-14C Chemical compound [Na+].O[14C]([O-])=O UIIMBOGNXHQVGW-DEQYMQKBSA-M 0.000 claims abstract description 3
- 238000003760 magnetic stirring Methods 0.000 claims description 27
- ZSIAUFGUXNUGDI-UHFFFAOYSA-N hexan-1-ol Chemical compound CCCCCCO ZSIAUFGUXNUGDI-UHFFFAOYSA-N 0.000 claims description 20
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 claims description 16
- 239000002131 composite material Substances 0.000 claims description 16
- 239000011521 glass Substances 0.000 claims description 16
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 13
- 238000013019 agitation Methods 0.000 claims description 13
- 239000002253 acid Substances 0.000 claims description 10
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 10
- 239000003643 water by type Substances 0.000 claims description 10
- 239000003153 chemical reaction reagent Substances 0.000 claims description 9
- 238000010438 heat treatment Methods 0.000 claims description 8
- 229910000030 sodium bicarbonate Inorganic materials 0.000 claims description 8
- 235000017557 sodium bicarbonate Nutrition 0.000 claims description 8
- 238000005728 strengthening Methods 0.000 claims description 8
- CDQSJQSWAWPGKG-UHFFFAOYSA-N butane-1,1-diol Chemical class CCCC(O)O CDQSJQSWAWPGKG-UHFFFAOYSA-N 0.000 claims description 7
- 239000011800 void material Substances 0.000 claims description 6
- 230000001699 photocatalysis Effects 0.000 abstract description 7
- 239000003344 environmental pollutant Substances 0.000 abstract description 3
- 150000001875 compounds Chemical class 0.000 abstract 2
- 238000001816 cooling Methods 0.000 abstract 2
- 230000003197 catalytic effect Effects 0.000 abstract 1
- 239000008367 deionised water Substances 0.000 abstract 1
- 229910021641 deionized water Inorganic materials 0.000 abstract 1
- 238000001035 drying Methods 0.000 abstract 1
- 235000011187 glycerol Nutrition 0.000 abstract 1
- 239000011229 interlayer Substances 0.000 abstract 1
- 238000002156 mixing Methods 0.000 abstract 1
- 239000003960 organic solvent Substances 0.000 abstract 1
- 238000007146 photocatalysis Methods 0.000 description 6
- 238000006555 catalytic reaction Methods 0.000 description 5
- 230000007613 environmental effect Effects 0.000 description 3
- 238000000034 method Methods 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 229910052747 lanthanoid Inorganic materials 0.000 description 2
- 231100000719 pollutant Toxicity 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
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Abstract
一种薄层状钛酸铋材料及其制备方法,配制钛醇盐溶液:以复合有机溶剂、钛酸正丙醇酯、导向剂和表面活性剂搅拌混合制备;制备溶胶:加入去离子水、硝酸铋、草酸铵、碳酸氢钠、冰醋酸和甘油以形成溶胶;制备薄层凝胶:将钛网放在石英玻璃片上,再覆盖透明溶胶,在溶胶未完全凝固前盖上石英玻璃片,在鼓风干燥箱内115℃干燥12 h;煅烧:将包有钛酸铋薄层凝胶的复合夹层放在程控箱式电炉中,在650~950℃煅烧6~8 h;冷却至室温,制得薄层状钛酸铋材料;材料稳定性好、活性成分分布均匀、催化活性高。可广泛用于反应器中对环境污染物的光催化治理,在环境领域有广阔的应用前景。
Description
技术领域
本发明涉及一种环境净化功能材料领域,具体涉及一种薄层状钛酸铋材料及其制备方法。
背景技术
在治理环境污染物的诸多技术手段中,光催化氧化技术已经发展了超过40年;在该技术的工业化应用过程中,适宜的光催化材料是最重要的影响因素;工业化的光催化净化反应器往往对材料的形状有特殊的要求,单纯的粉体材料不能满足连续性的污染物净化处理过程;为了避免污水处理后与光催化材料的分离步骤,在实际应用中往往采用负载型材料,而最终的材料形状通常受到载体的制约,对载体的选择还要考虑到光催化材料制备条件的限制;在通常采用的平板型反应器中需要使用薄层状的光催化材料;这类材料的基本特点是能够充分接收光源的辐射,同时还必须具备一定的机械强度,能够保持长时间的使用寿命。
镧系钛酸盐具有良好的热稳定性和较为适宜的禁带宽度,成为当前富有潜力的一类新型光催化材料;对该类材料的研究基本还处在理论研究阶段,缺少对其实际应用型产品的研制,尤其是未曾按照常用光催化反应器的具体要求制备特殊形状的镧系钛酸盐;针对平板型反应器对光催化材料的特殊需要,本专利公开一种薄层状钛酸铋材料及其制备方法。
发明内容
本发明的目的,是提供一种薄层状钛酸铋材料,该材料可广泛用于反应器中对环境污染物的光催化治理,在环境领域有广阔的应用前景。
本发明的另一个目的,是提供一种薄层状钛酸铋材料的制备方法。制备方法简明、合成条件温和且易于重复、材料结构和性能稳定。
采用的技术方案是:
一种薄层状钛酸铋材料,其特征是:
主要由50~76 mL无水乙醇、16~23 mL正己醇、5~7 mL丁二醇、6~8 mL钛酸正丙醇酯、1.5~2.6 mL导向剂ST-6、0.9-1.3 mL表面活性剂TW-8、21~26 mL去离子水、3.5~5.2g硝酸铋、1.5~1.6 g草酸铵、0.8~1.0 g碳酸氢钠、2.1~3.2 mL冰醋酸、0.8~1.3 mL甘油制备成,以上试剂浓度全部为分析纯。
一种薄层状钛酸铋材料的制备方法,其特征是:
(1) 配制钛醇盐溶液:
在200 mL玻璃烧杯中分别加入50~76 mL无水乙醇、16~23 mL正己醇和5~7 mL丁二醇,将烧杯放于磁力搅拌器上搅拌10~20min;
加入6~8 mL钛酸正丙醇酯、1.5~2.6 mL导向剂ST-6、0.9~1.3 mL表面活性剂TW-8,继续搅拌10~20 min至形成透明溶液,得到钛醇盐溶液,备用;
(2) 制备溶胶:
在100 mL玻璃烧杯中加入21~26 mL去离子水,称取3.5~5.2 g硝酸铋并加入水中,在磁力搅拌器上搅拌使之充分溶解;
取1.5~1.6 g草酸铵、0.8~1.0 g碳酸氢钠和2.1~3.2 mL冰醋酸并加入上述溶液中,在磁力搅拌器上搅拌20~30 min,完全溶解后形成透明溶液,得到硝酸铋溶液;
在搅拌下将硝酸铋溶液滴入钛醇盐溶液中,再加入0.8~1.3 mL甘油,继续搅拌30~40min,形成透明而略带粘稠的溶胶,备用;
(3) 制备薄层凝胶:
将钛网放在平整的石英玻璃片上,将步骤2制备的透明溶胶滴在钛网上至完全覆盖钛丝;
静置60~70 min,在溶胶未完全凝固前在上面盖上另一片石英玻璃片;
将上述复合夹层置于鼓风干燥箱内,在115 ℃干燥12 h,在两片石英玻璃片间形成由钛网强化的钛酸铋薄层凝胶;
(4) 煅烧:
将包有钛酸铋薄层凝胶的复合夹层放置在程控箱式电炉中,从室温开始以5 ℃/min的升温速率将煅烧温度升至650~950 ℃,并保持煅烧温度6~8 h;待材料冷却至室温后,即制得薄层状钛酸铋材料;
本制备方法中所述的磁力搅拌器的转速为200转/分,试剂浓度全部为分析纯。
本发明的优点在于:
1、本发明专利稳定性好、活性成分分布均匀、催化活性高,可广泛用于反应器中对环境污染物的光催化治理,在环境领域有广阔的应用前景。
2、本发明专利的制备方法简明、合成条件温和且易于重复。
具体实施方式
实施实例1
一种薄层状钛酸铋材料的制备方法,其特征是:
(1) 配制钛醇盐溶液:
在200 mL玻璃烧杯中分别加入52 mL无水乙醇、17 mL正己醇和5.3 mL丁二醇,将烧杯放于磁力搅拌器上搅拌10 min;
加入6.1 mL钛酸正丙醇酯、1.5 mL导向剂ST-6和0.9 mL表面活性剂TW-8,继续搅拌10min至形成透明溶液,得到钛醇盐溶液,备用;
(2) 制备溶胶:
在100 mL玻璃烧杯中加入22 mL去离子水,称取3.5 g硝酸铋并加入水中,在磁力搅拌器上搅拌使之充分溶解;
取1.5 g草酸铵、0.8 g碳酸氢钠和2.1 mL冰醋酸并加入上述溶液中,在磁力搅拌器上搅拌20 min,完全溶解后形成透明溶液,得到硝酸铋溶液;
在搅拌下将硝酸铋溶液滴入钛醇盐溶液中,再加入0.8 mL甘油,继续搅拌30 min,形成透明而略带粘稠的溶胶,备用;
(3) 制备薄层凝胶:
将5cm×5cm尺寸的钛网放在平整的石英玻璃片上,钛网由直径0.5 mm钛丝制成,钛丝间空隙尺寸为1mm×1mm,将步骤2制备的透明溶胶滴在钛网上至完全覆盖钛丝;
静置60 min,在溶胶未完全凝固前在上面盖上另一片石英玻璃片;
将上述复合夹层置于鼓风干燥箱内,在115 ℃干燥12 h,在两片石英玻璃片间形成由钛网强化的钛酸铋薄层凝胶;
(4) 煅烧:
将包有钛酸铋薄层凝胶的复合夹层放置在程控箱式电炉中,从室温开始以5 ℃/min的升温速率将煅烧温度升至660 ℃,并保持煅烧温度8 h;待材料冷却至室温后,即制得薄层状钛酸铋材料;
本制备方法所述的磁力搅拌器的转速为200转/分,试剂浓度全部为分析纯。
实施实例2
一种薄层状钛酸铋材料的制备方法,其特征是:
(1) 配制钛醇盐溶液:
在200 mL玻璃烧杯中分别加入67 mL无水乙醇、19 mL正己醇和6 mL丁二醇,将烧杯放于磁力搅拌器上搅拌10 min;
加入7.1 mL钛酸正丙醇酯、2.1 mL导向剂ST-6和1.0 mL表面活性剂TW-8,继续搅拌10min至形成透明溶液,得到钛醇盐溶液,备用;
(2) 制备溶胶:
在100 mL玻璃烧杯中加入22 mL去离子水,称取4.2 g硝酸铋并加入水中,在磁力搅拌器上搅拌使之充分溶解;
取1.5 g草酸铵、0.8 g碳酸氢钠和2.6 mL冰醋酸并加入上述溶液中,在磁力搅拌器上搅拌20 min,完全溶解后形成透明溶液,得到硝酸铋溶液;
在搅拌下将硝酸铋溶液滴入钛醇盐溶液中,再加入1.1 mL甘油,继续搅拌30 min,形成透明而略带粘稠的溶胶,备用;
(3) 制备薄层凝胶:
将5cm×5cm尺寸的钛网放在平整的石英玻璃片上,钛网由直径0.5 mm钛丝制成,钛丝间空隙尺寸为1mm×1mm,将步骤2制备的透明溶胶滴在钛网上至完全覆盖钛丝;
静置60 min,在溶胶未完全凝固前在上面盖上另一片石英玻璃片;
将上述复合夹层置于鼓风干燥箱内,在115 ℃干燥12 h,在两片石英玻璃片间形成由钛网强化的钛酸铋薄层凝胶;
(4) 煅烧:
将包有钛酸铋薄层凝胶的复合夹层放置在程控箱式电炉中,从室温开始以5 ℃/min的升温速率将煅烧温度升至750 ℃,并保持煅烧温度7 h;待材料冷却至室温后,即制得薄层状钛酸铋材料;
本制备方法所述的磁力搅拌器的转速为200转/分,试剂浓度全部为分析纯。
实施实例3
一种薄层状钛酸铋材料的制备方法,其特征是:
(1) 配制钛醇盐溶液:
在200 mL玻璃烧杯中分别加入72 mL无水乙醇、22 mL正己醇和7 mL丁二醇,将烧杯放于磁力搅拌器上搅拌10 min;
加入7 mL钛酸正丙醇酯、2.5 mL导向剂ST-6和1.2 mL表面活性剂TW-8,继续搅拌10min至形成透明溶液,得到钛醇盐溶液,备用;
(2) 制备溶胶:
在100 mL玻璃烧杯中加入25 mL去离子水,称取5.1 g硝酸铋并加入水中,在磁力搅拌器上搅拌使之充分溶解;
取1.6 g草酸铵、1.0 g碳酸氢钠和3.1 mL冰醋酸并加入上述溶液中,在磁力搅拌器上搅拌20 min,完全溶解后形成透明溶液,得到硝酸铋溶液;
在搅拌下将硝酸铋溶液滴入钛醇盐溶液中,再加入1.2 mL甘油,继续搅拌30 min,形成透明而略带粘稠的溶胶,备用;
(3) 制备薄层凝胶:
将5cm×5cm尺寸的钛网放在平整的石英玻璃片上,钛网由直径0.5 mm钛丝制成,钛丝间空隙尺寸为1mm×1mm,将步骤2制备的透明溶胶滴在钛网上至完全覆盖钛丝;
静置60 min,在溶胶未完全凝固前在上面盖上另一片石英玻璃片;
将上述复合夹层置于鼓风干燥箱内,在115 ℃干燥12 h,在两片石英玻璃片间形成由钛网强化的钛酸铋薄层凝胶;
(4) 煅烧:
将包有钛酸铋薄层凝胶的复合夹层放置在程控箱式电炉中,从室温开始以5 ℃/min的升温速率将煅烧温度升至900 ℃,并保持煅烧温度7 h;待材料冷却至室温后,即制得薄层状钛酸铋材料;
本制备方法所述的磁力搅拌器的转速为200转/分,试剂浓度全部为分析纯。
Claims (6)
1.一种薄层状钛酸铋材料,其特征是:
主要由50~76 mL无水乙醇、16~23 mL正己醇、5~7 mL丁二醇、6~8 mL钛酸正丙醇酯、1.5~2.6 mL导向剂ST-6、0.9~1.3 mL表面活性剂TW-8、21~26 mL去离子水、3.5~5.2g硝酸铋、1.5~1.6 g草酸铵、0.8~1.0 g碳酸氢钠、2.1~3.2 mL冰醋酸、0.8~1.3 mL甘油制备成,以上试剂浓度全部为分析纯。
2.根据权利要求1所述的一种薄层状钛酸铋材料的制备方法,其特征是:
(1) 配制钛醇盐溶液:
在200 mL玻璃烧杯中分别加入50~76 mL无水乙醇、16~23 mL正己醇和5~7 mL丁二醇,将烧杯放于磁力搅拌器上搅拌10~20min;
加入6~8 mL钛酸正丙醇酯、1.5~2.6 mL导向剂ST-6和0.9~1.3 mL表面活性剂TW-8,继续搅拌10~20 min至形成透明溶液,得到钛醇盐溶液,备用;
(2) 制备溶胶:
在100 mL玻璃烧杯中加入21~26 mL去离子水,称取3.5~5.2 g硝酸铋并加入水中,在磁力搅拌器上搅拌使之充分溶解;
取1.5~1.6 g草酸铵、0.8~1.0 g碳酸氢钠和2.1~3.2 mL冰醋酸并加入上述溶液中,在磁力搅拌器上搅拌20~30 min,完全溶解后形成透明溶液,得到硝酸铋溶液;
在搅拌下将硝酸铋溶液滴入钛醇盐溶液中,再加入0.8~1.3 mL甘油,继续搅拌30~40min,形成透明而略带粘稠的溶胶,备用;
(3) 制备薄层凝胶:
将钛网放在平整的石英玻璃片上,将步骤2制备的透明溶胶滴在钛网上至完全覆盖钛丝;
静置60~70 min,在溶胶未完全凝固前在上面盖上另一片石英玻璃片;
将上述复合夹层置于鼓风干燥箱内,在115 ℃干燥12 h,在两片石英玻璃片间形成由钛网强化的钛酸铋薄层凝胶;
(4) 煅烧:
将包有钛酸铋薄层凝胶的复合夹层放置在程控箱式电炉中,从室温开始以5 ℃/min的升温速率将煅烧温度升至650~950 ℃,并保持煅烧温度6~8 h;待材料冷却至室温后,即制得薄层状钛酸铋材料。
3.根据权利要求1或2所述的一种薄层状钛酸铋材料及其制备方法,所述的磁力搅拌器的转速为200转/分。
4.根据权利要求1所述的一种薄层状钛酸铋材料的制备方法,其特征是:
(1) 配制钛醇盐溶液:
在200 mL玻璃烧杯中分别加入67 mL无水乙醇、19 mL正己醇和6 mL丁二醇,将烧杯放于磁力搅拌器上搅拌10 min;
加入7.1 mL钛酸正丙醇酯、2.1 mL导向剂ST-6和1.0 mL表面活性剂TW-8,继续搅拌10min至形成透明溶液,得到钛醇盐溶液,备用;
(2) 制备溶胶:
在100 mL玻璃烧杯中加入22 mL去离子水,称取4.2 g硝酸铋并加入水中,在磁力搅拌器上搅拌使之充分溶解;
取1.5 g草酸铵、0.8 g碳酸氢钠和2.6 mL冰醋酸并加入上述溶液中,在磁力搅拌器上搅拌20 min,完全溶解后形成透明溶液,得到硝酸铋溶液;
在搅拌下将硝酸铋溶液滴入钛醇盐溶液中,再加入1.1 mL甘油,继续搅拌30 min,形成透明而略带粘稠的溶胶,备用;
(3) 制备薄层凝胶:
将5cm×5cm尺寸的钛网放在平整的石英玻璃片上,钛网由直径0.5 mm钛丝制成,钛丝间空隙尺寸为1mm×1mm,将步骤2制备的透明溶胶滴在钛网上至完全覆盖钛丝;
静置60 min,在溶胶未完全凝固前在上面盖上另一片石英玻璃片;
将上述复合夹层置于鼓风干燥箱内,在115 ℃干燥12 h,在两片石英玻璃片间形成由钛网强化的钛酸铋薄层凝胶;
(4) 煅烧:
将包有钛酸铋薄层凝胶的复合夹层放置在程控箱式电炉中,从室温开始以5 ℃/min的升温速率将煅烧温度升至750 ℃,并保持煅烧温度7 h;待材料冷却至室温后,即制得薄层状钛酸铋材料;
本制备方法所述的磁力搅拌器的转速为200转/分,试剂浓度全部为分析纯。
5.根据权利要求1所述的一种薄层状钛酸铋材料的制备方法,其特征是:
(1) 配制钛醇盐溶液:
在200 mL玻璃烧杯中分别加入72 mL无水乙醇、22 mL正己醇和7 mL丁二醇,将烧杯放于磁力搅拌器上搅拌10 min;
加入7 mL钛酸正丙醇酯、2.5 mL导向剂ST-6和1.2 mL表面活性剂TW-8,继续搅拌10min至形成透明溶液,得到钛醇盐溶液,备用;
(2) 制备溶胶:
在100 mL玻璃烧杯中加入25 mL去离子水,称取5.1 g硝酸铋并加入水中,在磁力搅拌器上搅拌使之充分溶解;
取1.6 g草酸铵,1.0 g碳酸氢钠和3.1 mL冰醋酸并加入上述溶液中,在磁力搅拌器上搅拌20 min,完全溶解后形成透明溶液,得到硝酸铋溶液;
在搅拌下将硝酸铋溶液滴入钛醇盐溶液中,再加入1.2 mL甘油,继续搅拌30 min,形成透明而略带粘稠的溶胶,备用;
(3) 制备薄层凝胶:
将5cm×5cm尺寸的钛网放在平整的石英玻璃片上,钛网由直径0.5 mm钛丝制成,钛丝间空隙尺寸为1mm×1mm,将步骤2制备的透明溶胶滴在钛网上至完全覆盖钛丝;
静置60 min,在溶胶未完全凝固前在上面盖上另一片石英玻璃片;
将上述复合夹层置于鼓风干燥箱内,在115 ℃干燥12 h,在两片石英玻璃片间形成由钛网强化的钛酸铋薄层凝胶;
(4) 煅烧:
将包有钛酸铋薄层凝胶的复合夹层放置在程控箱式电炉中,从室温开始以5 ℃/min的升温速率将煅烧温度升至900 ℃,并保持煅烧温度7 h;待材料冷却至室温后,即制得薄层状钛酸铋材料;
本制备方法所述的磁力搅拌器的转速为200转/分,试剂浓度全部为分析纯。
6.根据权利要求1所述的一种薄层状钛酸铋材料的制备方法,其特征是:
(1) 配制钛醇盐溶液:
在200 mL玻璃烧杯中分别加入50~76 mL无水乙醇、16~23 mL正己醇和5~7 mL丁二醇,将烧杯放于磁力搅拌器上搅拌10 min;
加入6~8 mL钛酸正丙醇酯、1.5~2.6 mL导向剂ST-6和0.9~1.3 mL表面活性剂TW-8,继续搅拌10 min至形成透明溶液,得到钛醇盐溶液,备用;
(2) 制备溶胶:
在100 mL玻璃烧杯中加入21~26 mL去离子水,称取3.5~5.2 g硝酸铋并加入水中,在磁力搅拌器上搅拌使之充分溶解;
取1.5~1.6 g草酸铵、0.8~1.0 g碳酸氢钠和2.1~3.2 mL冰醋酸并加入上述溶液中,在磁力搅拌器上搅拌20 min,完全溶解后形成透明溶液,得到硝酸铋溶液;
在搅拌下将硝酸铋溶液滴入钛醇盐溶液中,再加入0.8~1.3 mL甘油,继续搅拌30min,形成透明而略带粘稠的溶胶,备用;
(3) 制备薄层凝胶:
将5cm×5cm尺寸的钛网放在平整的石英玻璃片上,钛网由直径0.5 mm钛丝制成,钛丝间空隙尺寸为1mm×1mm,将步骤2制备的透明溶胶滴在钛网上至完全覆盖钛丝;
静置60 min,在溶胶未完全凝固前在上面盖上另一片石英玻璃片;
将上述复合夹层置于鼓风干燥箱内,在115 ℃干燥12 h,在两片石英玻璃片间形成由钛网强化的钛酸铋薄层凝胶;
(4) 煅烧:
将包有钛酸铋薄层凝胶的复合夹层放置在程控箱式电炉中,从室温开始以5 ℃/min的升温速率将煅烧温度升至650~950 ℃,并保持煅烧温度6~8 h;待材料冷却至室温后,即制得薄层状钛酸铋材料;
本制备方法所述的磁力搅拌器的转速为200转/分,试剂浓度全部为分析纯。
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CN107096522A (zh) * | 2017-06-05 | 2017-08-29 | 沈阳理工大学 | 一种涂饰钛酸铋的陶瓷纤维布的制备方法及其应用 |
CN108301253A (zh) * | 2018-01-08 | 2018-07-20 | 沈阳理工大学 | 一种表面包覆钛硼氧化物涂层的陶瓷纤维纸的制备方法 |
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CN103100414A (zh) * | 2013-01-31 | 2013-05-15 | 沈阳理工大学 | 一种具有光催化功能的分子筛及其制备方法 |
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