CN107413322A - 纳米TiO2柱撑蒙脱石的生产方法及应用 - Google Patents
纳米TiO2柱撑蒙脱石的生产方法及应用 Download PDFInfo
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- 229910052901 montmorillonite Inorganic materials 0.000 title claims abstract description 95
- GUJOJGAPFQRJSV-UHFFFAOYSA-N dialuminum;dioxosilane;oxygen(2-);hydrate Chemical compound O.[O-2].[O-2].[O-2].[Al+3].[Al+3].O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O GUJOJGAPFQRJSV-UHFFFAOYSA-N 0.000 title claims abstract description 76
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 30
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 36
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims abstract description 21
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000010936 titanium Substances 0.000 claims abstract description 20
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 20
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims abstract description 16
- 229910000278 bentonite Inorganic materials 0.000 claims abstract description 14
- 239000000440 bentonite Substances 0.000 claims abstract description 14
- SVPXDRXYRYOSEX-UHFFFAOYSA-N bentoquatam Chemical compound O.O=[Si]=O.O=[Al]O[Al]=O SVPXDRXYRYOSEX-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000003960 organic solvent Substances 0.000 claims abstract description 12
- 238000003756 stirring Methods 0.000 claims abstract description 9
- 229910003002 lithium salt Inorganic materials 0.000 claims abstract description 7
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- 238000000034 method Methods 0.000 claims description 20
- LCKIEQZJEYYRIY-UHFFFAOYSA-N Titanium ion Chemical compound [Ti+4] LCKIEQZJEYYRIY-UHFFFAOYSA-N 0.000 claims description 14
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- 239000002245 particle Substances 0.000 claims description 3
- 238000000926 separation method Methods 0.000 claims description 3
- 238000005245 sintering Methods 0.000 claims description 2
- 229910010066 TiC14 Inorganic materials 0.000 claims 2
- 239000003054 catalyst Substances 0.000 abstract description 9
- 230000001699 photocatalysis Effects 0.000 abstract description 8
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- 150000003384 small molecules Chemical class 0.000 abstract description 4
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- 238000007146 photocatalysis Methods 0.000 description 4
- 239000004065 semiconductor Substances 0.000 description 4
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 3
- 229910003074 TiCl4 Inorganic materials 0.000 description 3
- 150000001768 cations Chemical class 0.000 description 3
- 229910001416 lithium ion Inorganic materials 0.000 description 3
- 238000012545 processing Methods 0.000 description 3
- 239000010865 sewage Substances 0.000 description 3
- 229910010413 TiO 2 Inorganic materials 0.000 description 2
- 150000001722 carbon compounds Chemical class 0.000 description 2
- 230000015556 catabolic process Effects 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 238000006731 degradation reaction Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000005342 ion exchange Methods 0.000 description 2
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 description 2
- 229910052808 lithium carbonate Inorganic materials 0.000 description 2
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- 229910018516 Al—O Inorganic materials 0.000 description 1
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
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- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
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- 229910052760 oxygen Inorganic materials 0.000 description 1
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 description 1
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
- B01J21/16—Clays or other mineral silicates
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- B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
- B01J21/06—Silicon, titanium, zirconium or hafnium; Oxides or hydroxides thereof
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Abstract
本发明公开了一种纳米TiO2柱撑蒙脱石的生产方法及应用,属于膨润土加工领域。将锂盐溶于草酸水溶液中,再加入到膨润土中处理后得到锂基蒙脱石;将锂基蒙脱石分散于有机溶剂再加入钛盐搅拌反应后分离得到钛基蒙脱石;将钛基蒙脱石在氧化气氛中焙烧后粉碎得纳米TiO2柱撑蒙脱石成品。本发明的纳米级的TiO2柱撑蒙脱石由于其量子尺寸效应等作用,其光催化活性较高,可将各类有机污染物快速转化为CO2、H2O和小分子无机物,以达到净化治污的目的;其生产过程简单,将纳米TiO2置于蒙脱石载体中,不单可以降低光催化剂的成本,还能回收使用过的光催化剂及载体,通过处理蒙脱石载体,可以使TiO2再生,从而降低其生产和使用成本。
Description
技术领域
本发明涉及一种蒙脱石的生产方法,具体讲是一种纳米TiO2柱撑蒙脱石的生产方法及应用,属于膨润土加工领域。
背景技术
纳米TiO2柱撑蒙脱石主要应用于有机污水的处理,是一种能高效降解碳化合物、芳香族化合物、氮化合物、表面活性剂等有机污染物的光催化剂,其通过光催化作用,将各类有机污染物转化为CO2、H2O和小分子无机物,以达到净化污水的目的,光催化剂处理有机废水的特点是工艺设备简单、动力消耗少、占地面积小等优点。将纳米TiO2置于蒙脱石载体中,不单可以降低光催化剂的成本,还能回收使用过的光催化剂及载体,通过处理蒙脱石载体,还可以使TiO2再生,从而使得有机废水的处理变得更为简单,成本更为低廉。目前纳米TiO2柱撑蒙脱石的生产方法主要包括TiCl4水解法和溶胶-凝胶法。2003年3月27日,申请号为011256591中国发明专利申请公开一种名称为纳米二氧化钛柱撑膨润土及其制备方法,就是采用溶胶-凝胶法。该生产方法过程复杂,工艺控制较困难,生产成本较高,无法满足常规的工业生产。
发明内容
本发明所要解决的技术问题在于克服现有技术缺陷,提供一种光催化活性高,生产工艺简单、成本较低的纳米TiO2柱撑蒙脱石的生产方法及应用。
为了解决上述技术问题,本发明提供的纳米TiO2柱撑蒙脱石的生产方法,包括以下步骤:
1)将锂盐溶于浓度为10%的草酸水溶液中,再加入到膨润土中,搅拌、挤压、干燥、粉碎后得到锂基蒙脱石;
2)将步骤1)得到的锂基蒙脱石分散于有机溶剂中,加入钛盐搅拌反应后,再分离得到钛基蒙脱石;
3)将步骤2)得到的钛基蒙脱石在氧化气氛中焙烧,使钛离子氧化成纳米级TiO2颗粒,柱撑于蒙脱石层间,然后粉碎得纳米TiO2柱撑蒙脱石成品。
本发明中,所述步骤1)中锂盐用量为膨润土质量的3-4%,草酸用量为膨润土质量的3-5%。
本发明中,所述步骤2)中有机溶剂为乙醇,所述锂基蒙脱石在乙醇中的含量为20%。
本发明中,所述步骤2)中钛盐为TiCl4,所述TiCl4用量为锂基蒙脱石质量的6%。
本发明中,所述分离过程为先采用沉淀法,后采用加热分馏法分离出钛基蒙脱石和有机溶剂。
本发明中,所述步骤3)中焙烧温度为300-500℃,焙烧时长1-2小时。
上述所制备的纳米TiO2柱撑蒙脱石在水处理领域中的应用。
本发明纳米TiO2柱撑蒙脱石的制备原理:通过蒙脱石的离子交换性能,将钛离子引入蒙脱石的结构层,再通过焙烧工艺将层间的钛离子氧化成TiO2,由于蒙脱石为纳米级的层间距,在层间形成的TiO2,也势必是纳米级,这些纳米级的TiO2如柱子般支撑在蒙脱石层间,称为纳米TiO2柱撑蒙脱石。
本发明的有益效果在于:(1)利用膨润土中的主要矿物蒙脱石的离子交换性、电荷性和纳米层间距等性能,在有机溶剂中将钛离子引入蒙脱石层间,得到钛基蒙脱石,然后将钛基蒙脱石在氧化气氛中和在一定温度下焙烧一定的时间,将蒙脱石层间的钛离子氧化成纳米级的TiO2,得到纳米TiO2柱撑蒙脱石。由于纳米TiO2是一种宽禁带半导体,在紫外线照射下,电子由低能价带向高能导带跃迁,形成光生电子和光生空穴。光生空穴可以夺取半导体表面吸附物质的电子,而使吸附物质被氧化,达到氧化分解吸附的有机物的目的。纳米级的TiO2柱撑蒙脱石由于其量子尺寸效应等作用,其光催化活性较高,可将各类有机污染物快速转化为CO2、H2O和小分子无机物,以达到净化治污的目的;其生产过程简单,将纳米TiO2置于蒙脱石载体中,不单可以降低光催化剂的成本,还能回收使用过的光催化剂及载体,通过处理蒙脱石载体,还可以使TiO2再生,从而降低其生产和使用成本;(2)在分离有机溶剂和钛基蒙脱石时,先采用沉淀法,后采用加热分馏法分离出钛基蒙脱石和有机溶剂,可实现有机溶剂的回收再利用,进一步降低了生产成本。
具体实施方式
下面结合实施例对本发明作进一步详细说明。
蒙脱石是一种粘土矿物,其结构层为2:1型,即由二层Si-O四面体夹着一层Al-O八面体。由蒙脱石矿物组成的岩石叫膨润土,广泛分布于自然界中,具有膨胀、分散、吸附、润滑、触变、增稠和粘结等性能,广泛应用于冶金、铸造、钻井、化工、建筑等行业,有“万能粘土”之称。蒙脱石八面体中的Al3+可以被一些二价阳离子置换,导致电荷不平衡,结构层面带负电。为了达到平衡,蒙脱石层间必须吸附阳离子,如:Ca2+,Mg2+,Na+等,这些阳离子可以根据交换能力和浓度进行交换,例如将钙基蒙脱石转化为钠基蒙脱石。正是由于蒙脱石具有阳离子交换性能,才可以将不同的阳离子,包括钛离子引入蒙脱石结构层间。蒙脱石的另一个性能是层状结构,其层间距在1.2~1.5纳米之间。由于具有离子交换性能,这一纳米级的层间域,就成为良好的化学反应场所。
纳米TiO2是一种宽禁带半导体,在紫外线照射下,电子由低能价带向高能导带跃迁,形成光生电子和光生空穴。光生空穴可以夺取半导体表面吸附物质的电子,而使吸附物质被氧化;光生电子可以传递给吸附物质,使吸附物质被还原。在这个氧化还原过程中,氧气的存在是必要的,因为氧化剂是O2 -和O-。光诱发电子和空穴向吸附的物质转移,而使吸附物质发生氧化-还原反应,叫光催化作用。许多半导体如:ZnO、CdO、PbS等都有光催化作用,但TiO2的催化活性最高,化学性能稳定,产生的光生电子和空穴的电势电位高,具有很强的氧化性和还原性,是目前最有潜力的光催化剂。纳米级的TiO2,由于其量子尺寸效应等作用,使光催化活性得到成倍的提高。
本发明的纳米TiO2柱撑蒙脱石的生产方法,主要包括以下工序:锂离子改型---有机相分散和钛离子改型-----焙烧粉碎。本发明以下实施例中所使用的试剂均为市售试剂,在此不一一展开描述。
实施例1
纳米TiO2柱撑蒙脱石的生产方法具体过程如下:
1、锂离子改型。将3克锂盐(碳酸锂)溶于40ml10%的草酸水溶液中,然后再加入到100克的膨润土中,搅拌、挤压、干燥、磨粉后得到锂基蒙脱石。
2、钛离子改型。将上述锂基蒙脱石粉末分散于乙醇溶液中,锂基蒙脱石在乙醇中的浓度为20%,加入锂基蒙脱石质量6%的TiCl4,搅拌反应1小时后,先采用沉淀法,后采用加热分馏法分离出钛基蒙脱石和乙醇,得到钛基蒙脱石;回收后的有机溶剂可以再利用,从而降低纳米TiO2柱撑蒙脱石的生产成本。
本发明中钛离子改型是在乙醇中进行的,其目的是防止TiCl4遇水水解形成偏钛酸,而得不到钛离子,从而不能形成钛基蒙脱石。
3、焙烧粉碎。将分离得到的钛基蒙脱石置于马弗炉中在500℃的氧化气氛中焙烧温1小时,使钛离子氧化成纳米级TiO2颗粒,柱撑于蒙脱石层间,然后用粉碎机粉碎,得纳米TiO2柱撑蒙脱石成品。
实施例2
纳米TiO2柱撑蒙脱石的生产方法具体过程如下:
1、锂离子改型。将4克锂盐(碳酸锂)溶于50ml10%的草酸水溶液中,然后再加入到100克的膨润土中,搅拌、挤压、干燥、磨粉后得到锂基蒙脱石。
2、钛离子改型。将上述锂基蒙脱石粉末分散于乙醇溶液中,其浓度为20%,加入锂基蒙脱石质量6%的TiCl4,搅拌反应1小时后,先采用沉淀法,后采用加热分馏法分离出钛基蒙脱石和乙醇,得到钛基蒙脱石;回收后的有机溶剂可以再利用,从而降低纳米TiO2柱撑蒙脱石的生产成本。
3、焙烧粉碎。将分离得到的钛基蒙脱石置于马弗炉中在350℃的氧化气氛中焙烧温2小时,使钛离子氧化成纳米级TiO2颗粒,柱撑于蒙脱石层间,然后用粉碎机粉碎,得纳米TiO2柱撑蒙脱石成品。
上述生产得到的纳米TiO2柱撑蒙脱石可应用于有机污水的处理,纳米TiO2柱撑蒙脱石作为一种能高效降解有机污染物的光催化剂,通过光催化作用,将碳化合物、芳香族化合物、氮化合物、表面活性剂等有机污染物转化为CO2、H2O和小分子等无机物,以达到净化污水的目的。。
本发明提供了一种纳米TiO2柱撑蒙脱石的生产方法及应用,具体实现该技术方案的方法和途径很多,以上所述仅是本发明的优选实施方式,应当指出,对于本技术领域的普通技术人员来说,在不脱离本发明原理的前提下,还可以做出若干改进和润饰,这些改进和润饰也应视为本发明的保护范围。本实施例中未明确的各组成部分均可用现有技术加以实现。
Claims (7)
1.一种纳米TiO2柱撑蒙脱石的生产方法,其特征在于包括以下步骤:
1)将锂盐溶于浓度为10%的草酸水溶液中,再加入到膨润土中,搅拌、挤压、干燥、粉碎后得到锂基蒙脱石;
2)将步骤1)得到的锂基蒙脱石分散于有机溶剂中,加入钛盐搅拌反应后,再分离得到钛基蒙脱石;
3)将步骤2)得到的钛基蒙脱石在氧化气氛中焙烧,使钛离子氧化成纳米级TiO2颗粒,柱撑于蒙脱石层间,然后粉碎得纳米TiO2柱撑蒙脱石成品。
2.根据权利要求1所述的纳米TiO2柱撑蒙脱石的生产方法,其特征在于:所述步骤1)中锂盐用量为膨润土质量的3-4%,草酸用量为膨润土质量的3-5%。
3.根据权利要求1或2所述的纳米TiO2柱撑蒙脱石的生产方法,其特征在于:所述步骤2)中有机溶剂为乙醇,所述锂基蒙脱石在乙醇中的含量为20%。
4.根据权利要求3所述的纳米TiO2柱撑蒙脱石的生产方法,其特征在于:所述步骤2)中钛盐为TiC14,所述TiC14用量为锂基蒙脱石质量的6%。
5.根据权利要求4所述的纳米TiO2柱撑蒙脱石的生产方法,其特征在于:所述分离过程为先采用沉淀法,后采用加热分馏法分离出钛基蒙脱石和有机溶剂。
6.根据权利要求5所述的纳米TiO2柱撑蒙脱石的生产方法,其特征在于:所述步骤3)中焙烧温度为300-500℃,焙烧时长1-2小时。
7.权利要求1至6任一项所制备的纳米TiO2柱撑蒙脱石在水处理领域中的应用。
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