CN105944683B - 一种降解甲醛的介孔复合材料及其制备方法 - Google Patents
一种降解甲醛的介孔复合材料及其制备方法 Download PDFInfo
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- 239000002131 composite material Substances 0.000 title claims abstract description 54
- 230000015556 catabolic process Effects 0.000 title claims abstract description 28
- 238000006731 degradation reaction Methods 0.000 title claims abstract description 28
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 title abstract description 101
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 38
- 239000013335 mesoporous material Substances 0.000 claims abstract description 31
- 229910021650 platinized titanium dioxide Inorganic materials 0.000 claims abstract description 17
- 238000003756 stirring Methods 0.000 claims description 42
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 32
- 150000001875 compounds Chemical class 0.000 claims description 28
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims description 26
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 21
- 239000007787 solid Substances 0.000 claims description 16
- 239000006071 cream Substances 0.000 claims description 15
- 239000008367 deionised water Substances 0.000 claims description 14
- 229910021641 deionized water Inorganic materials 0.000 claims description 14
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 13
- 238000001035 drying Methods 0.000 claims description 13
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 13
- 229910052710 silicon Inorganic materials 0.000 claims description 13
- 239000010703 silicon Substances 0.000 claims description 13
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- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 11
- 229910052697 platinum Inorganic materials 0.000 claims description 11
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- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 9
- 238000005406 washing Methods 0.000 claims description 9
- 238000001354 calcination Methods 0.000 claims description 8
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 claims description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 7
- 238000001816 cooling Methods 0.000 claims description 7
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- TZBAVQKIEKDGFH-UHFFFAOYSA-N n-[2-(diethylamino)ethyl]-1-benzothiophene-2-carboxamide;hydrochloride Chemical compound [Cl-].C1=CC=C2SC(C(=O)NCC[NH+](CC)CC)=CC2=C1 TZBAVQKIEKDGFH-UHFFFAOYSA-N 0.000 claims description 7
- 238000006243 chemical reaction Methods 0.000 claims description 6
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 6
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 4
- 239000010936 titanium Substances 0.000 claims description 4
- 229910052719 titanium Inorganic materials 0.000 claims description 4
- 239000004411 aluminium Substances 0.000 claims description 3
- 238000000227 grinding Methods 0.000 claims description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims 1
- 230000031709 bromination Effects 0.000 claims 1
- 238000005893 bromination reaction Methods 0.000 claims 1
- 125000000913 palmityl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 claims 1
- CLSUSRZJUQMOHH-UHFFFAOYSA-L platinum dichloride Chemical compound Cl[Pt]Cl CLSUSRZJUQMOHH-UHFFFAOYSA-L 0.000 claims 1
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- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical group [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 description 7
- 108010093096 Immobilized Enzymes Proteins 0.000 description 7
- FOSZYDNAURUMOT-UHFFFAOYSA-J azane;platinum(4+);tetrachloride Chemical compound N.N.N.N.[Cl-].[Cl-].[Cl-].[Cl-].[Pt+4] FOSZYDNAURUMOT-UHFFFAOYSA-J 0.000 description 7
- 238000006555 catalytic reaction Methods 0.000 description 7
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 6
- FPCJKVGGYOAWIZ-UHFFFAOYSA-N butan-1-ol;titanium Chemical compound [Ti].CCCCO.CCCCO.CCCCO.CCCCO FPCJKVGGYOAWIZ-UHFFFAOYSA-N 0.000 description 6
- 238000009826 distribution Methods 0.000 description 6
- SMZOGRDCAXLAAR-UHFFFAOYSA-N aluminium isopropoxide Chemical compound [Al+3].CC(C)[O-].CC(C)[O-].CC(C)[O-] SMZOGRDCAXLAAR-UHFFFAOYSA-N 0.000 description 5
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- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 3
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- 238000003915 air pollution Methods 0.000 description 3
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 3
- 230000036541 health Effects 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
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- 241000894006 Bacteria Species 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 239000003463 adsorbent Substances 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
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- 229910002092 carbon dioxide Inorganic materials 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
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- JKGITWJSGDFJKO-UHFFFAOYSA-N ethoxy(trihydroxy)silane Chemical compound CCO[Si](O)(O)O JKGITWJSGDFJKO-UHFFFAOYSA-N 0.000 description 1
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Abstract
本发明提供了一种降解甲醛的介孔复合材料及其制备方法,以介孔Al‑MCM‑41为基体材料,通过Al掺杂使得基体介孔材料具有较高的活性和较大的比表面积,且Pt‑TiO2/Al‑MCM‑41复合材料的比表面积高,确保复合材料较大的吸附能力。另一方面,本发明利用介孔材料的孔道限制效应有效阻止了纳米粒子的尺寸增长,确保其高的反应活性,同时利用贵金属Pt对纳米TiO2进行表面修饰,进一步提高了光催化剂的反应活性。因此,本发明制备的介孔复合材料对高浓度甲醛具有高效吸附降解能力。
Description
技术领域
本发明涉及无机催化材料技术领域,尤其涉及一种降解甲醛的介孔复合材料及其制备方法。
背景技术
据世界卫生组织发布报告,室内空气污染是危害现代家庭健康的头号杀手。消除室内空气污染,是促进现代家居健康的关键。世界各国科学家纷纷把攻克室内空气污染作为研究课题。
传统的室内有害气体如甲醛、苯系物的脱除方法一般会通过通风透气、摆放绿色植物、使用活性炭等方法去除,脱除的方式以物理吸附为主。使用固体活性炭脱除室内有害气体是利用活性炭的多孔特点,可以对甲醛等有害物质具有很强的吸附作用。但是该类型吸附剂只是将这些气体富集于吸附剂上,而未真正的将有害气体进行分解。
光触媒是一种最优质的除甲醛产品,光触媒在光的照射下,会产生类似光合作用的光催化反应,产生出氧化能力极强的自由氢氧基和活性氧,具有很强的光氧化还原功能,可氧化分解各种有机化合物和部分无机物,能破坏细菌的细胞膜和固化病毒的蛋白质,可杀灭细菌和分解有机污染物,把有机污染物分解成无污染的水(H2O)、二氧化碳(CO2)和其它无害物质,因而具有极强的杀菌、除臭、防霉、防污自洁、净化空气功能。申请号为201310738713的中国专利文献报道了一种一种除甲醛纳米混合物及其制备方法,利用纳米氧化钛以及与其他物质复合作为光触媒去除甲醛,其48小时对甲醛的去除率可达85%。但是,纳米TiO2对甲醛的光降解是接触反应,由于纳米TiO2本身并不具备较大的比表面积和高的吸附活性,因此对甲醛的去除率受限于吸附到纳米TiO2颗粒表面的甲醛量;此外,纳米TiO2针对低浓度甲醛具有较高的活性,但对高浓度甲醛却不能有效的降解,同时单一纳米TiO2在光催化反应过程中的活性也受到很大的限制。
因此,开发出一种对高浓度甲醛具有高效降解能力的复合功能材料具有十分重要的现实意义。
发明内容
本发明解决的技术问题在于提供一种降解甲醛的介孔复合材料及其制备方法,该介孔复合材料对高浓度甲醛具有高效吸附降解能力。
有鉴于此,本发明提供了一种降解甲醛的介孔复合材料的制备方法,包括以下步骤:
将铂源化合物溶于去离子水中,搅拌后得到第一溶液;
将TiO2/Al-MCM-41超声分散于所述第一溶液中,搅拌,然后在80℃的水浴中继续搅拌,得到膏状固体;
将所述膏状固体烘干、研磨,在300-350℃下煅烧,得到Pt-TiO2/Al-MCM-41复合材料。
优选的,所述铂源化合物为二氯四氨合铂。
优选的,所述TiO2/Al-MCM-41按照如下方法制备:
将钛源化合物与无水乙醇混合,搅拌后得到第二溶液;
将Al-MCM-41加入所述第二溶液中,超声分散后得到悬浮液;
向所述悬浮液中加入蒸馏水得到溶胶,继续搅拌30min后将溶胶置于80℃的水浴中继续搅拌得到干凝胶,冷却后磨细,在500℃下煅烧后得到TiO2/Al-MCM-41。
优选的,所述Al-MCM-41按照如下方法制备:
将重量比为2∶1的模板剂和聚乙二醇4000溶解到去离子水中,在50℃的水浴中搅拌溶解均匀,得到第三溶液;
将硅源化合物和铝源化合物加入所述第三溶液中,调节pH值得到溶胶液;
将所述溶胶液转移至反应釜进行水热反应,抽滤、洗涤、烘干后得到固体产物,在550℃下煅烧,得到Al-MCM-41介孔材料。
优选的,所述模板剂为十六烷基三甲基溴化铵。
优选的,所述硅源化合物为正硅酸乙酯,铝源化合物为正硅酸乙酯。
优选的,所述硅源化合物和铝源化合物按照硅与铝的摩尔比为20-40∶1进行投料。
优选的,所述水热反应的温度为110-120℃,水热反应的时间为24-36h。
优选的,还包括:将Pt-TiO2/Al-MCM-41复合材料放入锥形瓶中,加入pH为7.0的磷酸盐缓冲溶液和甲醛溶解酶溶液,滴加7.5%的交联剂溶液至体积分数为0.75%,在恒温水浴振荡器中以180r/min转速在20℃恒温震荡2h,抽滤,利用pH为7.0的磷酸盐缓冲溶液洗涤,冷冻干燥后得到固定化酶催化剂。
相应的,本发明还提供一种降解甲醛的介孔复合材料,为Pt-TiO2/Al-MCM-41固定化酶复合材料。
本发明提供了一种降解甲醛的介孔复合材料及其制备方法,包括以下步骤:将铂源化合物溶于去离子水中,搅拌后得到第一溶液;将TiO2/Al-MCM-41超声分散于所述第一溶液中,搅拌,然后在80℃的水浴中继续搅拌,得到膏状固体;将所述膏状固体烘干、研磨,在300-350℃下煅烧,得到Pt-TiO2/Al-MCM-41复合材料。与现有技术相比,本发明以介孔Al-MCM-41为基体材料,通过Al掺杂使得基体介孔材料具有较高的活性和较大的比表面积,且Pt-TiO2/Al-MCM-41复合材料的比表面积高,确保复合材料较大的吸附能力。另一方面,本发明利用介孔材料的孔道限制效应有效阻止了纳米粒子的尺寸增长,确保其高的反应活性,同时利用贵金属Pt对纳米TiO2进行表面修饰,进一步提高了光催化剂的反应活性。因此,本发明制备的介孔复合材料对高浓度甲醛具有高效吸附降解能力。
具体实施方式
为了进一步理解本发明,下面结合实施例对本发明优选实施方案进行描述,但是应当理解,这些描述只是为进一步说明本发明的特征和优点,而不是对本发明权利要求的限制。
本发明实施例公开了一种降解甲醛的介孔复合材料的制备方法,包括以下步骤:将铂源化合物溶于去离子水中,搅拌后得到第一溶液;将TiO2/Al-MCM-41超声分散于所述第一溶液中,搅拌,然后在80℃的水浴中继续搅拌,得到膏状固体;将所述膏状固体烘干、研磨,在300-350℃下煅烧,得到Pt-TiO2/Al-MCM-41复合材料。作为优选方案,所述铂源化合物为二氯四氨合铂。得到Pt-TiO2/Al-MCM-41复合材料的步骤中,膏状固体的烘干温度优选为90-130℃,更优选为100-120℃,更优选为110℃;烘干时间优选为3-10h,更优选为4-8h,更优选为5h;煅烧温度优选为310-340℃,更优选为320℃;煅烧时间优选为1-5h,更优选为2h;煅烧程序升温速率优选为0.5-2℃/min,更优选为1℃/min。
本发明制备的Pt-TiO2/Al-MCM-41复合材料,纳米TiO2和纳米Pt粒子均匀组装到基体介孔材料Al-MCM-41的孔道中,纳米Pt粒子的尺寸优选为2-3nm;复合材料的孔径集中分布在3-4nm,孔容优选为1.0-1.2cm3/g,比表面积优选为980-1020m2/g。介孔硅基纳米复合材料中,TiO2所占质量分数优选为10-15%,Pt所占质量分数优选为0.5-0.8%。
作为优选方案,所述TiO2/Al-MCM-41按照如下方法制备:将钛源化合物与无水乙醇混合,搅拌后得到第二溶液;将Al-MCM-41加入所述第二溶液中,超声分散后得到悬浮液;向所述悬浮液中加入蒸馏水得到溶胶,继续搅拌30min后将溶胶置于80℃的水浴中继续搅拌得到干凝胶,冷却后磨细,在500℃下煅烧后得到TiO2/Al-MCM-41。其中,所述钛源化合物优选为钛酸丁酯。
得到第二溶液的步骤中,搅拌时间优选为20-60min,更优选为30min;得到悬浮液的步骤中,超声分散的时间优选为10-30min,更优选为15min;得到TiO2/Al-MCM-41的步骤中,煅烧程序升温速率优选为0.5-2℃/min,更优选为1℃/min。
上述制备的TiO2/Al-MCM-41中,纳米TiO2的晶体结构为锐钛矿型。
作为优选方案,所述Al-MCM-41按照以下方法制备:将重量比为2∶1的模板剂和聚乙二醇4000溶解到去离子水中,在50℃的水浴中搅拌溶解均匀,得到第三溶液;将硅源化合物和铝源化合物加入所述第三溶液中,调节pH值得到溶胶液;将所述溶胶液转移至反应釜进行水热反应,抽滤、洗涤、烘干后得到固体产物,在550℃下煅烧,得到Al-MCM-41介孔材料。
其中,所述模板剂优选为十六烷基三甲基溴化铵;所述硅源化合物优选为正硅酸乙酯,铝源化合物优选为正硅酸乙酯。所述硅源化合物和铝源化合物优选按照硅与铝的摩尔比为20-40∶1进行投料。所述水热反应的温度优选为110-120℃,水热反应的时间优选为24-36h。所述溶胶液的pH值优选为10-11。得到Al-MCM-41介孔材料的步骤中,煅烧程序升温速率优选为0.5-2℃/min,更优选为1℃/min
上述制备的Al-MCM-41为Al掺杂MCM-41,成分是Al掺杂介孔硅,其中,MCM-41是介孔材料的一种。Al-MCM-41的孔径优选集中分布在3-3.8nm,孔容优选为0.8-1.1cm3/g,比表面积优选为1024-1156m2/g。
作为优选方案,本发明还包括:将Pt-TiO2/Al-MCM-41复合材料放入锥形瓶中,加入pH为7.0的磷酸盐缓冲溶液和甲醛溶解酶溶液,滴加7.5%的交联剂溶液至体积分数为0.75%,在恒温水浴振荡器中以180r/min转速在20℃恒温震荡2h,抽滤,利用pH为7.0的磷酸盐缓冲溶液洗涤,冷冻干燥后得到固定化酶催化剂。其中,所述的交联剂优选为戊二醛。上述步骤具体为:称取0.5g的Pt-TiO2/Al-MCM-41复合材料放入锥形瓶中,加入20ml的pH=7.0的磷酸盐缓冲溶液、10ml的甲醛溶解酶溶液(含有有效酶含量为15mg,利用pH=7.0的磷酸盐缓冲溶液配制),并滴加7.5%的交联剂溶液至体积分数为0.75%,至于恒温水浴振荡器中在180r/min转速20℃恒温震荡2h,抽滤,用pH7.0的磷酸盐缓冲溶液洗涤、冷冻干燥得到固定化酶催化剂。
本发明制备的固定化酶催化剂在48h内对20g/L浓度的甲醛降解率为99%,对0.1g/L的甲醛降解率为99%。
从以上方案可以看出,本发明制备的协同降解甲醛的介孔复合材料具有如下积极效果:
(1)、以介孔Al-MCM-41为基体材料,通过Al掺杂使得基体介孔材料具有较高的活性和较大的比表面积,高达1024-1156m2/g,所得Pt-TiO2/Al-MCM-41复合材料的比表面积仍高达980-1020m2/g,确保复合材料较大的吸附能力。
(2)、通过介孔材料的孔道限制效应有效阻止了纳米粒子的尺寸增长,确保其高的反应活性,同时利用贵金属Pt对纳米TiO2进行表面修饰,进一步提高了光催化剂的反应活性。
(3)、优选采用固定甲醛溶解酶,可以有效发挥生物酶对高浓度甲醛降解的特性,与光催化剂高效催化降解低浓度甲醛形成协同效应,可以有效吸附降解高浓度甲醛。
为了进一步理解本发明,下面结合实施例对本发明提供的技术方案进行详细说明,本发明的保护范围不受以下实施例的限制。
本实施例中所用化学试剂均为市售。其中十六烷基三甲基溴化铵、聚乙二醇4000、钛酸丁酯均产自天津科密欧化学试剂有限公司,正硅酸乙酯和异丙醇铝产自国药集团化学试剂有限公司,二氯四氨合铂产自sigma aldrich公司。
实施例1
(1)、制备基体介孔材料Al-MCM-41。首先称取2g的十六烷基三甲基溴化铵和1g的聚乙二醇4000溶解到100mL的去离子水中,在50℃的水浴中搅拌溶解均匀,然后称取2.08g的正硅酸乙酯、0.102g异丙醇铝加入上述溶液中,调节上述溶液的pH值为10.0得到乳白色溶胶,将所得溶胶液转移反应釜,在110℃下进行水热反应,反应24h后,抽滤、洗涤烘干得到固体产物,将固体产物在550℃下按照1℃/min的程序升温速率煅烧6h,获得Al-MCM-41介孔材料,材料中Si/Al摩尔比为20,所得基体Al-MCM-41介孔材料孔径集中分布在3.2nm,孔容0.9cm3/g,比表面积为1056m2/g;
(2)、制备TiO2/Al-MCM-41。室温下量取0.86g的钛酸丁酯50ml的无水乙醇混合,搅拌30min得到均匀透明的黄色溶液,称取2g的Al-MCM-41介孔材料加入到上述溶液中,超声分散15min得到均匀的悬浮液,然后逐滴加入10ml的蒸馏水获得溶胶,继续搅拌30min后将溶胶置于80℃的水浴中继续搅拌获得干凝胶,冷却后磨细、按照1℃/min的升温速率在500℃下煅烧2h得到TiO2/Al-MCM-41介孔材料;
(3)、制备Pt-TiO2/Al-MCM-41。称取0.017g的二氯四氨合铂溶于去离子水中,搅拌30min得到透明的溶液,称取2g的TiO2/Al-MCM-41介孔材料超声分散于上述溶液中得到混合液,将上述混合液搅拌6h后转移至80℃的水浴中继续搅拌蒸发多余水分得到膏状固体,将所得膏状固体在110℃下烘干5h后磨细,最后按照1℃/min的升温速率在320℃下煅烧2h得到Pt-TiO2/Al-MCM-41复合材料;复合材料的孔径集中分布在3.4nm,孔容1.0cm3/g,比表面积为984m2/g;TiO2在复合材料中所占质量分数为5.2%,Pt所占质量分数为0.5%。Pt-TiO2/Al-MCM-41复合材料在48h内对20g/L浓度的甲醛降解率为52%,对0.1g/L的甲醛降解率为98%。
实施例2
(1)、制备基体介孔材料Al-MCM-41。首先称取2g的十六烷基三甲基溴化铵和1g的聚乙二醇4000溶解到100mL的去离子水中,在50℃的水浴中搅拌溶解均匀,然后称取2.08g的正硅酸乙酯、0.051g异丙醇铝加入上述溶液中,调节上述溶液的pH值为11.0得到乳白色溶胶,将所得溶胶液转移反应釜,在120℃下进行水热反应,反应32h后,抽滤、洗涤烘干得到固体产物,将固体产物在550℃下按照1℃/min的程序升温速率煅烧6h,获得Al-MCM-41介孔材料,材料中Si/Al摩尔比为40,所得基体Al-MCM-41介孔材料孔径集中分布在3.8nm,孔容1.1cm3/g,比表面积为1148m2/g;
(2)、制备TiO2/Al-MCM-41。室温下量取0.86g的钛酸丁酯与50ml的无水乙醇混合,搅拌30min得到均匀透明的黄色溶液,称取1.3g的Al-MCM-41介孔材料加入到上述溶液中,超声分散15min得到均匀的悬浮液,然后逐滴加入10ml的蒸馏水获得溶胶,继续搅拌30min后将溶胶置于80℃的水浴中继续搅拌获得干凝胶,冷却后磨细、按照1℃/min的升温速率在500℃下煅烧2h得到TiO2/Al-MCM-41介孔材料;
(3)、制备Pt-TiO2/Al-MCM-41。称取0.017g的二氯四氨合铂溶于去离子水中,搅拌30min得到透明的溶液,称取1.8g的TiO2/Al-MCM-41介孔材料超声分散于上述溶液中得到混合液,将上述混合液搅拌6h后转移至80℃的水浴中继续搅拌蒸发多余水分得到膏状固体,将所得膏状固体在110℃下烘干5h后磨细,最后按照1℃/min的升温速率在320℃下煅烧2h得到Pt-TiO2/Al-MCM-41复合材料;
(4)制备Pt-TiO2/Al-MCM-41固定化酶。称取0.5g的Pt-TiO2/Al-MCM-41复合材料放入锥形瓶中,加入20ml的pH=7.0的磷酸盐缓冲溶液、10ml的甲醛溶解酶溶液(含有有效酶含量为15mg,利用pH=7.0的磷酸盐缓冲溶液配制),并滴加7.5%的戊二醛溶液至体积分数为0.75%,至于恒温水浴振荡器中在180r/min转速20℃恒温震荡2h,抽滤,用pH7.0的磷酸盐缓冲溶液洗涤、冷冻干燥得到Pt-TiO2/Al-MCM-41固定化酶复合材料。复合材料的孔径集中分布在4.0nm,孔容1.2cm3/g,比表面积为1020m2/g;TiO2在复合材料中所占质量分数为6.0%,Pt所占质量分数为0.8%;复合材料在48h内对20g/L浓度的甲醛降解率为98%,对0.1g/L的甲醛降解率为99%。
实施例3
(1)、制备基体介孔材料Al-MCM-41。首先称取2g的十六烷基三甲基溴化铵和1g的聚乙二醇4000溶解到100mL的去离子水中,在50℃的水浴中搅拌溶解均匀,然后称取2.08g的正硅酸乙酯、0.068g异丙醇铝加入上述溶液中,调节上述溶液的pH值为10.0得到乳白色溶胶,将所得溶胶液转移反应釜,在110℃下进行水热反应,反应36h后,抽滤、洗涤烘干得到固体产物,将固体产物在550℃下按照1℃/min的程序升温速率煅烧6h,获得Al-MCM-41介孔材料,材料中Si/Al摩尔比为30,所得基体Al-MCM-41介孔材料孔径集中分布在3.0nm,孔容0.8cm3/g,比表面积为1024m2/g;
(2)、制备TiO2/Al-MCM-41。室温下量取0.86g的钛酸丁酯与50ml的无水乙醇混合,搅拌30min得到均匀透明的黄色溶液,称取1.3g的Al-MCM-41介孔材料加入到上述溶液中,超声分散15min得到均匀的悬浮液,然后逐滴加入10ml的蒸馏水获得溶胶,继续搅拌30min后将溶胶置于80℃的水浴中继续搅拌获得干凝胶,冷却后磨细、按照1℃/min的升温速率在500℃下煅烧2h得到TiO2/Al-MCM-41介孔材料;
(3)、制备Pt-TiO2/Al-MCM-41。称取0.017g的二氯四氨合铂溶于去离子水中,搅拌30min得到透明的溶液,称取1.8g的TiO2/Al-MCM-41介孔材料超声分散于上述溶液中得到混合液,将上述混合液搅拌6h后转移至80℃的水浴中继续搅拌蒸发多余水分得到膏状固体,将所得膏状固体在110℃下烘干5h后磨细,最后按照1℃/min的升温速率在320℃下煅烧2h得到Pt-TiO2/Al-MCM-41复合材料;
(4)制备Pt-TiO2/Al-MCM-41固定化酶。称取0.5g的Pt-TiO2/Al-MCM-41复合材料放入锥形瓶中,加入20ml的pH=7.0的磷酸盐缓冲溶液、10ml的甲醛溶解酶溶液(含有有效酶含量为15mg,利用pH=7.0的磷酸盐缓冲溶液配制),并滴加7.5%的戊二醛溶液至体积分数为0.75%,至于恒温水浴振荡器中在180r/min转速20℃恒温震荡2h,抽滤,用pH7.0的磷酸盐缓冲溶液洗涤、冷冻干燥得到Pt-TiO2/Al-MCM-41固定化酶复合材料。复合材料的孔径集中分布在3.2nm,孔容0.9cm3/g,比表面积为984m2/g;TiO2在复合材料中所占质量分数为5.8%,Pt所占质量分数为0.7%;复合材料在48h内对20g/L浓度的甲醛降解率为99%,对0.1g/L的甲醛降解率为99%。
实施例4
(1)、制备基体介孔材料Al-MCM-41。首先称取2g的十六烷基三甲基溴化铵和1g的聚乙二醇4000溶解到100mL的去离子水中,在50℃的水浴中搅拌溶解均匀,然后称取2.08g的正硅酸乙酯、0.102g异丙醇铝加入上述溶液中,调节上述溶液的pH值为10.5得到乳白色溶胶,将所得溶胶液转移反应釜,在115℃下进行水热反应,反应28h后,抽滤、洗涤烘干得到固体产物,将固体产物在550℃下按照1℃/min的程序升温速率煅烧6h,获得Al-MCM-41介孔材料,材料中Si/Al摩尔比为20,所得基体Al-MCM-41介孔材料孔径集中分布在3.6nm,孔容0.9cm3/g,比表面积为1135m2/g;
(2)、制备TiO2/Al-MCM-41。室温下量取0.86g的钛酸丁酯与50ml的无水乙醇混合,搅拌30min得到均匀透明的黄色溶液,称取2g的Al-MCM-41介孔材料加入到上述溶液中,超声分散15min得到均匀的悬浮液,然后逐滴加入10ml的蒸馏水获得溶胶,继续搅拌30min后将溶胶置于80℃的水浴中继续搅拌获得干凝胶,冷却后磨细、按照1℃/min的升温速率在500℃下煅烧2h得到TiO2/Al-MCM-41介孔材料;
(3)、制备Pt-TiO2/Al-MCM-41。称取0.017g的二氯四氨合铂溶于去离子水中,搅拌30min得到透明的溶液,称取2g的TiO2/Al-MCM-41介孔材料超声分散于上述溶液中得到混合液,将上述混合液搅拌6h后转移至80℃的水浴中继续搅拌蒸发多余水分得到膏状固体,将所得膏状固体在110℃下烘干5h后磨细,最后按照1℃/min的升温速率在320℃下煅烧2h得到Pt-TiO2/Al-MCM-41复合材料;
(4)制备Pt-TiO2/Al-MCM-41固定化酶。称取0.5g的Pt-TiO2/Al-MCM-41复合材料放入锥形瓶中,加入20ml的pH=7.0的磷酸盐缓冲溶液、10ml的甲醛溶解酶溶液(含有有效酶含量为15mg,利用pH=7.0的磷酸盐缓冲溶液配制),并滴加7.5%的戊二醛溶液至体积分数为0.75%,至于恒温水浴振荡器中在180r/min转速20℃恒温震荡2h,抽滤,用pH7.0的磷酸盐缓冲溶液洗涤、冷冻干燥得到Pt-TiO2/Al-MCM-41固定化酶复合材料。复合材料的孔径集中分布在3.8nm,孔容1.0cm3/g,比表面积为995m2/g;TiO2在复合材料中所占质量分数为5.6%,Pt所占质量分数为0.6%;复合材料在48h内对20g/L浓度的甲醛降解率为99%,对0.1g/L的甲醛降解率为98%。
以上实施例的说明只是用于帮助理解本发明的方法及其核心思想。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,还可以对本发明进行若干改进和修饰,这些改进和修饰也落入本发明权利要求的保护范围内。
对所公开的实施例的上述说明,使本领域专业技术人员能够实现或使用本发明。对这些实施例的多种修改对本领域的专业技术人员来说将是显而易见的,本文中所定义的一般原理可以在不脱离本发明的精神或范围的情况下,在其它实施例中实现。因此,本发明将不会被限制于本文所示的这些实施例,而是要符合与本文所公开的原理和新颖特点相一致的最宽的范围。
Claims (2)
1.一种降解甲醛的介孔复合材料的制备方法,其特征在于,包括以下步骤:
将铂源化合物溶于去离子水中,搅拌后得到第一溶液,所述铂源化合物为二氯四氨合铂;
将TiO2/Al-MCM-41超声分散于所述第一溶液中,搅拌,然后在80℃的水浴中继续搅拌,得到膏状固体,
所述TiO2/Al-MCM-41按照如下方法制备:将钛源化合物与无水乙醇混合,搅拌后得到第二溶液;将Al-MCM-41加入所述第二溶液中,超声分散后得到悬浮液;向所述悬浮液中加入蒸馏水得到溶胶,继续搅拌30min后将溶胶置于80℃的水浴中继续搅拌得到干凝胶,冷却后磨细,在500℃下煅烧后得到TiO2/Al-MCM-41,
所述Al-MCM-41按照如下方法制备:将重量比为2:1的模板剂和聚乙二醇4000溶解到去离子水中,在50℃的水浴中搅拌溶解均匀,得到第三溶液;将硅源化合物和铝源化合物加入所述第三溶液中,调节pH值得到溶胶液;将所述溶胶液转移至反应釜进行水热反应,抽滤、洗涤、烘干后得到固体产物,在550℃下煅烧,得到Al-MCM-41介孔材料,所述硅源化合物为正硅酸乙酯,所述硅源化合物和铝源化合物按照硅与铝的摩尔比为20-40:1进行投料,所述水热反应的温度为110-120℃,水热反应的时间为24-36h;
将所述膏状固体烘干、研磨,在300-350℃下煅烧,得到Pt-TiO2/Al-MCM-41复合材料。
2.根据权利要求1所述的制备方法,其特征在于,所述模板剂为十六烷基三甲基溴化铵。
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