CN110240194A - 一种卵状透明碳包裹单晶二氧化钛微球、制备方法及其应用 - Google Patents
一种卵状透明碳包裹单晶二氧化钛微球、制备方法及其应用 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 95
- 239000004408 titanium dioxide Substances 0.000 title claims abstract description 39
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 37
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 36
- 239000013078 crystal Substances 0.000 title claims abstract description 31
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 238000006243 chemical reaction Methods 0.000 claims abstract description 22
- 239000000463 material Substances 0.000 claims abstract description 19
- 230000015556 catabolic process Effects 0.000 claims abstract description 16
- 238000006731 degradation reaction Methods 0.000 claims abstract description 16
- 238000000034 method Methods 0.000 claims abstract description 11
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- 230000001699 photocatalysis Effects 0.000 claims abstract description 5
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- 238000007146 photocatalysis Methods 0.000 claims abstract description 3
- 239000000356 contaminant Substances 0.000 claims abstract 2
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 claims description 10
- FDZZZRQASAIRJF-UHFFFAOYSA-M malachite green Chemical compound [Cl-].C1=CC(N(C)C)=CC=C1C(C=1C=CC=CC=1)=C1C=CC(=[N+](C)C)C=C1 FDZZZRQASAIRJF-UHFFFAOYSA-M 0.000 claims description 7
- 229940107698 malachite green Drugs 0.000 claims description 7
- 239000013049 sediment Substances 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 229960005070 ascorbic acid Drugs 0.000 claims description 5
- 235000010323 ascorbic acid Nutrition 0.000 claims description 5
- 239000011668 ascorbic acid Substances 0.000 claims description 5
- 239000008367 deionised water Substances 0.000 claims description 5
- 229910021641 deionized water Inorganic materials 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 5
- XROWMBWRMNHXMF-UHFFFAOYSA-J titanium tetrafluoride Chemical compound [F-].[F-].[F-].[F-].[Ti+4] XROWMBWRMNHXMF-UHFFFAOYSA-J 0.000 claims description 5
- 239000011258 core-shell material Substances 0.000 claims description 4
- 239000000843 powder Substances 0.000 claims description 3
- 239000006228 supernatant Substances 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims description 3
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 claims 1
- 238000001027 hydrothermal synthesis Methods 0.000 abstract description 2
- 230000007613 environmental effect Effects 0.000 abstract 1
- 239000002994 raw material Substances 0.000 abstract 1
- 230000035484 reaction time Effects 0.000 abstract 1
- 239000002086 nanomaterial Substances 0.000 description 7
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 5
- 238000001228 spectrum Methods 0.000 description 4
- 230000015572 biosynthetic process Effects 0.000 description 3
- 239000002131 composite material Substances 0.000 description 3
- 238000005286 illumination Methods 0.000 description 3
- 239000005416 organic matter Substances 0.000 description 3
- 238000003786 synthesis reaction Methods 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 238000002835 absorbance Methods 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 239000003575 carbonaceous material Substances 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 229960000935 dehydrated alcohol Drugs 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 238000000870 ultraviolet spectroscopy Methods 0.000 description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000013065 commercial product Substances 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 230000005518 electrochemistry Effects 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 229910021389 graphene Inorganic materials 0.000 description 1
- 230000004298 light response Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 1
- 230000000116 mitigating effect Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002071 nanotube Substances 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 239000002957 persistent organic pollutant Substances 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 238000012876 topography Methods 0.000 description 1
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- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G23/00—Compounds of titanium
- C01G23/04—Oxides; Hydroxides
- C01G23/047—Titanium dioxide
- C01G23/053—Producing by wet processes, e.g. hydrolysing titanium salts
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- 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
- B01J21/18—Carbon
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Abstract
本发明公开了一种卵状透明碳包裹单晶二氧化钛的制备方法和应用。本发明采用一步水热法合成碳包裹单晶二氧化钛微球。微球尺寸为1~1.5微米,其中外壳碳层为无定型微孔状结构、内核二氧化钛为锐钛矿相。该方法操作简便,工艺设备简单,原料易得,制备成本较低,反应周期短,可重复性高。这种材料应用在光催化降解有机污染物方面有着突出的性能。这种新型卵状透明碳包裹单晶二氧化钛在环境科学以及太阳能转换领域有着非常重要的用途。
Description
技术领域
本发明属于一种具有核壳结构碳包裹单晶二氧化钛纳米材料,该材料采用一步水热法制备而成,在光催化降解有机物方面具备优异性能,在其他能源开发和环境保护领域也具备潜在应用性能。
背景技术
TiO2半导体因其长期的热力学稳定性,强氧化能力和相对无毒性而被认为是最好的光催化材料之一。另外,普通TiO2多晶型物,金红石和锐钛矿的大多数应用由于其大于3eV的带隙而限于光谱的UV光区域,这使得在TiO2对于太阳光利用率很低。近几十年来,已经做了许多研究来改变TiO2的电子能带结构,以试图利用更大部分的太阳光。为了增加可见光吸收,已经采用了许多缩小带隙的方法,最常用的方法是用碳材料掺杂TiO2,来提高光催化效率。碳材料表现出优异的导电性,优异的化学和电化学稳定性,物理性质和良好的光响应。基于石墨烯的材料与其它材料的结合可以改善电子导电性和稳定性,并且具有独特的结构和低毒性,以及它们优异的电子,热,电化学和机械性能。根据最近的研究,TiO2/碳基材料的复合材料可以整合优势,完美地减轻各个组件的缺点,使复合材料具有更高的稳定性,增强的导电性,高选择性和模板效果,碳改性的TiO2已在文献中广泛描述,(石墨烯-TiO2纳米管,碳量子点/TiO2复合材料。然而对于碳层包裹单晶TiO2很少得到关注。本发明中我们设计了一种碳包裹单晶二氧化钛纳米材料,该材料作为稳定高效且可见光响应的光催化剂,在模拟太阳光下对有机污染物有很高的降解效果。
发明内容
鉴于以上问题,本发明的目的是提供一种具有卵状透明结构的碳包裹单晶二氧化钛纳米材料及其制备方法和应用,制备方法简单,成本低。所制备的纳米材料具有优异的光催化降解性能。合成过程中不需要复杂的仪器、操作简单,有利于大规模的生产。
为实现上述目的,本发明采用如下技术方案:
一种核壳结构碳包裹单晶二氧化钛纳米材料,所述纳米材料尺寸为1~1.5微米,其中外壳碳层为微孔无定型结构,内核二氧化钛晶形为锐钛矿相。
一种核壳结构碳包裹单晶二氧化钛纳米材料的制备方法,包括如下步骤:
(1)在反应釜的聚四氟乙烯内衬中加入去离子水(20ml)和抗坏血酸(0.12-0.28g),再将配好的四氟化钛溶液(浓度为53毫摩尔,10毫升)加入反应釜中。然后,再加入HF(0.4ml)溶液,搅拌均匀后将混合液至于高温高压反应釜中,放入180℃烘箱,反应3.5小时;
(2)待反应釜冷却到室温,吸取上层清液弃掉。将下层沉淀用去离子水洗涤3次,再用无水乙醇洗涤1次。洗涤完成后将沉淀物放入烘箱中在60℃下真空干燥12小时,得到碳包裹单晶二氧化钛材料,颜色为黑色粉末,其中二氧化钛晶相为锐钛矿相。
上述碳包裹单晶二氧化钛材料的应用,用于光催化降解有机物。
上述应用方法如下:在模拟太阳光下,碳包裹单晶二氧化钛微球对孔雀石绿(10mg/L)的降解光催化活性。10~20毫克催化剂加入到50~100毫升染料中,光照情况下,对反应溶液进行每隔五分钟取一次样,通过UV-vis光谱法测量孔雀石绿的最高吸光度的变化,测试表明,在模拟太阳光下光照30分钟的降解率达到95%。
本发明的有益效果在于:
(1)采用简单的一步水热法合成卵状透明碳包裹单晶二氧化钛微球材料,合成方法简单,操作简便,条件温和,目标产物纯度高,安全无毒,可以大批量合成;
(2)将纳米尺寸碳包裹单晶二氧化钛微球材料来光催化降解有机物,结果表明其具有较好的光催化降解性能和较好的稳定性。在模拟太阳光下光照射30分钟对孔雀石绿的降解率达到95%;
(3)制备过程中,所有试剂均为商业产品,不需要进一步处理;
(4)合成方法简单,得到的材料易于应用,有利于在工业化生产中推广应用,用于污水净化、光降解污染物工艺材料。
附图说明
图1是实施例1所制备的卵状透明碳包裹单晶二氧化钛微球材料的电子照片;
图2是实施例1所制备的卵状透明碳包裹单晶二氧化钛微球材料作为光降解催化剂的性能图;
图3是实施例1所制备的卵状透明碳包裹单晶二氧化钛微球材料X射线衍射图谱
图4是实施例1所制备的卵状碳包裹单晶二氧化钛微球材料的透射电镜图片;
图5是实施例1所制备的卵状碳包裹单晶二氧化钛微球材料扫描电镜图片。
具体实施方式
实施例1
步骤一、卵状透明碳包裹单晶二氧化钛微球材料的制备
(1)在反应釜的聚四氟乙烯内衬中加入去离子水(20ml)和抗坏血酸(0.28g),再将配好的四氟化钛溶液(浓度为53毫摩尔,10毫升)加入反应釜中。然后,再加入HF(0.4ml)溶液,搅拌均匀后将混合液至于高温高压反应釜中,放入180℃烘箱,反应3.5小时;
(2)待反应釜冷却到室温,吸取上层清液弃掉。将下层沉淀用去离子水洗涤6次,再用无水乙醇洗涤1次。洗涤完成后将沉淀物放入60℃烘箱真空干燥12小时,得到碳包裹单晶二氧化钛材料,颜色为黑色粉末,其中二氧化钛晶相为锐钛矿相。
步骤二、性能表征测试
在模拟太阳光下,碳包裹单晶二氧化钛微球对孔雀石绿(10mg/L)的降解光催化活性。10~20毫克催化剂加入到50~100毫升染料中,光照情况下,对反应溶液进行每隔五分钟取一次样,通过UV-vis光谱法测量孔雀石绿的最高吸光度的变化,测试表明,在模拟太阳光下光照30分钟的降解率达到95%。
图2是实施例1所制备的卵状碳包裹单晶二氧化钛微球光催化降解的性能图。其中:曲线1是以实施例1所制备的卵状碳包裹单晶二氧化钛微球光降解性能图,模拟太阳光照射下,降解50毫升20毫克/升孔雀石绿溶液的测试条件下的光降解曲线。从图2可知,在模拟太阳光下光照30分钟的降解率达到95%。
图3为产品的X射线衍射图谱,曲线是所制备的卵状透明碳包裹单晶二氧化钛微球在扫描速度为3°/min,扫描范围为10°-80°的X射线衍射图谱。
图4为实施例1透射电镜图,通过观察样品为明显的卵状透明碳包裹二氧化钛微球结构。
图5为实施例1扫描电镜图,通过观察样品形貌,其为1~1.5微米卵状透明碳包裹二氧化钛微球结构。
实施例2
步骤一、卵状透明碳包裹二氧化钛微球的制备
在反应釜的聚四氟乙烯内衬中加入去离子水(20ml)和抗坏血酸(0.14g),再将配好的四氟化钛溶液(浓度为53毫摩尔,10毫升)加入反应釜中。然后,再加入HF(0.4ml)溶液,搅拌均匀后将混合液至于高温高压反应釜中,放入180℃烘箱,反应3.5小时,特征和性能与实施例1类似。
实施例3
步骤一、卵状透明碳包裹二氧化钛微球的制备
在反应釜的聚四氟乙烯内衬中加入去离子水(20ml)和抗坏血酸(0.12g),再将配好的四氟化钛溶液(浓度为53毫摩尔,10毫升)加入反应釜中。然后,再加入HF(0.4ml)溶液,搅拌均匀后将混合液至于高温高压反应釜中,放入180℃烘箱,反应3.5小时,特征和性能与实施例1类似。
以上所述仅为本发明的较佳实施例,凡依本发明申请专利范围所做的均等变化与修饰,皆应属本发明的涵盖范围。
Claims (4)
1.一种卵状透明碳包裹单晶二氧化钛微球,其特征在于,所述微球尺寸为1~1.5微米,其中外壳碳层为无定型微孔状结构、内核二氧化钛为锐钛矿相。
2.一种卵状透明碳包裹单晶二氧化钛微球的制备方法,其特征在于,包括如下步骤:
(1)在反应釜的聚四氟乙烯内衬中加入去离子水(20ml)和抗坏血酸(0.12-0.28g),再将配好的四氟化钛溶液(浓度为53毫摩尔)加入反应釜中。然后,再加入HF(0.4ml)溶液,搅拌均匀后将混合液至于高温高压反应釜中,放入180℃烘箱,反应3.5小时;
(2)待反应釜冷却到室温,吸取上层清液弃掉。将下层沉淀用去离子水洗涤3次,再用无水乙醇洗涤1次。洗涤完成后将沉淀物放入烘箱在60℃下真空干燥12小时,得到碳包裹单晶二氧化钛材料,颜色为黑色粉末,其中二氧化钛晶相为锐钛矿相。
3.权利要求1所述卵状透明碳包裹单晶二氧化钛球的应用,其特征在于,所述核壳结构微球用于光催化降解有机污染物。
4.根据权利要求3所述的应用,其特征在于,应用方法如下:在模拟太阳光下,碳包裹单晶二氧化钛微球对孔雀石绿(10mg/L)的降解光催化活性。
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