CN109012738A - 一种制备钒铋氧化物分子筛的方法 - Google Patents
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- 239000002808 molecular sieve Substances 0.000 title claims abstract description 35
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 title claims abstract description 35
- DPSWNBLFKLUQTP-UHFFFAOYSA-N bismuth vanadium Chemical compound [V].[Bi] DPSWNBLFKLUQTP-UHFFFAOYSA-N 0.000 title claims abstract description 21
- 238000000034 method Methods 0.000 title claims abstract description 15
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 22
- 239000007787 solid Substances 0.000 claims abstract description 22
- 229910052797 bismuth Inorganic materials 0.000 claims abstract description 17
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 claims abstract description 17
- 229910052720 vanadium Inorganic materials 0.000 claims abstract description 17
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 claims abstract description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 11
- 239000000203 mixture Substances 0.000 claims description 17
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 15
- 238000010992 reflux Methods 0.000 claims description 15
- 238000001354 calcination Methods 0.000 claims description 10
- 229910052799 carbon Inorganic materials 0.000 claims description 10
- 239000008367 deionised water Substances 0.000 claims description 10
- 229910021641 deionized water Inorganic materials 0.000 claims description 10
- 238000003756 stirring Methods 0.000 claims description 10
- VDZOOKBUILJEDG-UHFFFAOYSA-M tetrabutylammonium hydroxide Chemical compound [OH-].CCCC[N+](CCCC)(CCCC)CCCC VDZOOKBUILJEDG-UHFFFAOYSA-M 0.000 claims description 10
- BMVXCPBXGZKUPN-UHFFFAOYSA-N 1-hexanamine Chemical compound CCCCCCN BMVXCPBXGZKUPN-UHFFFAOYSA-N 0.000 claims description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 5
- NWGKJDSIEKMTRX-AAZCQSIUSA-N Sorbitan monooleate Chemical compound CCCCCCCC\C=C/CCCCCCCC(=O)OC[C@@H](O)[C@H]1OC[C@H](O)[C@H]1O NWGKJDSIEKMTRX-AAZCQSIUSA-N 0.000 claims description 5
- 229910021552 Vanadium(IV) chloride Inorganic materials 0.000 claims description 5
- 239000002253 acid Substances 0.000 claims description 5
- JHXKRIRFYBPWGE-UHFFFAOYSA-K bismuth chloride Chemical compound Cl[Bi](Cl)Cl JHXKRIRFYBPWGE-UHFFFAOYSA-K 0.000 claims description 5
- 239000003795 chemical substances by application Substances 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 5
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 5
- 239000003995 emulsifying agent Substances 0.000 claims description 5
- 230000004048 modification Effects 0.000 claims description 5
- 238000012986 modification Methods 0.000 claims description 5
- 239000000843 powder Substances 0.000 claims description 5
- 235000019832 sodium triphosphate Nutrition 0.000 claims description 5
- 229910001220 stainless steel Inorganic materials 0.000 claims description 5
- 239000010935 stainless steel Substances 0.000 claims description 5
- JTJFQBNJBPPZRI-UHFFFAOYSA-J vanadium tetrachloride Chemical compound Cl[V](Cl)(Cl)Cl JTJFQBNJBPPZRI-UHFFFAOYSA-J 0.000 claims description 5
- 230000003647 oxidation Effects 0.000 claims 1
- 238000007254 oxidation reaction Methods 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 5
- 239000005416 organic matter Substances 0.000 abstract description 5
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 abstract description 4
- 239000001569 carbon dioxide Substances 0.000 abstract description 2
- 229910002092 carbon dioxide Inorganic materials 0.000 abstract description 2
- 238000004140 cleaning Methods 0.000 abstract description 2
- 238000005286 illumination Methods 0.000 abstract description 2
- VUZPPFZMUPKLLV-UHFFFAOYSA-N methane;hydrate Chemical compound C.O VUZPPFZMUPKLLV-UHFFFAOYSA-N 0.000 abstract description 2
- 239000002994 raw material Substances 0.000 abstract description 2
- 229920006395 saturated elastomer Polymers 0.000 abstract description 2
- 238000001179 sorption measurement Methods 0.000 abstract description 2
- 238000001035 drying Methods 0.000 abstract 1
- 238000001914 filtration Methods 0.000 abstract 1
- VOSWFBNIBDYAOM-UHFFFAOYSA-N [V].[Bi]=O Chemical compound [V].[Bi]=O VOSWFBNIBDYAOM-UHFFFAOYSA-N 0.000 description 7
- 239000011148 porous material Substances 0.000 description 4
- 238000010521 absorption reaction Methods 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 239000004615 ingredient Substances 0.000 description 2
- 229910000323 aluminium silicate Inorganic materials 0.000 description 1
- 208000002925 dental caries Diseases 0.000 description 1
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000002957 persistent organic pollutant Substances 0.000 description 1
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000008929 regeneration Effects 0.000 description 1
- 238000011069 regeneration method Methods 0.000 description 1
- 238000012163 sequencing technique Methods 0.000 description 1
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Abstract
一种制备钒铋氧化物分子筛的方法,属于环境净化材料领域,工艺方法:将原料混合制备出钒溶液和铋溶液,再将钒溶液和铋溶液混合,水热反应后,经过滤、清洗、干燥,将得到固体A与盐酸溶液混合,再次过滤、清洗、干燥,将得到的固体B煅烧,研磨,即制得钒铋氧化物分子筛;本发明的产物具有极强的饱和吸附容量,并与有机物具有相当强的亲和性,在光照条件下,可以分解吸附在表面的有机物分子,并可将其完全氧化成二氧化碳和水,达到完全净化的目的。
Description
技术领域
本发明属于环境净化材料领域,具体涉及一种制备钒铋氧化物分子筛的方法。
背景技术
分子筛具有均匀的孔隙结构,孔隙的大小从微米到纳米尺寸,可以容纳相应大小的有机物分子。由于分子筛由骨架结构组成,其中存在丰富的孔道和空腔,从而具有很大的比表面积。常见的分子筛通常由结晶型的硅铝酸盐组成,由其形成分子筛的空腔结构。新型分子筛可由其它不同元素和晶体所组成,由于制备方法和组成不同,分子筛具有不同的孔道特征和尺寸,可以应用于各种使用条件。应用于环境净化的分子筛包括各种天然和人工分子筛,利用分子筛孔道对有机物分子的吸附和容纳作用来净化受污染的大气和水。由于分子筛吸附有机物的容量有限,在吸附达到饱和后就不再能够继续吸附有机物,同时对其再生处理需要特定的设备和条件。解决这一问题的关键是使分子筛具有自清洁能力,即自发地分解所吸附的有机物,从而能够释放出分子筛的表面和孔隙。为了达到这一目的,需要对分子筛的组成和结构进行创新性的改进。
发明内容
针对现有技术存在的问题,本发明旨在提供一种制备钒铋氧化物分子筛的方法。此种材料以钒铋氧化物组成分子筛骨架,并在材料内部形成规则的三维孔道和空腔,可用于环境中有机污染物的吸附与光催化降解。
本发明采用的技术方案是:
一种制备钒铋氧化物分子筛的方法,包括下述工艺步骤:
步骤1:制备钒溶液
(1)在烧瓶中加入500mL无水乙醇、6~10mL正己胺、10~15mL四氯化钒、3~5g导向剂P123、5~7mL四丁基氢氧化铵25%甲醇溶液,将混合物加热至65℃,在此温度回流60min;
(2)在烧瓶中再加入3~7g乳化剂Span-80,继续在65℃回流30min,制得钒溶液;
步骤2:制备铋溶液
(1)在200mL的0.5mol/L盐酸溶液中加入12~16g氯化铋,搅拌使之完全溶解,得到溶液A;
(2)在溶液A中添加7~10g三聚磷酸钠,搅拌使之完全溶解,得到铋溶液;
步骤3:水热反应
(1)将钒溶液和铋溶液混合后置于不锈钢水热反应釜中,将混合液加热至180~220℃,反应50~60h;
(2)将所得产物过滤,用去离子水清洗,在210℃干燥15h,得到固体A;
步骤4:酸修饰
(1)将固体A与500mL的0.2mol/L盐酸溶液混合,并加热至80℃,在此温度回流3h,得到混合物;
(2)将混合物过滤,用去离子水清洗,在210℃干燥15h,得到固体B;
步骤5:煅烧定孔
将固体B在720~910℃煅烧3~6h,冷却,研磨成粒径小于6μm的粉末,即制得钒铋氧化物分子筛。
上述步骤1和步骤2无先后顺序。
本发明制备的钒铋氧化物分子筛具有如下技术特征:孔隙尺寸15~26nm,比表面积550~760m2/g,孔隙率大于65%。
本发明的一种制备钒铋氧化物分子筛的方法,与现有技术相比,优点在于:
以钒铋氧化物组成分子筛骨架,骨架中的主要结构成分为钒氧铋三元氧化物键合体,在分子筛内部形成规则的三维孔道和空腔。钒铋氧化物分子筛的孔道大小与常见中小有机物分子的尺寸相当,可以用于吸附空气和水中绝大多数的可扩散或可溶有机物,具有极强的饱和吸附容量,并与有机物具有相当强的亲和性。在光照条件下,该钒铋氧化物分子筛可以分解吸附在表面的有机物分子,并可将其完全氧化成二氧化碳和水,达到完全净化的目的。
具体实施方式
下述实施例中所用原料均为纯料。
实施例1
一种制备钒铋氧化物分子筛的方法,包括下述工艺步骤:
步骤1:制备钒溶液
(1)在烧瓶中加入500mL无水乙醇、6mL正己胺、10mL四氯化钒、3g导向剂P123、5mL四丁基氢氧化铵25%甲醇溶液,将混合物加热至65℃,在此温度回流60min;
(2)在烧瓶中再加入3g乳化剂Span-80,继续在65℃回流30min,制得钒溶液;
步骤2:制备铋溶液
(1)在200mL的0.5mol/L盐酸溶液中加入12g氯化铋,搅拌使之完全溶解,得到溶液A;
(2)在溶液A中添加7g三聚磷酸钠,搅拌使之完全溶解,得到铋溶液;
步骤3:水热反应
(1)将钒溶液和铋溶液混合后置于不锈钢水热反应釜中,将混合液加热至180℃,反应60h;
(2)将所得产物过滤,用去离子水清洗,在210℃干燥15h,得到固体A;
步骤4:酸修饰
(1)将固体A与500mL的0.2mol/L盐酸溶液混合,并加热至80℃,在此温度回流3h,得到混合物;
(2)将上述混合物过滤,用去离子水清洗,在210℃干燥15h,得到固体B;
步骤5:煅烧定孔
将固体B在720℃煅烧6h,冷却,研磨成粒径小于6μm的粉末,即制得钒铋氧化物分子筛。
本实施例制得钒铋氧化物分子筛的孔隙尺寸为15nm,比表面积550m2/g,孔隙率67%。
实施例2
一种制备钒铋氧化物分子筛的方法,包括下述工艺步骤:
步骤1:制备钒溶液
(1)在烧瓶中加入500mL无水乙醇、8mL正己胺、12mL四氯化钒、4g导向剂P123、6mL四丁基氢氧化铵25%甲醇溶液,将混合物加热至65℃,在此温度回流60min;
(2)在烧瓶中再加入5g乳化剂Span-80,继续在65℃回流30min,制得钒溶液;
步骤2:制备铋溶液
(1)在200mL的0.5mol/L盐酸溶液中加入14g氯化铋,搅拌使之完全溶解,得到溶液A;
(2)在溶液A中添加8g三聚磷酸钠,搅拌使之完全溶解,得到铋溶液;
步骤3:水热反应
(1)将钒溶液和铋溶液混合后置于不锈钢水热反应釜中,将混合液加热至200℃,反应55h;
(2)将所得产物过滤,用去离子水清洗,在210℃干燥15h,得到固体A;
步骤4:酸修饰
(1)将固体A与500mL的0.2mol/L盐酸溶液混合,并加热至80℃,在此温度回流3h,得到混合物;
(2)将上述混合物过滤,用去离子水清洗,在210℃干燥15h,得到固体B;
步骤5:煅烧定孔
将固体B在800℃煅烧4h,冷却,研磨成粒径小于6μm的粉末,即制得钒铋氧化物分子筛。
本实施例制得钒铋氧化物分子筛的孔隙尺寸为20nm,比表面积630m2/g,孔隙率70%。
实施例3
一种制备钒铋氧化物分子筛的方法,包括下述工艺步骤:
步骤1:制备钒溶液
(1)在烧瓶中加入500mL无水乙醇、10mL正己胺、15mL四氯化钒、3~5g导向剂P123、7mL四丁基氢氧化铵25%甲醇溶液,将混合物加热至65℃,在此温度回流60min;
(2)在烧瓶中再加入7g乳化剂Span-80,继续在65℃回流30min,制得钒溶液;
步骤2:制备铋溶液
(1)在200mL的0.5mol/L盐酸溶液中加入16g氯化铋,搅拌使之完全溶解,得到溶液A;
(2)在溶液A中添加10g三聚磷酸钠,搅拌使之完全溶解,得到铋溶液;
步骤3:水热反应
(1)将钒溶液和铋溶液混合后置于不锈钢水热反应釜中,将混合液加热至220℃,反应50h;
(2)将所得产物过滤,用去离子水清洗,在210℃干燥15h,得到固体A;
步骤4:酸修饰
(1)将固体A与500mL的0.2mol/L盐酸溶液混合,并加热至80℃,在此温度回流3h,得到混合物;
(2)将上述混合物过滤,用去离子水清洗,在210℃干燥15h,得到固体B;
步骤5:煅烧定孔
将固体B在910℃煅烧3h,冷却,研磨成粒径小于6μm的粉末,即制得钒铋氧化物分子筛。
本实施例制得钒铋氧化物分子筛的孔隙尺寸为26nm,比表面积760m2/g,孔隙率75%。
Claims (2)
1.一种制备钒铋氧化物分子筛的方法,其特征在于,包括下述工艺步骤:
步骤1:制备钒溶液
(1)在烧瓶中加入500mL无水乙醇、6~10mL正己胺、10~15mL四氯化钒、3~5g导向剂P123、5~7mL四丁基氢氧化铵25%甲醇溶液,将混合物加热至65℃,在此温度回流60min;
(2)在烧瓶中再加入3~7g乳化剂Span-80,继续在65℃回流30min,制得钒溶液;
步骤2:制备铋溶液
(1)在200mL的0.5mol/L盐酸溶液中加入12~16g氯化铋,搅拌使之完全溶解,得到溶液A;
(2)在溶液A中添加7~10g三聚磷酸钠,搅拌使之完全溶解,得到铋溶液;
步骤3:水热反应
(1)将钒溶液和铋溶液混合后置于不锈钢水热反应釜中,将混合液加热至180~220℃,反应50~60h;
(2)将所得产物过滤,用去离子水清洗,在210℃干燥15h,得到固体A;
步骤4:酸修饰
(1)将固体A与500mL的0.2mol/L盐酸溶液混合,并加热至80℃,在此温度回流3h,得到混合物;
(2)将混合物过滤,用去离子水清洗,在210℃干燥15h,得到固体B;
步骤5:煅烧定孔
将固体B在720~910℃煅烧3~6h,冷却,研磨成粒径小于6μm的粉末,即制得钒铋氧化物分子筛。
2.根据权利要求1所述的一种制备钒铋氧化物分子筛的方法,其特征在于,通过所述方法制得的钒铋氧化物分子筛具有如下技术特征:孔隙尺寸15~26nm,比表面积550~760m2/g,孔隙率大于65%。
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