CN114411176B - 一种光电催化制备h2o2装置及其应用 - Google Patents
一种光电催化制备h2o2装置及其应用 Download PDFInfo
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- YECIFGHRMFEPJK-UHFFFAOYSA-N lidocaine hydrochloride monohydrate Chemical compound O.[Cl-].CC[NH+](CC)CC(=O)NC1=C(C)C=CC=C1C YECIFGHRMFEPJK-UHFFFAOYSA-N 0.000 title claims description 4
- 239000012528 membrane Substances 0.000 claims abstract description 91
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- OEYIOHPDSNJKLS-UHFFFAOYSA-N choline Chemical compound C[N+](C)(C)CCO OEYIOHPDSNJKLS-UHFFFAOYSA-N 0.000 claims description 21
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Abstract
本发明属于H2O2制备领域,具体涉及一种光电催化制备H2O2装置及其应用。为解决催化剂表面氧气浓度较小、生成的H2O2不稳定的问题,本发明是一种含有光电催化复合膜的装置,能够进行光电催化制备H2O2,并利用生成的H2O2进行烯烃环氧化反应的装置。多孔疏水性膜有利于氧气的转移和富集,确保光电催化剂表面具有充足的氧气;双极膜中间界面层水解离产生的H+确保H2O2合成反应过程中具有足够的H+供应;光电催化剂表面产生的电子确保足够的电子,与催化剂表面富集的氧气、双极膜中间界面层水解离产生的H+结合,生成H2O2,并利用生成的H2O2进行烯烃环氧化反应。
Description
技术领域
本发明属于H2O2制备领域,具体涉及一种光电催化制备H2O2装置及其应用。
背景技术
H2O2作为一种有效的氧化还原试剂,被广泛应用于水净化、抗菌、漂白、清洗剂、有机化合物合成和燃料电池等领域。目前大规模生产H2O2的方法主要有电化学合成、醇氧化、蒽醌自氧化等多种,但这些方法并非是理想的方法,因为需要消耗大量的能源和有机溶剂。半导体光催化技术制备H2O2近年来受到广泛关注,该过程以水和氧气为原料,能量来自太阳光,是一种绿色的制备H2O2技术。
然而,在光催化制备H2O2过程中,通常遇到以下问题:(1)氧气在水中的溶解度较小,导致催化剂表面氧气浓度较小;(2)通常需要额外添加醇类或者酸等提供质子;(3)生成的H2O2不稳定,在光照下发生分解。针对以上问题,传统解决方法通常主要是集中在对现有催化剂进行改性、调控,或者寻求新型催化剂。
发明内容
针对在光催化制备H2O2过程中,存在(1)氧气在水中的溶解度较小,导致催化剂表面氧气浓度较小;(2)通常需要额外添加醇类或者酸等提供质子;(3)生成的H2O2不稳定,在光照下发生分解的问题,本发明提出一种光电催化制备H2O2装置及其在烯烃环氧化反应中的应用。
为了达到上述目的,本发明采用了下列技术方案:
一种光电催化制备H2O2装置,包括反应器、光电催化复合膜、阴极、阳极、直流电源、光源、导气管;所述光电催化复合膜设置在反应器内,将反应器分为阳极室和阴极室,所述阳极和阴极分别设置在阳极室和阴极室内,所述直流电源的正极和负极分别与阳极和阴极连接,所述光源设置在阴极室的上方,所述导气管位于阴极室内将氧气通入阴极室;
所述光电催化复合膜由双极膜和表面负载光电催化剂的多孔疏水膜构成,双极膜是由阴离子交换膜和阳离子交换膜复合而成;所述阳极室为电解质水溶液,阴极室为含酶的低共熔溶剂水溶液,所述光源为氙灯。
进一步,所述光电催化复合膜的制备方法如下:
(1)采用聚乙烯醇、聚乙烯吡咯烷酮、聚砜、聚乙烯苄基氯中的一种或几种任意比例的混合物作为阴离子交换膜的支撑,采用一种或几种按任意比混合的含有伯氨基、仲氨基、叔氨基或季氨基的化合物作为阴离子交换膜的固定基团,加入戊二醛溶液作为交联剂,配制阴离子交换膜液,通过流延法制备阴离子交换膜;
(2)采用聚乙烯醇、聚乙烯吡咯烷酮、聚苯醚、聚砜和苯乙烯中的一种或几种任意比例的混合物作为阳离子交换膜的支撑,采用一种或几种按任意比混合的含有磺酸基、羧酸基或磷酸基的化合物作为阳离子交换膜的固定基团,加入FeCl3或CaCl2溶液作为交联剂,配制阳离子交换膜液,流延于步骤(1)制备的阴离子交换膜表面,得到阳离子交换膜;
(3)将表面负载光电催化剂的多孔疏水性材料超声分散于去离子水或无水乙醇中,流延于阳离子交换膜表面,得到表面负载光电催化剂的多孔疏水膜。
进一步,所述光电催化剂为C3N4、TiO2、MoS2、CdS、Cu2O、Fe2O3和BiOCl中的一种,所述多孔疏水性材料为碳纤维、碳纳米管、疏水介孔SiO2、疏水分子筛、疏水金属有机框架材料中对的一种。
进一步,所述电解质水溶液为Na2SO4、NaOH或KOH,浓度为0.01~3.0mol L-1;所述低共熔溶剂包括:氯化胆碱-尿素、氯化胆碱-乙酰胺、氯化胆碱-乙二醇、氯化胆碱-丙三醇、氯化胆碱-木糖醇、氯化胆碱-山梨醇、氯化胆碱-木糖-水、氯化胆碱-葡萄糖-水、氯化胆碱-蔗糖-水、甜菜碱-苹果酸、甜菜碱-柠檬酸、甜菜碱-甘油、甜菜碱-木糖醇、甜菜碱-尿素;所述酶为脂肪酶。
进一步,所述直流电源的电压为0.4~1.5V。
一种光电催化制备H2O2装置的应用,应用在烯烃环氧化反应中。
进一步,应用在烯烃环氧化反应中的具体方法为:在阴极室加入辛酸和不饱和烯烃,利用光电催化生成的H2O2,在酶催化作用下进行烯烃环氧化反应。
更近一步,所述不饱和烯烃包括:环辛烯、1-己烯、环己烯、1-癸烯、1-十八烯、苯乙烯、α-甲基苯乙烯。
与现有技术相比本发明具有以下优点:
(1)本发明的多孔疏水性膜有利于氧气的转移和富集,确保光电催化剂表面具有充足的氧气。
(2)本发明在直流电场作用下,双极膜中间界面层发生水解离,产生的H+透过阳离子交换膜表面,迁移至光电催化剂表面参与反应,确保H2O2合成反应过程中具有足够的H+供应;同时,通过控制双极膜中间界面层的水解离速率,使H+供应量与合成H2O2反应所需相匹配,避免出现由于H+供应量不足而导致H2O2合成受阻,或者由于H+过剩而导致溶液pH变小,从而影响酶的活性和稳定性。
(3)本发明在光电作用下,光电催化剂表面产生的电子与催化剂表面富集的氧气、双极膜中间界面层水解离产生的H+结合,生成H2O2。
(4)本发明在阴极室加入辛酸和不饱和烯烃,利用生成的H2O2进行烯烃环氧化反应,H2O2边生成边消耗,不仅可以有效避免H2O2浓度过大而导致酶的活性和稳定性下降,同时由于H2O2及时消耗而避免其发生分解。
(5)本发明利用膜液具有粘性的特征,将光电催化剂流延于阳离子膜表面,不仅有效避免了传统方法将催化剂粉末直接加入到油水双相体系而发生团聚现象,而且便于光电催化剂的循环再利用。
附图说明
图1是本发明光电催化制备H2O2装置的示意图;
图2是将双极膜在液氮中脆断后的截面SEM图;
图3是实施例1制备阳离子交换膜采用FeCl3溶液交联示意图;
图4是实施例1制备的MoS2光催化剂的形貌图。
具体实施方式
实施例1
如图1所示,一种光电催化制备H2O2装置,反应器、光电催化复合膜、阴极、阳极、直流电源、光源、导气管;所述光电催化复合膜设置在反应器内,将反应器分为阳极室和阴极室,所述阳极和阴极分别设置在阳极室和阴极室内,所述直流电源的正极和负极分别与阳极和阴极连接,所述光源设置在阴极室的上方,所述导气管位于阴极室内将氧气通入阴极室;
所述光电催化复合膜由双极膜和表面负载光电催化剂的多孔疏水膜构成,双极膜是由阴离子交换膜和阳离子交换膜复合而成;所述阳极室为电解质水溶液,阴极室为含酶的低共熔溶剂水溶液,所述光源为氙灯。
所述光电催化复合膜的制备方法如下:
(1)将质量相等的聚乙烯醇和壳聚糖混合后倒入烧杯,加入质量分数为0.01%的醋酸水溶液,在60℃恒温水浴锅中不断搅拌,完全溶解后加入戊二醛,继续搅拌1h,静置脱泡后,流延于平整干洁的带边框玻璃板上,放入鼓风干燥箱中烘干,得到阴离子交换膜;
(2)将质量相等的聚乙烯醇和羧甲基纤维素钠混合后倒入烧杯,搅拌下加入去离子水,加热到60℃溶解,待完全溶解后加入FeCl3溶液,继续搅拌1h,静置脱泡后,流延于上述制备的阴离子交换膜表面,得到阳离子交换膜;
(3)将光电催化剂C3N4负载于疏水性碳纤维表面,然后超声分散于水溶液或者无水乙醇中,流延于阳离子交换膜表面,得到负载光电催化剂的疏水性膜。
以光电催化复合膜作为阳极室和阴极室的隔膜,阳极室加浓度为0.01mol L-1的Na2SO4电解质水溶液,阴极室加含有脂肪酶的氯化胆碱-山梨醇低共熔溶剂水溶液,并加入辛酸和1-己烯,通过鼓泡的方式通入O2气体,在氙灯光源照射下,直流电源电压为1.0V下,进行光电催化制备H2O2,然后利用生成的H2O2进行烯烃环氧化反应。反应36小时后,采用气相色谱分析产物,得到环辛烯的转化率为6.12%。
图2是将双极膜在液氮中脆断后的截面SEM图,从图中可以清晰看到构成双极膜的阴离子交换膜和阳离子交换膜,以及两膜层之间的中间界面层。双极膜中间界面层的厚度通常只有纳米级厚度,因此,即使在双极膜两侧施加很小的电压,双极膜中间界面层也可以形成强大的电场,在强大的电场作用,双极膜中间界面层的水分子即可发生水解离。
图3是采用FeCl3溶液交联阳离子交换膜的示意图,从图中可以看出,通过FeCl3溶液交联后,阳离子交换膜形成网状结构,有利于提高膜的机械性能,从而可提高膜的使用寿命。
图4是制备的MoS2光催化剂的形貌图,从图中可以看出,MoS2光催化剂呈现单层或少层的片层结构,有利于提高光生载流子的分离效率,从而提高光电催化效率。
实施例2
与实施例1的不同之处在于,光电催化复合膜的制备方法,具体步骤如下:
(1)将质量比为2:1的聚乙烯吡咯烷酮和季铵聚砜混合后倒入烧杯,加入质量分数为0.02%的醋酸水溶液,在50℃恒温水浴锅中不断搅拌,完全溶解后加入戊二醛,继续搅拌1h,静置脱泡后,流延于平整干洁的带边框玻璃板上,放入鼓风干燥箱中烘干,得到阴离子交换膜;
(2)将质量相等的聚乙烯吡咯烷酮和磷酸纤维素混合后倒入烧杯,搅拌下加入去离子水,加热到60℃溶解,待完全溶解后加入CaCl2溶液,继续搅拌1h,静置脱泡后,流延于上述制备的阴离子交换膜表面,得到阳离子交换膜;
(3)将光电催化剂TiO2负载于疏水性碳纳米管表面,然后超声分散于水溶液或者无水乙醇中,流延于阳离子交换膜表面,得到负载光电催化剂的疏水性膜。
以光电催化复合膜作为阳极室和阴极室的隔膜,阳极室加浓度为3.0mol L-1的K2SO4电解质水溶液,阴极室加含有脂肪酶的氯化胆碱-尿素低共熔溶剂水溶液,并加入辛酸和环已烯,通过鼓泡的方式通入O2气体,在氙灯光源照射下,直流电源电压为1.5V下,进行光电催化制备H2O2,然后利用生成的H2O2进行烯烃环氧化反应。反应30小时后,采用气相色谱分析产物,得到环己烯的转化率为3.52%。
实施例3
与实施例1的不同之处在于,光电催化复合膜的制备方法,具体步骤如下:
(1)将质量比为3:1的聚乙烯苄基氯和聚酰亚胺混合后倒入烧杯,加入质量分数为0.03%的醋酸水溶液,在60℃恒温水浴锅中不断搅拌,完全溶解后加入戊二醛,继续搅拌1.5h,静置脱泡后,流延于平整干洁的带边框玻璃板上,放入鼓风干燥箱中烘干,得到阴离子交换膜;
(2)将质量相等的聚苯醚和磺酸基纤维混合后倒入烧杯,搅拌下加入去离子水,加热到70℃溶解,待完全溶解后加入CaCl2溶液,继续搅拌1h,静置脱泡后,流延于上述制备的阴离子交换膜表面,得到阳离子交换膜;
(3)将光电催化剂MoS2负载于疏水分子筛表面,然后超声分散于水溶液或者无水乙醇中,流延于阳离子交换膜表面,得到负载光电催化剂的疏水性膜。
以光电催化复合膜作为阳极室和阴极室的隔膜,阳极室加浓度为0.01mol L-1的K2SO4电解质水溶液,阴极室加含有脂肪酶的氯化胆碱-乙二醇的低共熔溶剂水溶液,并加入辛酸和1-十八烯,通过鼓泡的方式通入O2气体,在氙灯光源照射下,直流电源电压为0.8V下,进行光电催化制备H2O2,然后利用生成的H2O2进行烯烃环氧化反应。反应42小时后,采用气相色谱分析产物,得到1-十八烯的转化率为1.76%。
实施例4
与实施例1的不同之处在于,光电催化复合膜的制备方法,具体步骤如下:
(1)将质量比为0.5:1的聚砜和甘油基三甲基氯化铵混合后倒入烧杯,加入质量分数为0.005%的醋酸水溶液,在70℃恒温水浴锅中不断搅拌,完全溶解后加入戊二醛,继续搅拌2.5h,静置脱泡后,流延于平整干洁的带边框玻璃板上,放入鼓风干燥箱中烘干,得到阴离子交换膜;
(2)将质量相等的聚乙烯吡咯烷酮和醋酸纤维素混合后倒入烧杯,搅拌下加入质量分数为0.05%的磷酸水溶液,加热到70℃溶解,待完全溶解后加入FeCl3溶液,继续搅拌1h,静置脱泡后,流延于上述制备的阴离子交换膜表面,得到阳离子交换膜;
(3)将光电催化剂BiOCl负载于疏水介孔SiO2表面,然后超声分散于水溶液或者无水乙醇中,流延于阳离子交换膜表面,得到负载光电催化剂的疏水性膜。
以光电催化复合膜作为阳极室和阴极室的隔膜,阳极室加浓度为0.01mol L-1的NaOH电解质水溶液,阴极室加含有脂肪酶的甜菜碱-苹果酸的低共熔溶剂水溶液,并加入辛酸和苯乙烯,通过鼓泡的方式通入O2气体,在氙灯光源照射下,直流电源电压为0.4V下,进行光电催化制备H2O2,然后利用生成的H2O2进行烯烃环氧化反应。反应48小时后,采用气相色谱分析产物,得到苯乙烯的转化率为2.23%。
Claims (6)
1.一种光电催化制备H2O2装置,其特征在于,所述装置包括反应器、光电催化复合膜、阴极、阳极、直流电源、光源、导气管;所述光电催化复合膜设置在反应器内,将反应器分为阳极室和阴极室,所述阳极和阴极分别设置在阳极室和阴极室内,所述直流电源的正极和负极分别与阳极和阴极连接,所述光源设置在阴极室的上方,所述导气管位于阴极室内将氧气通入阴极室;
所述光电催化复合膜由双极膜和表面负载光电催化剂的多孔疏水膜构成,双极膜是由阴离子交换膜和阳离子交换膜复合而成;所述阳极室为电解质水溶液,阴极室为含酶的低共熔溶剂水溶液,所述光源为氙灯;
所述表面负载光电催化剂的多孔疏水膜的制备方法为:将表面负载光电催化剂的多孔疏水性材料超声分散于去离子水或无水乙醇中,流延于阳离子交换膜表面,得到表面负载光电催化剂的多孔疏水膜;
所述光电催化剂为C3N4、TiO2、MoS2、CdS、Cu2O、Fe2O3和BiOCl中的一种,所述多孔疏水性材料为碳纤维、碳纳米管、疏水介孔SiO2、疏水分子筛、疏水金属有机框架材料中对的一种;所述电解质水溶液为Na2SO4、NaOH或KOH,浓度为0.01~3.0 mol L-1;所述低共熔溶剂包括:氯化胆碱-尿素、氯化胆碱-乙酰胺、氯化胆碱-乙二醇、氯化胆碱-丙三醇、氯化胆碱-木糖醇、氯化胆碱-山梨醇、氯化胆碱-木糖-水、氯化胆碱-葡萄糖-水、氯化胆碱-蔗糖-水、甜菜碱-苹果酸、甜菜碱-柠檬酸、甜菜碱-甘油、甜菜碱-木糖醇、甜菜碱-尿素;所述酶为脂肪酶。
2.根据权利要求1所述的一种光电催化制备H2O2装置,其特征在于,所述光电催化复合膜的制备方法如下:
(1)采用聚乙烯醇、聚乙烯吡咯烷酮、聚砜、聚乙烯苄基氯中的一种或几种任意比例的混合物作为阴离子交换膜的支撑,采用一种或几种按任意比混合的含有伯氨基、仲氨基、叔氨基或季氨基的化合物作为阴离子交换膜的固定基团,加入戊二醛溶液作为交联剂,配制阴离子交换膜液,通过流延法制备阴离子交换膜;
(2)采用聚乙烯醇、聚乙烯吡咯烷酮、聚苯醚、聚砜和苯乙烯中的一种或几种任意比例的混合物作为阳离子交换膜的支撑,采用一种或几种按任意比混合的含有磺酸基、羧酸基或磷酸基的化合物作为阳离子交换膜的固定基团,加入FeCl3或CaCl2溶液作为交联剂,配制阳离子交换膜液,流延于步骤(1)制备的阴离子交换膜表面,得到阳离子交换膜;
(3)将表面负载光电催化剂的多孔疏水性材料超声分散于去离子水或无水乙醇中,流延于阳离子交换膜表面,得到表面负载光电催化剂的多孔疏水膜。
3.根据权利要求1所述的一种光电催化制备H2O2装置,其特征在于,所述直流电源的电压为0.4~1.5V。
4.一种权利要求1所述的光电催化制备H2O2装置的应用,其特征在于,应用在烯烃环氧化反应中。
5.根据权利要求4所述的一种光电催化制备H2O2装置的应用,其特征在于,应用在烯烃环氧化反应中的具体方法为:在阴极室加入辛酸和不饱和烯烃,利用光电催化生成的H2O2,在酶催化作用下进行烯烃环氧化反应。
6.根据权利要求5所述的一种光电催化制备H2O2装置的应用,其特征在于,所述不饱和烯烃包括环辛烯、1-己烯、环己烯、1-癸烯、1-十八烯、苯乙烯、α-甲基苯乙烯。
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