Photocatalyst-loaded Co-based MOFs-porous carbon composite adsorption material and preparation method thereof

A composite adsorption material and photocatalyst technology, which is applied in the field of photocatalyst loaded Co-based MOFs-porous carbon composite adsorption materials, can solve the problems of secondary pollution of small molecule water bodies, poor adsorption effect of heavy metals and their ions, and low degradation efficiency. Achieve excellent and good photochemical activity, good electrical conductivity and electron transport performance, increase the effect of diffusion and transmission rate

Inactive Publication Date: 2020-05-08
黄春美
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Problems solved by technology

[0006] Aiming at the deficiencies of the prior art, the present invention provides a photocatalyst-supported Co-based MOFs-porous carbon composite adsorption material and its preparation method, which solves the problem that the degradation efficiency of organic pollutants by photocatalysts is not high, and at the same time, small molecules are produced by degradation It is easy to cause secondary pollution to the water body, and at the same time solves the problem that the current photocatalytic materials have poor adsorption effect on heavy metals and their ions

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preparation example Construction

[0028] 巯基修饰Co基MOFs制备方法包括以下步骤:

[0029] (1)向反应瓶加入适量的 N , N -二甲基甲酰胺溶剂,再依次加入CoCl 2 和有机MOF配体2,4,6-三(4-羧基苯基)-1,3,5-三嗪,两者物质的量摩尔比1.5-1.8:1,将反应瓶置于超声处理仪中进行加热至60-70 ℃,超声频率为20-22 Kz,进行超声分散处理1-2 h,将溶液转移进自动水热反应釜中,加热至120-130 ℃,匀速搅拌反应35-40 h,反应结束将溶液冷却至室温,过滤除去溶液,依次使用适量的蒸馏水和无水乙醇洗涤固体,并置于烘箱中加热至120-130 ℃,充分干燥12-15 h得到Co基MOFs。

[0030] (2)向反应瓶中加入适量的甲苯溶剂,再加入乙二硫醇和Co基MOFs,两者质量比为25-30:1,将反应瓶置于油浴锅中,加热至115-125 ℃,匀速搅拌回流反应30-35 h,将溶液通过高速离心机中,进行离心分离除去溶剂,并使用适量的无水乙醇洗涤固体产物,并置于烘箱中加热至70-80 ℃,充分干燥制备得到巯基修饰Co基MOFs。

[0031] 光催化剂负载Co基MOFs-多孔碳复合吸附材料制备方法包括以下步骤:

[0032] (1)向反应瓶中加入适量的蒸馏水和乙二醇溶剂,两者体积比为1.5-2:1,再依次加入14-30份巯基修饰Co基MOFs、16-21份TiO 2 、6-8份Ta 2 o 5 和4-5份Na 2 CO 3 ,三者质量比为4-4.2:1.5-1.6:1,搅拌均匀后,将反应瓶置于将反应瓶置于超声处理仪中进行加热至80-90 ℃,超声频率为20-22 Kz,进行超声分散处理2-3 h,将溶液置于坩埚中蒸发浓缩,冷却结晶。

[0033] (2)将固体产物研磨直至物料全部通过200-300目网筛,置于煅烧电阻炉中,升温速率为10-15 ℃ / min,在1200-1250 ℃下煅烧18-20 h,将煅烧产物置于质量分数为10-12%的稀盐酸溶液中,匀速搅拌96-120 h,进行酸化反应,过滤除去溶剂,使用适量的蒸馏水洗涤固体产物,并置于烘箱中加热至80-90 ℃充分干燥,制备得到层状HTiTaO 5 负载Co-MOFs基光催化材料。

[0034] (3)向反应瓶中加入质量分数为5-10...

Embodiment 1

[0036] (1)制备Co基MOFs组分1:向反应瓶加入适量的 N , N -二甲基甲酰胺溶剂,再依次加入CoCl 2 和有机MOF配体2,4,6-三(4-羧基苯基)-1,3,5-三嗪,两者物质的量摩尔比1.5:1,将反应瓶置于超声处理仪中进行加热至60 ℃,超声频率为20 Kz,进行超声分散处理1 h,将溶液转移进自动水热反应釜中,加热至120 ℃,匀速搅拌反应35 h,反应结束将溶液冷却至室温,过滤除去溶液,依次使用适量的蒸馏水和无水乙醇洗涤固体,并置于烘箱中加热至120 ℃,充分干燥12 h得到Co基MOFs组分1。

[0037] (2)制备巯基修饰Co基MOFs组分1:向反应瓶中加入适量的甲苯溶剂,再加入乙二硫醇和Co基MOFs组分1,两者质量比为25:1,将反应瓶置于油浴锅中,加热至115 ℃,匀速搅拌回流反应30 h,将溶液通过高速离心机中,进行离心分离除去溶剂,并使用适量的无水乙醇洗涤固体产物,并置于烘箱中加热至70 ℃,充分干燥制备得到巯基修饰Co基MOFs组分1。

[0038] (3)制备层状HTiTaO 5 负载Co-MOFs基光催化材料组分1:向反应瓶中加入适量的蒸馏水和乙二醇溶剂,两者体积比为1.5:1,再依次加入30份巯基修饰Co基MOFs组分1、16份TiO 2 、6份Ta 2 o 5 和4份Na 2 CO 3 ,搅拌均匀后,将反应瓶置于将反应瓶置于超声处理仪中进行加热至80 ℃,超声频率为20 Kz,进行超声分散处理2 h,将溶液置于坩埚中蒸发浓缩,冷却结晶,将固体产物研磨直至物料全部通过200目网筛,置于煅烧电阻炉中,升温速率为10 ℃ / min,在1200 ℃下煅烧18 h,将煅烧产物置于质量分数为10%的稀盐酸溶液中,匀速搅拌96h,进行酸化反应,过滤除去溶剂,使用适量的蒸馏水洗涤固体产物,并置于烘箱中加热至80℃充分干燥,制备得到层状HTiTaO 5 负载Co-MOFs基光催化材料组分1。

[0039] (4)制备光催化剂负载Co基MOFs-多孔碳复合吸附材料1:向反应瓶中加入质量分数为5 %的醋酸溶液和质量分数为20%的硫酸溶液,两者体积比为10:1,再依次加入4份壳聚糖、40份煤灰渣,将反应瓶置于超声处理仪中进行加热至70 ℃,超声频率为20 Kz,进行超声分散处理3 h,将反...

Embodiment 2

[0041] (1)制备Co基MOFs组分2:向反应瓶加入适量的 N , N -二甲基甲酰胺溶剂,再依次加入CoCl 2 和有机MOF配体2,4,6-三(4-羧基苯基)-1,3,5-三嗪,两者物质的量摩尔比1.8:1,将反应瓶置于超声处理仪中进行加热至60 ℃,超声频率为22 Kz,进行超声分散处理2 h,将溶液转移进自动水热反应釜中,加热至130 ℃,匀速搅拌反应35 h,反应结束将溶液冷却至室温,过滤除去溶液,依次使用适量的蒸馏水和无水乙醇洗涤固体,并置于烘箱中加热至120 ℃,充分干燥12 h得到Co基MOFs组分2。

[0042] (2)制备巯基修饰Co基MOFs组分2:向反应瓶中加入适量的甲苯溶剂,再加入乙二硫醇和Co基MOFs组分2,两者质量比为25:1,将反应瓶置于油浴锅中,加热至125 ℃,匀速搅拌回流反应30 h,将溶液通过高速离心机中,进行离心分离除去溶剂,并使用适量的无水乙醇洗涤固体产物,并置于烘箱中加热至70 ℃,充分干燥制备得到巯基修饰Co基MOFs组分2。

[0043] (3)制备层状HTiTaO 5 负载Co-MOFs基光催化材料组分2:向反应瓶中加入适量的蒸馏水和乙二醇溶剂,两者体积比为1.5:1,再依次加入25份巯基修饰Co基MOFs组分2、17.3份TiO 2 、6.5份Ta 2 o 5 和4.2份Na 2 CO 3 ,搅拌均匀后,将反应瓶置于将反应瓶置于超声处理仪中进行加热至90 ℃,超声频率为22 Kz,进行超声分散处理3 h,将溶液置于坩埚中蒸发浓缩,冷却结晶,将固体产物研磨直至物料全部通过200目网筛,置于煅烧电阻炉中,升温速率为10℃ / min,在1200 ℃下煅烧20 h,将煅烧产物置于质量分数为10%的稀盐酸溶液中,匀速搅拌96 h,进行酸化反应,过滤除去溶剂,使用适量的蒸馏水洗涤固体产物,并置于烘箱中加热至80 ℃充分干燥,制备得到层状HTiTaO 5 负载Co-MOFs基光催化材料组分2。

[0044] (4)制备光催化剂负载Co基MOFs-多孔碳复合吸附材料2:向反应瓶中加入质量分数为10 %的醋酸溶液和质量分数为20%的硫酸溶液,两者体积比为10:1,再依次加入4.5份壳聚糖、41.5份煤灰渣,将反应瓶置于超声处理仪中进行加热至70 ℃,超声频率为22 Kz,进行...

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Abstract

The invention relates to the technical field of photodegradable adsorption materials, and discloses a photocatalyst-loaded Co-based MOFs-porous carbon composite adsorption material and a preparation method thereof, and the photocatalyst-loaded Co-based MOFs-porous carbon composite adsorption material comprises the following formula raw materials: chitosan, coal ash, TiO2, Ta2O5, Na2CO3 and sulfydryl-modified Co-based MOFs. The invention discloses the photocatalyst loaded Co-based MOFs-porous carbon composite adsorption material and the preparation method thereof. Due to the HTiTaO5 lamellar structure, the transmission distance of charge carriers is shortened, the transmission rate of electrons is increased, the HTiTaO5 is uniformly loaded into the specific surface and the mesoporous structure of a sulfydryl modified Co-MOFs calcined product, the calcined product of the carbon skeleton has good conductivity, the diffusion and transmission rate of photon-generated carriers can be increased, the compounding of HTiTaO5 photo-induced electrons and photo-induced holes is effectively inhibited, hydrogen bonds and Van der Waals' force can be formed between chitosan hydroxyl and amino groups and organic pollutants, and the recycled waste coal ash has a rich pore structure and can be used for well physically adsorbing heavy metals such as copper, cadmium, arsenic, mercury and ions thereof in water.

Description

technical field [0001] The invention relates to the technical field of photodegradable adsorption materials, in particular to a photocatalyst-supported Co-based MOFs-porous carbon composite adsorption material and a preparation method thereof. Background technique [0002] In recent years, the problem of water resources and water pollution in my country has become increasingly serious. The pollution problem has caused adverse social impacts and major economic losses. At the same time, it has caused serious harm to people's health and sustainable development of society. Water pollution is caused by harmful Chemical substances reduce or lose the use value of water and pollute the environment. Pollutants mainly come from industrial wastewater discharged without treatment, domestic sewage discharged without treatment, and farmland sewage caused by extensive use of chemical fertilizers, pesticides, and herbicides etc., the increasing water pollution has posed a major threat to huma...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/22B01J20/30B01J23/20C02F1/30C02F1/28C02F101/30
CPCB01J20/20B01J20/22B01J23/20B01J35/004C02F1/283C02F1/30C02F2101/30
Inventor 黄春美
Owner 黄春美
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