CN104874409A - Preparation method of novel nano rod Bi2O(OH)2SO4 photocatalyst - Google Patents

Preparation method of novel nano rod Bi2O(OH)2SO4 photocatalyst Download PDF

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Publication number
CN104874409A
CN104874409A CN201510228538.2A CN201510228538A CN104874409A CN 104874409 A CN104874409 A CN 104874409A CN 201510228538 A CN201510228538 A CN 201510228538A CN 104874409 A CN104874409 A CN 104874409A
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hydrogen peroxide
preparation
bismuth nitrate
photochemical catalyst
water
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Chinese (zh)
Inventor
庞露
张棋棋
赵正阳
杜茜
余东方
任鸣
张波
�田�浩
滕飞
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Nanjing University of Information Science and Technology
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Nanjing University of Information Science and Technology
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Abstract

The invention discloses a preparation method of a novel nano rod Bi2O(OH)2SO4 photocatalyst. The preparation method comprises the following steps: preparing a hydrogen peroxide solution, namely adding 30% hydrogen peroxide into water to obtain a hydrogen peroxide solution, wherein the volume ratio of 30% hydrogen peroxide to the water ranges from (1 to 1) to (5 to 1), and stirring; dissolving at a room temperature, namely adding bismuth nitrate and sodium sulfate into the hydrogen peroxide solution, and stirring at a room temperature to dissolve bismuth nitrate so as to prepare a mixed solution with the bismuth nitrate concentration being 0.95mmol/30ml-1.05mmol/30ml, wherein the mol ratio of the bismuth nitrate to the sodium sulfate ranges from (1 to 0.5) to (1 to 2); and carrying out hydrothermal reaction, namely adding the mixed solution into a polytetrafluoroethylene liner and carrying out a constant-temperature hydrothermal reaction at 80-180 DEG C for 2-24 hours, centrifuging, washing and drying to obtain the nano rod Bi2O(OH)2SO4 photocatalyst. The method is simple and feasible and is easy to popularize in a large scale; and compared with a method which is reported by documents, the Bi2O(OH)2SO4 photocatalyst with different shapes and relatively high catalytic activity can be prepared, and can be used for catalyzing and degrading organic pollutants.

Description

A kind of novel nano rod Bi 2o (OH) 2sO 4the preparation method of photochemical catalyst
Technical field
The present invention relates to field of catalyst preparation, be specifically related to a kind of novel nano rod Bi 2o (OH) 2sO 4the preparation method of photochemical catalyst.
Background technology
In recent years, the degrade research of noxious pollutant, waste water or dyestuff of conductor photocatalysis material and technology is adopted to come into one's own.Compared to other technologies, the advantages such as photocatalysis technology has low energy consumption, reaction rate is fast, degraded is thorough, non-secondary pollution, easily recovery.So Treatment by Photocatalysis Oxidation technology, be the method for treating water extremely having application prospect, and day by day become the study hotspot of sewage treatment area.But owing to relating to the many factors such as material cost, chemical stability, anti-light corrosive power and light matching performance, real practical material is still needed optimizing research.TiO 2be the most common and be studied one of maximum catalyst, but its photo-generate electron-hole produced is to being easy to compound, cause electronics and hole can not migrate to surface in time and participate in redox reaction, thus phototranstormation efficiency is lower.Therefore, explore more efficient, stable, have more the new photochemical catalyst of application prospect, be still the focus of photocatalysis research.
Bismuth-containing series compound has purposes widely, not only may be used for pharmaceuticals industry, also can be applicable to semiconductor.Due to the metal that bismuth element is a kind of nontoxic green relatively, in recent years in the preparation of photochemical catalyst, day by day replace compound that is leaded, the toxic element such as antimony, cadmium, mercury.Sulfovinic acid oxygen bismuth as a kind of functional material, the rarely seen report of the research in photocatalysis.The flower-shaped Bi of disclosed You Tianhao invention at present 2o (OH) 2sO 4and hexagon hollow tubulose Bi (CN201410075395.1) 2o (OH) 2sO 4(CN201410075405.1).
Summary of the invention
The object of the present invention is to provide a kind of novel nano rod Bi 2o (OH) 2sO 4the preparation method of photochemical catalyst, the method is simple, be easy to large-scale promotion, can obtain the Bi that shape is different, catalytic activity is higher 2o (OH) 2sO 4photochemical catalyst;
Another object of the present invention is to the novel nano rod Bi providing described method to prepare 2o (OH) 2sO 4photochemical catalyst, the novel nano rod Bi that the method is obtained 2o (OH) 2sO 4photochemical catalyst catalytic activity is higher;
An also object of the present invention is to provide this novel nano rod Bi 2o (OH) 2sO 4the application of photochemical catalyst in catalyze and degrade organic pollutants.
Above-mentioned purpose is achieved by the following technical solution:
A kind of novel nano rod Bi 2o (OH) 2sO 4the preparation method of photochemical catalyst, comprises the steps:
(1) hydrogen peroxide solution preparation: Xiang Shuizhong adds 30% hydrogen peroxide, and the volume ratio of 30% hydrogen peroxide and water is 1:1 ~ 5:1, stirs;
(2) normal-temperature dissolution: add bismuth nitrate and sodium sulphate in hydrogen peroxide solution, stirred at ambient temperature makes bismuth nitrate dissolve, make the mixed solution that bismuth nitrate concentration is 0.95mmol/30ml ~ 1.05mmol/30ml, the mol ratio of bismuth nitrate and sodium sulphate is 1:0.5 ~ 1:2;
(3) hydro-thermal reaction: join in polytetrafluoroethyllining lining by above-mentioned mixed solution, 80 ~ 180 DEG C of incubation water heatings reaction 2 ~ 24 hours, namely obtains nanometer rods Bi after centrifugal, washing, drying 2o (OH) 2sO 4photochemical catalyst.
Further, describedly prepare in the method for bismuthyl fluorite photochemical catalyst, step (2) bismuth nitrate is five water bismuth nitrates.
Further, describedly prepare in the method for bismuthyl fluorite photochemical catalyst, step (3) the incubation water heating reaction time is 5 hours, and temperature is 120 DEG C.
The nanometer rods Bi that above-mentioned preparation method obtains 2o (OH) 2sO 4photochemical catalyst.
The nanometer rods Bi that above-mentioned preparation method obtains 2o (OH) 2sO 4the application of photochemical catalyst in catalyze and degrade organic pollutants.
beneficial effect of the present invention:
1, provided by the invention prepare novel nano rod Bi 2o (OH) 2sO 4the method of photochemical catalyst is simple, is easy to large-scale promotion, obtained novel nano rod Bi 2o (OH) 2sO 4the Bi that the method for photochemical catalyst and existing patent report is obtained 2o (OH) 2sO 4photochemical catalyst form is different, and catalytic activity is higher.
2, the novel nano rod Bi using preparation method of the present invention to prepare 2o (OH) 2sO 4photochemical catalyst Absorbable organic halogens exists, and form is good, and catalytic activity is high, can rhodamine B (RhB) more efficiently in degrading waste water solution.
Accompanying drawing explanation
Fig. 1: nanometer rods Bi prepared by embodiment 1 2o (OH) 2sO 4photochemical catalyst SEM schemes;
Fig. 2: nanometer rods Bi prepared by embodiment 1 2o (OH) 2sO 4photochemical catalyst X-ray diffraction (XRD) figure;
Fig. 3: nanometer rods Bi prepared by embodiment 1 2o (OH) 2sO 4photochemical catalyst and flower-shaped, hexagon hollow tubulose Bi 2o (OH) 2sO 4photochemical catalyst compares RhB catalytic degradation effect.
Detailed description of the invention
Technical scheme of the present invention is described in detail below in conjunction with specific embodiment.
embodiment 1: novel nano rod Bi 2 o (OH) 2 sO 4 the preparation of photochemical catalyst
(1) hydrogen peroxide solution preparation: Xiang Shuizhong adds 30% hydrogen peroxide, and the volume ratio of 30% hydrogen peroxide and water is 1:1;
(2) water-bath is dissolved: get 30ml hydrogen peroxide solution, add five water bismuth nitrate 0.4851g(1mmol) and sodium sulphate 0.1421g(1mmol), stirred at ambient temperature makes bismuth nitrate dissolve and obtains mixed solution;
(3) hydro-thermal reaction: join in polytetrafluoroethyllining lining by above-mentioned mixed solution, 120 DEG C of incubation water heatings react 5 hours, and the centrifugal 3min of 3000 turns/min, uses distilled water and absolute ethanol washing successively, and 60 DEG C of dry 4h, obtain nanometer rods Bi 2o (OH) 2sO 4photochemical catalyst.
As shown in Figure 2, obtained catalyst is pure, and degree of crystallinity is higher; As shown in Figure 1, the shape of this catalyst is bar-shaped, and homogeneity is very high.
embodiment 2: novel nano rod Bi 2 o (OH) 2 sO 4 the preparation of photochemical catalyst
(1) hydrogen peroxide solution preparation: Xiang Shuizhong adds 30% hydrogen peroxide, and the volume ratio of 30% hydrogen peroxide and water is 2:1;
(2) normal-temperature dissolution: get 30ml hydrogen peroxide solution, adds five water bismuth nitrate 0.4608g(0.95mmol) and sodium sulphate 0.0675g(0.475mmol), stirring at room temperature makes bismuth nitrate dissolve and obtains mixed solution;
(3) hydro-thermal reaction: join in polytetrafluoroethyllining lining by above-mentioned mixed solution, 80 DEG C of incubation water heatings react 24 hours, and the centrifugal 3min of 3000 turns/min, uses distilled water and absolute ethanol washing successively, and 60 DEG C of dry 4h, obtain nanometer rods Bi 2o (OH) 2sO 4photochemical catalyst.
Obtained catalyst composition is consistent with embodiment 1, and physical property is similar with catalytic activity.
embodiment 3: novel nano rod Bi 2 o (OH) 2 sO 4 the preparation of photochemical catalyst
(1) hydrogen peroxide solution preparation: Xiang Shuizhong adds 30% hydrogen peroxide, and the volume ratio of 30% hydrogen peroxide and water is 5:1;
(2) normal-temperature dissolution: get 30ml hydrogen peroxide solution, adds five water bismuth nitrate 0.5094g(1.05mmol) and sodium sulphate 0.2984g(2.1mmol), stirring at room temperature makes bismuth nitrate dissolve and obtains mixed solution;
(3) hydro-thermal reaction: join in polytetrafluoroethyllining lining by above-mentioned mixed solution, 180 DEG C of incubation water heatings react 2 hours, and the centrifugal 3min of 3000 turns/min, uses distilled water and absolute ethanol washing successively, and 60 DEG C of dry 4h, obtain nanometer rods Bi 2o (OH) 2sO 4photochemical catalyst.
Obtained catalyst composition is consistent with embodiment 1, and physical property is similar with catalytic activity.
embodiment 4: nanometer rods Bi 2 o (OH) 2 sO 4 photochemical catalyst is to the Degrading experiment of RhB, and flower-shaped, the hexagon hollow tubulose Bi obtained with literature procedure 2 o (OH) 2 sO 4 photochemical catalyst contrasts
Take embodiment 1 and the obtained flower-shaped Bi of literature method (preparation method is shown in CN201410075395.1 and CN201410075405.1) respectively 2o (OH) 2sO 4photochemical catalyst, hexagon hollow tubulose Bi 2o (OH) 2sO 4photochemical catalyst 0.1g, adds the RhB solution of 200ml respectively, and RhB concentration is 10mg/L.First lucifuge stirs 30min, makes dyestuff reach absorption/desorption equilibrium at catalyst surface.Then open xenon source and carry out light-catalyzed reaction under UV-irradiation, supernatant spectrophotometer detects.According to RhB change in concentration in 553nm place light absorption value determination degradation process.
RhB degrades situation as shown in Figure 3, and abscissa is light application time, and ordinate is the ratio of RhB concentration value and the RhB initial concentration measured after irradiating a period of time.As can be seen from Figure, after illumination 50min, novel nano rod Bi prepared by the inventive method 2o (OH) 2sO 4photochemical catalyst energy (A) catalytic degradation RhB 80%, than Bi prepared by existing method 2o (OH) 2sO 4high (the B:CN201410075395.1 of photochemical catalyst catalytic activity; C:CN201410075405.1).

Claims (5)

1. a novel nano rod Bi 2o (OH) 2sO 4the preparation method of photochemical catalyst, is characterized in that comprising the steps:
(1) hydrogen peroxide solution preparation: Xiang Shuizhong adds 30% hydrogen peroxide, and the volume ratio of 30% hydrogen peroxide and water is 1:1 ~ 5:1, stirs;
(2) normal-temperature dissolution: add bismuth nitrate and sodium sulphate in hydrogen peroxide solution, stirred at ambient temperature makes bismuth nitrate dissolve, make the mixed solution that bismuth nitrate concentration is 0.95mmol/30ml ~ 1.05mmol/30ml, the mol ratio of bismuth nitrate and sodium sulphate is 1:0.5 ~ 1:2;
(3) hydro-thermal reaction: join in polytetrafluoroethyllining lining by above-mentioned mixed solution, 80 ~ 180 DEG C of incubation water heatings reaction 2 ~ 24 hours, namely obtains nanometer rods Bi after centrifugal, washing, drying 2o (OH) 2sO 4photochemical catalyst.
2. preparation method according to claim 1, is characterized in that: in step (2), bismuth nitrate is five water bismuth nitrates.
3. preparation method according to claim 1 and 2, is characterized in that: in step (3), the incubation water heating reaction time is 5 hours, and temperature is 120 DEG C.
4. the nanometer rods Bi for preparing of claims 1 to 3 either method 2o (OH) 2sO 4photochemical catalyst.
5. nanometer rods Bi described in claim 4 2o (OH) 2sO 4the application of photochemical catalyst in catalyze and degrade organic pollutants.
CN201510228538.2A 2015-05-07 2015-05-07 Preparation method of novel nano rod Bi2O(OH)2SO4 photocatalyst Pending CN104874409A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108714428A (en) * 2018-06-15 2018-10-30 南京信息工程大学 A kind of nano wire photochemical catalyst and the preparation method and application thereof
CN112520819A (en) * 2020-12-02 2021-03-19 西安建筑科技大学 Bismuth-series three-dimensional microsphere heterojunction photoelectrode and preparation and application thereof

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103253704A (en) * 2013-04-12 2013-08-21 武汉理工大学 Semiconductor porous bismuth oxide nanosphere and preparation method and application thereof
CN103663559A (en) * 2012-09-05 2014-03-26 中国石油化工股份有限公司 Dibismuth trimolybdenum dodecaoxide nanocrystalline as well as preparation method and application thereof
CN103787413A (en) * 2014-03-04 2014-05-14 南京信息工程大学 Preparation method and application of hexagonal hollow tubular Bi2O(OH)2SO4 photocatalyst
CN103785425A (en) * 2014-03-04 2014-05-14 南京信息工程大学 Preparation method and application of flower-like Bi2O(OH)2SO4 photocatalyst

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103663559A (en) * 2012-09-05 2014-03-26 中国石油化工股份有限公司 Dibismuth trimolybdenum dodecaoxide nanocrystalline as well as preparation method and application thereof
CN103253704A (en) * 2013-04-12 2013-08-21 武汉理工大学 Semiconductor porous bismuth oxide nanosphere and preparation method and application thereof
CN103787413A (en) * 2014-03-04 2014-05-14 南京信息工程大学 Preparation method and application of hexagonal hollow tubular Bi2O(OH)2SO4 photocatalyst
CN103785425A (en) * 2014-03-04 2014-05-14 南京信息工程大学 Preparation method and application of flower-like Bi2O(OH)2SO4 photocatalyst

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108714428A (en) * 2018-06-15 2018-10-30 南京信息工程大学 A kind of nano wire photochemical catalyst and the preparation method and application thereof
CN108714428B (en) * 2018-06-15 2021-02-09 南京信息工程大学 Nanowire photocatalyst and preparation method and application thereof
CN112520819A (en) * 2020-12-02 2021-03-19 西安建筑科技大学 Bismuth-series three-dimensional microsphere heterojunction photoelectrode and preparation and application thereof
CN112520819B (en) * 2020-12-02 2023-08-22 西安建筑科技大学 Bismuth-system three-dimensional microsphere heterojunction photoelectrode and preparation and application thereof

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