CN105289680A - Preparation method for visible-light-driven photocatalyst compositing bismuth oxychloride/silver carbonate - Google Patents

Preparation method for visible-light-driven photocatalyst compositing bismuth oxychloride/silver carbonate Download PDF

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Publication number
CN105289680A
CN105289680A CN201510836133.7A CN201510836133A CN105289680A CN 105289680 A CN105289680 A CN 105289680A CN 201510836133 A CN201510836133 A CN 201510836133A CN 105289680 A CN105289680 A CN 105289680A
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bismoclite
preparation
silver carbonate
silver
visible light
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李忠玉
方姗姗
丛田田
梁倩
徐松
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Changzhou University
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Changzhou University
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Abstract

The invention relates to a preparation method for a visible-light-driven photocatalyst compositing bismuth oxychloride/silver carbonate. The preparation method comprises the following steps: preparing bismuth oxychloride; adding bismuth oxychloride into distilled water, performing ultrasonic stirring, adding silver nitrate, performing stirring, adding a sodium bicarbonate solution dropwise, performing stirring, performing centrifugation, washing the product by ethanol and water in turn, and drying the product. The preparation method is simple, and the preparation condition is easy to control. Moreover, the prepared visible-light-driven photocatalyst compositing bismuth oxychloride/silver carbonate is a green catalyst with high performance, is pollution-free, has high catalytic efficiency, and has a certain application value.

Description

The preparation method of bismoclite/silver carbonate composite visible light catalyst
Technical field
The invention belongs to photocatalysis technology field, relate to the preparation method of a kind of bismoclite/silver carbonate composite visible light catalyst.
Background technology
Silver carbonate is the Novel silver salt semiconductor with visible light catalysis activity of up-to-date report, its band gap is 2.30eV, its valence band current potential is 2.673eV, conduction band current potential is 0.373eV, because its band gap is narrower, thus can absorb visible ray, and its valence band current potential has very strong oxidability, because of but more satisfactory visible light catalyst.But due to Ag 2cO 3/ Ag reduction potential is 0.47eV, and thus pure silver carbonate is easy to be reduced into elemental silver under visible light.The generation of elemental silver causes silver carbonate photocatalytic activity to reduce.In order to address this problem, the hetero-junctions that silver carbonate and other semiconductor junction symphysis become can be reduced being combined again of light induced electron and hole, improving visible light catalysis activity further.
Bismoclite is V-VI-VII race's semiconducting compound, and be the novel photocatalyst of development recent years, its crystal structure can be regarded as along c-axis direction, two Cl sheath and Bi 2o 2layer be alternately arranged form layer structure.The energy gap of bismoclite is about 3.4eV, under ultraviolet excitation condition, show certain photocatalysis performance.
This patent mainly adopts in situ Precipitation to prepare bismoclite/silver carbonate composite visible light catalyst, and this catalyst can be applicable in photocatalysis oxidation technique, effectively can remove the organic pollution in environment.
Summary of the invention
The technical problem to be solved in the present invention is: based on the problems referred to above, the invention provides the preparation method of a kind of bismoclite/silver carbonate composite visible light catalyst.
The present invention solves the technical scheme that its technical problem adopts: the preparation method of a kind of bismoclite/silver carbonate composite visible light catalyst, comprises the following steps:
(1) preparation of bismoclite: bismuth nitrate solution and Klorvess Liquid mixing, stir 1 ~ 2h, mixed solution goes in hydrothermal reaction kettle, 150 ~ 180 DEG C of reaction 10 ~ 14h, cooling, and filtering and washing is dried;
(2) preparation of bismoclite/silver carbonate composite photo-catalyst: add bismoclite in distilled water, ultrasonic agitation 1 ~ 3h, adds silver nitrate, stir 30 ~ 50min, dropwise drip sodium bicarbonate solution, stir 24 ~ 28h, centrifugal, successively use ethanol and water washing, dry and obtain product.
Further, in step (1), the mass ratio of potassium chloride and bismuth nitrate is 1:3 ~ 5, and the solvent of bismuth nitrate solution and Klorvess Liquid is ethylene glycol.
Further, in step (2), bismoclite accounts for 2 ~ 4% of silver nitrate quality, and the mass ratio of sodium acid carbonate and silver nitrate is 1:4.
The invention has the beneficial effects as follows: this preparation method is comparatively simple, and preparation condition easily controls, and prepared bismoclite/silver carbonate composite visible light catalyst is environmental protection high performance catalyst, and pollution-free, catalytic efficiency is high, has certain using value.
Accompanying drawing explanation
Below in conjunction with accompanying drawing, the present invention is further described.
Fig. 1 is 10,000 times of scanning electron microscope (SEM) photographs amplified of bismoclite/silver carbonate composite visible light catalyst that the embodiment of the present invention 1 prepares;
Fig. 2 is 30,000 times of scanning electron microscope (SEM) photographs amplified of bismoclite/silver carbonate composite visible light catalyst that the embodiment of the present invention 1 prepares;
Fig. 3 is the X-ray diffractogram of bismoclite/silver carbonate composite visible light catalyst that the embodiment of the present invention 1 prepares;
Fig. 4 is that the ultraviolet-visible absorption spectroscopy of bismoclite/silver carbonate composite visible light catalyst light degradation rhodamine B that the embodiment of the present invention 1 prepares is with light application time variation diagram.
Detailed description of the invention
The invention will be further described in conjunction with specific embodiments now, and following examples are intended to the present invention instead of limitation of the invention further are described.
Embodiment 1
(1) preparation of bismoclite: the ethylene glycol measuring 20mL adds the bismuth nitrate of 1.1184g, the ethylene glycol measuring 20mL again adds the potassium chloride of 0.3728g, 1h is stirred by after above-mentioned two kinds of solution mixing, solution in reaction vessel is gone in hydrothermal reaction kettle, 150 DEG C of reaction 10h, cooling, filtering and washing is dried;
(2) bismoclite of the preparation of bismoclite/silver carbonate composite photo-catalyst: 17mg adds 50mL distilled water, ultrasonic agitation 1h, add 0.85g silver nitrate, stir 30min, dropwise drip the sodium bicarbonate solution of 50mL0.05mol/L again, stir 24h, centrifugal, priority ethanol and water washing, namely obtain product after oven dry.
Embodiment 2
(1) preparation of bismoclite: the ethylene glycol measuring 70mL adds the bismuth nitrate of 6.9520g, the ethylene glycol measuring 70mL again adds the potassium chloride of 1.3904g, 2h is stirred by after above-mentioned two kinds of solution mixing, solution in reaction vessel is gone in hydrothermal reaction kettle, 180 DEG C of reaction 14h, cooling, filtering and washing is dried;
(2) bismoclite of the preparation of bismoclite/silver carbonate composite photo-catalyst: 68mg adds 100mL distilled water, ultrasonic agitation 3h, add 1.70g silver nitrate, stir 50min, dropwise drip the sodium bicarbonate solution of 100mL0.05mol/L again, stir 28h, centrifugal, priority ethanol and water washing, namely obtain product after oven dry.
The performance measurement of bismoclite/silver carbonate composite visible light catalyst
The pattern of the bismoclite/silver carbonate composite visible light catalyst adopting Japanese JSM-6360A type sem observation embodiment 1 to prepare, scanning electron microscope (SEM) photograph as depicted in figs. 1 and 2, as can be seen from Fig., the silver carbonate of the size uniform that the surface distributed of bismoclite is a large amount of in the composite visible light catalyst prepared of present embodiment.
The crystal phase structure of the bismoclite prepared by embodiment 1/silver carbonate composite visible light catalyst is analyzed by Rigaku D/max2500PC rotation x-ray diffractometer, and wherein, X-ray is Cu target K α voltage 40kV, electric current 100mA, step-length is 0.02 °, sweep limits 5 ° ~ 80 °.As shown in Figure 3, as seen from the figure, silver carbonate is the monoclinic phase structure of high-crystallinity to X ray diffracting spectrum, is due to bismoclite a small amount of being entrained in silver carbonate when not having the peak of obvious bismoclite to occur in composite photo-catalyst.
The photocatalysis performance of bismoclite/silver carbonate composite visible light catalyst and potential action oriented research
Using the bismoclite/silver carbonate of preparation in embodiment 1 as photocatalyst for degrading rhodamine B solution, wherein rhodamine B solution concentration 10mg/L, get bismoclite/silver carbonate photochemical catalyst 40mg, first dark reaction 30min reaches adsorption-desorption balance, carry out visible light catalytic reaction again, use 1000w xenon lamp as light source, extract 5ml reactant liquor with dropper at regular intervals, put into supercentrifuge centrifugal 4 minutes, the light degradation situation of rhodamine B utilizes ultraviolet-uisible spectrophotometer to detect.
Bismoclite prepared by embodiment 1/silver carbonate composite visible light catalyst to the degradation property of rhodamine B as shown in Figure 4.As seen from Figure 4, in 100 minutes, rhodamine B is almost degradable, and visible bismoclite/silver carbonate composite visible light catalyst has higher photocatalytic activity.
With above-mentioned according to desirable embodiment of the present invention for enlightenment, by above-mentioned description, relevant staff in the scope not departing from this invention technological thought, can carry out various change and amendment completely.The technical scope of this invention is not limited to the content on description, must determine its technical scope according to right.

Claims (3)

1. a preparation method for bismoclite/silver carbonate composite visible light catalyst, is characterized in that: comprise the following steps:
(1) preparation of bismoclite: bismuth nitrate solution and Klorvess Liquid mixing, stir 1 ~ 2h, mixed solution goes in hydrothermal reaction kettle, 150 ~ 180 DEG C of reaction 10 ~ 14h, cooling, and filtering and washing is dried;
(2) preparation of bismoclite/silver carbonate composite photo-catalyst: add bismoclite in distilled water, ultrasonic agitation 1 ~ 3h, adds silver nitrate, stir 30 ~ 50min, dropwise drip sodium bicarbonate solution, stir 24 ~ 28h, centrifugal, successively use ethanol and water washing, dry and obtain product.
2. the preparation method of bismoclite according to claim 1/silver carbonate composite visible light catalyst, it is characterized in that: in described step (1), the mass ratio of potassium chloride and bismuth nitrate is 1:3 ~ 5, and the solvent of bismuth nitrate solution and Klorvess Liquid is ethylene glycol.
3. the preparation method of bismoclite according to claim 1/silver carbonate composite visible light catalyst, is characterized in that: in described step (2), bismoclite accounts for 2 ~ 4% of silver nitrate quality, and the mass ratio of sodium acid carbonate and silver nitrate is 1:4.
CN201510836133.7A 2015-11-26 2015-11-26 Preparation method for visible-light-driven photocatalyst compositing bismuth oxychloride/silver carbonate Pending CN105289680A (en)

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Cited By (8)

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CN105709782A (en) * 2016-03-09 2016-06-29 安徽工业大学 Preparing method and application of Ag/AgBr/BiOCl-(001) nanometer composite material
CN106984351A (en) * 2017-04-01 2017-07-28 常州大学 A kind of preparation method of bismoclite@cadmium sulfides/silver carbonate composite visible light catalyst
CN106984350A (en) * 2017-03-30 2017-07-28 常州大学 A kind of silver carbonate is combined the preparation method of silver bromide photochemical catalyst
CN107262120A (en) * 2017-07-11 2017-10-20 四川理工学院 The preparation method that a kind of BiOCl surface photovoltages signal is significantly increased
CN109833887A (en) * 2019-03-13 2019-06-04 华南农业大学 A kind of preparation method of Visible Light Induced Photocatalytic organic dyestuff composite catalyst
CN113019409A (en) * 2021-03-23 2021-06-25 四川轻化工大学 Bi2O2CO3Preparation method and application of/BiOCl catalyst
CN114272943A (en) * 2021-11-26 2022-04-05 国家能源集团科学技术研究院有限公司 Preparation method and application of composite catalyst
CN114318845A (en) * 2021-12-24 2022-04-12 盐城工学院 Fabric finishing method based on metal salt bismuth oxybromide photocatalytic material

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CN103878000A (en) * 2014-03-21 2014-06-25 三峡大学 Bismuth oxyhalide photocatalyst and preparation method thereof
CN104646037A (en) * 2015-01-12 2015-05-27 内蒙古科技大学 BiOXs pholocatalyst, grapheme-compounded BiOXs pholocatalyst and preparation method thereof

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CN104646037A (en) * 2015-01-12 2015-05-27 内蒙古科技大学 BiOXs pholocatalyst, grapheme-compounded BiOXs pholocatalyst and preparation method thereof

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Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105709782A (en) * 2016-03-09 2016-06-29 安徽工业大学 Preparing method and application of Ag/AgBr/BiOCl-(001) nanometer composite material
CN106984350A (en) * 2017-03-30 2017-07-28 常州大学 A kind of silver carbonate is combined the preparation method of silver bromide photochemical catalyst
CN106984351A (en) * 2017-04-01 2017-07-28 常州大学 A kind of preparation method of bismoclite@cadmium sulfides/silver carbonate composite visible light catalyst
CN106984351B (en) * 2017-04-01 2019-11-12 常州大学 A kind of preparation method of bismuth oxychloride@cadmium sulfide/silver carbonate composite visible light catalyst
CN107262120A (en) * 2017-07-11 2017-10-20 四川理工学院 The preparation method that a kind of BiOCl surface photovoltages signal is significantly increased
CN107262120B (en) * 2017-07-11 2020-01-31 四川理工学院 Preparation method for remarkably enhancing BiOCl surface photovoltage signals
CN109833887A (en) * 2019-03-13 2019-06-04 华南农业大学 A kind of preparation method of Visible Light Induced Photocatalytic organic dyestuff composite catalyst
CN113019409A (en) * 2021-03-23 2021-06-25 四川轻化工大学 Bi2O2CO3Preparation method and application of/BiOCl catalyst
CN114272943A (en) * 2021-11-26 2022-04-05 国家能源集团科学技术研究院有限公司 Preparation method and application of composite catalyst
CN114318845A (en) * 2021-12-24 2022-04-12 盐城工学院 Fabric finishing method based on metal salt bismuth oxybromide photocatalytic material

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