CN109289880A - A kind of BiOI (100)/BiOI (001) is the same as phase homojunction and preparation method - Google Patents

A kind of BiOI (100)/BiOI (001) is the same as phase homojunction and preparation method Download PDF

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CN109289880A
CN109289880A CN201811085111.1A CN201811085111A CN109289880A CN 109289880 A CN109289880 A CN 109289880A CN 201811085111 A CN201811085111 A CN 201811085111A CN 109289880 A CN109289880 A CN 109289880A
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bioi
solution
phase
homojunction
bismuth oxide
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单连伟
肖彦薇
卢长慧
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Harbin University of Science and Technology
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    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J27/00Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
    • B01J27/06Halogens; Compounds thereof
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J35/00Catalysts, in general, characterised by their form or physical properties
    • B01J35/30Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
    • B01J35/39Photocatalytic properties
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J35/00Catalysts, in general, characterised by their form or physical properties
    • B01J35/50Catalysts, in general, characterised by their form or physical properties characterised by their shape or configuration
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J37/00Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
    • B01J37/08Heat treatment
    • B01J37/10Heat treatment in the presence of water, e.g. steam
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/30Treatment of water, waste water, or sewage by irradiation
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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    • C02F2101/308Dyes; Colorants; Fluorescent agents
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00Nature of the contaminant
    • C02F2101/30Organic compounds
    • C02F2101/34Organic compounds containing oxygen
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00Nature of the contaminant
    • C02F2101/30Organic compounds
    • C02F2101/36Organic compounds containing halogen
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00Nature of the contaminant
    • C02F2101/30Organic compounds
    • C02F2101/38Organic compounds containing nitrogen
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2305/00Use of specific compounds during water treatment
    • C02F2305/10Photocatalysts

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Abstract

The present invention relates to a kind of BiOI (100)/BiOI (001) with phase homojunction and preparation method.Steps are as follows for preparation method of the present invention: first with Bi (NO3)3•5H2O and KI, BiOI (100) basis material is prepared under hydrothermal conditions, obtained BiOI (100) basis material is mixed with the bismuth oxide powder of preparation, under hydrochloric acid effect bismuth oxide powder is converted to BiOI (001) in situ, and forms BiOI (100)/BiOI (001) with phase homojunction with BiOI (100).The advantages that present invention has preparation process novel, and operating process is simple, and low production cost, reaction condition is mild, is easy to large-scale production.

Description

A kind of BiOI (100)/BiOI (001) is the same as phase homojunction and preparation method
Technical field
The invention belongs to field of functional materials, it is related to a kind of BiOI (100)/BiOI (001) with phase homojunction and preparation side Method.
Background technique
With a large amount of consumption of the fossil fuels such as petroleum, natural gas, coal, such as acid rain, haze, photochemical fog are produced Etc. environmental problems.Since photocatalysis technology can directly solve energy problem using sunlight, air, water pollution are handled, Therefore it has obtained more and more attention, and photochemical catalyst is Key technique problem in this art.Conductor photocatalysis oxygen The photo-generate electron-hole pairs oxidative degradation organic pollutant that change technology utilizes illumination to generate, reaction efficiency is high, and stability is strong.Chlorine oxygen Changing bismuth is novel photocatalyst developed in recent years, cheap and easy to get and environmental-friendly, but itself photocatalytic activity is weaker, It is considered as improving the approach of its photocatalysis performance by further modification.For example, Sun etc. is with Bi (NO3)3•5H2O, KI is Primary raw material has prepared BiOI by low temperature water-bath method, has then used hydro-thermal method with Bi (NO3)3•5H2O, KCl is primary raw material, BiOCl has been obtained after 160 °C of lower 24 h of hydro-thermal, has been heat-treated 3 under 250 °C after BiOI and BiOCl powder is uniformly dispersed H is obtained with BiOI/BiOCl material (ACS Catal., 2015,5:3540 3551).Kim etc. is with Bi (NO3)3•5H2O、 KCl, KI are primary raw material, have obtained BiOI after 120 °C of lower 12 h of hydro-thermal reactionxI1−x(Applied Catalysis B: Environmental, 20141,47:711-725).The prior art is in terms of the photocatalysis performance for improving bismuth oxychloride, mainly It is all by introducing the means such as the second phase or doping, preparation process complexity causes production cost excessively high, it is difficult to realize extensive Production.So far, there is not been reported with the related work of phase homojunction by one pack system BiOI (100)/BiOI (001), by not Face face between preferentially exposing with BiOI crystallography face is compound, improves the photo-generated carrier separative efficiency of BiOI, urges for novel light Agent design provides new mentality of designing.
Summary of the invention
The purpose of the present invention is to provide a kind of BiOI (100)/BiOI (001) with the system of phase homojunction high efficiency photocatalyst Preparation Method has photocatalysis performance high, and low production cost is with short production cycle, is easy to the advantages that being mass produced.
The present invention adopts the following technical scheme:
Step 1, by a certain amount of Bi (NO3)3•5H2O is dissolved in nitric acid solution, KI solution is added, wherein Bi (NO3)3•5H2O It is 1:1 with the ratio between KI moles, then pH value is adjusted with NaOH solution, until pH=5.5~6.0 of mixed solution;
Step 2, in the solution investment reaction kettle step 1 obtained, hydro-thermal reaction 12 ~ 18 hours at 140~180oC, The BiOI powder of (100) face exposure will be obtained after precipitating filtering, cleaning;
Step 3, it weighs a certain amount of five water bismuth nitrate to be dissolved in the mixed solution of nitric acid and citric acid, then uses NaOH solution The pH for adjusting pH value to solution is 6~7, makes 0.35~0.75mol/L of concentration of five water bismuth nitrates;
Step 4, will the solution that obtained in the step 3 it is dry after obtain colloidal sol, be dried, grind, sieving, 400~ 3~5h is calcined at 450 DEG C, obtains bismuth oxide powder;
Step 5, bismuth oxide powder is mixed with BiOI powder obtained in step 2, ultrasonic disperse after deionized water is added, then Hydrochloric acid solution is added in above-mentioned system, wherein BiOI powder and bismuth oxide powder molar ratio are 1:(0 ~ 0.5), bismuth oxide with Hydrochloric acid molar ratio is 1:(7 ~ 9), precipitating is washed 3 times repeatedly using ethyl alcohol and deionized water, obtained after dry BiOI (100)/ BiOI (001) is the same as phase homojunction.
The BiOI (100)/BiOI (001) is the same as phase homojunction and preparation method, which is characterized in that the BiOI (100)/BiOI (001) is tetragonal phase, the BiOI with the structure of BiOI (100) and BiOI (001) in phase homojunction (100) the application of/BiOI (001) with phase homojunction in terms of photocatalysis.Compared with prior art, the present invention has beneficial below Effect:
The present invention is combined with soft chemical method using hydro-thermal method and is prepared for BiOI (100)/BiOI (001) with phase homojunction complex light Catalyst, present invention raising BiOI (100) more more efficient than the method for traditional physical mixed or Surface Creation and BiOI (001) Effective contact area, the present invention has novel design in the photocatalysis performance for not changing system ingredient premise down regulation BiOI, The advantages that production cost is low, short preparation period.
Detailed description of the invention
Fig. 1 is BiOI (100)/BiOI (001) for preparing in the embodiment of the present invention 1~3 with phase homojunction, BiOI (100) With the XRD diffracting spectrum of BiOI (001);
Fig. 2 is that BiOI (the 100)/BiOI (001) prepared in the embodiment of the present invention 1 schemes with the TEM of phase homojunction;
Fig. 3 is BiOI (100)/BiOI (001) for preparing in the embodiment of the present invention 1~3 with phase homojunction, BiOI (100) and The Photocatalytic Decoloration rate curve of BiOI (001);
Fig. 4 is BiOI (100)/BiOI (001) for preparing in the embodiment of the present invention 1~3 with phase homojunction, BiOI (100) and The fluorescence spectra of BiOI (001).
Specific embodiment
The present invention is described further with currently preferred specific embodiment with reference to the accompanying drawing, raw material is analysis It is pure.
Embodiment 1:
Step 1, by a certain amount of Bi (NO3)3•5H2O is dissolved in nitric acid solution, KI solution is added, wherein Bi (NO3)3•5H2O It is 1:1, Bi (NO with the ratio between KI moles3)3•5H2The concentration of O is 0.3mol/L, and the concentration of KI solution is 0.3mol/L, is then used NaOH solution adjusts pH value, until the pH=6.0 of mixed solution;
Step 2, in the solution investment reaction kettle step 1 obtained, hydro-thermal reaction 12 hours at 160oC will be precipitated The BiOI powder of (100) face exposure is obtained after filter, cleaning;
Step 3, it weighs a certain amount of five water bismuth nitrate to be dissolved in the mixed solution of nitric acid and citric acid, then uses NaOH solution The pH for adjusting pH value to solution is 6, makes the concentration 0.65mol/L of five water bismuth nitrates;
Step 4, colloidal sol will be obtained after the solution obtained in the step 3 drying, is dried, grinds, sieving, at 400 DEG C Lower calcining 4h, obtains bismuth oxide powder;
Step 5, bismuth oxide powder is mixed with BiOI powder obtained in step 2, ultrasonic disperse after deionized water is added, then Hydrochloric acid solution is added in above-mentioned system, wherein BiOI powder and bismuth oxide powder molar ratio are 1:0.2, bismuth oxide and hydrochloric acid Molar ratio is 1:8, and precipitating is washed 3 times repeatedly using ethyl alcohol and deionized water, obtains BiOI (100)/BiOI (001) after dry With phase homojunction.
Embodiment 2:
Step 1, by a certain amount of Bi (NO3)3•5H2O is dissolved in nitric acid solution, KI solution is added, wherein Bi (NO3)3•5H2O It is 1:1, Bi (NO with the ratio between KI moles3)3•5H2The concentration of O is 0.3mol/L, and the concentration of KI solution is 0.3mol/L, is then used NaOH solution adjusts pH value, until the pH=6.0 of mixed solution;
Step 2, in the solution investment reaction kettle step 1 obtained, hydro-thermal reaction 12 hours at 160oC will be precipitated The BiOI powder of (100) face exposure is obtained after filter, cleaning.
Embodiment 3:
Step 1, it weighs a certain amount of five water bismuth nitrate to be dissolved in the mixed solution of nitric acid and citric acid, then uses NaOH solution The pH for adjusting pH value to solution is 6, makes the concentration 0.65mol/L of five water bismuth nitrates;
Step 2, colloidal sol will be obtained after the solution obtained in the step 2 drying, is dried, grinds, sieving, at 420 DEG C Lower calcining 4h, obtains bismuth oxide powder.
Step 3, a certain amount of bismuth oxide powder is dispersed in 100mL deionized water, HCl acid solution is added dropwise, The molar ratio of middle bismuth oxide and HCl acid is 1:(7~9), HCl acid continues stirring 3~5 hours after dripping, by precipitating filtering, use Deionized water washs repeatedly, obtains the BiOI powder of (001) face exposure after drying.
Application examples:
To BiOI (100)/BiOI (001) obtained in implementation column 1~3 with phase homojunction, BiOI (100) and BiOI (001) Carry out photocatalytic activity evaluation, concrete operation step are as follows:
BiOI (100)/BiOI (001) obtained in Examples 1 to 3 is weighed with phase homojunction, BiOI (100) and BiOI (001) 100 mg of photochemical catalyst is taken respectively, add it in rhdamine B solution (100mL, 3.5 × 10-5mol·L-1), it is protected from light stirring 1h, opens 500W xenon source after De contamination reaches balance, detects the concentration of a dyestuff every 30min, Material prepared is symbolized within given time to the catalytic decolorization situation of rhodamine B.
Above said content is only the basic explanation under present inventive concept, by reading description of the invention to the present invention Any equivalent transformation that technical solution is taken should all belong to this hair as long as it does not depart from the spirit and scope of the technical scheme of the present invention Bright protection scope.

Claims (7)

1. a kind of BiOI (100)/BiOI (001) is the same as phase homojunction and preparation method, it is characterised in that knot is tetragonal phase structure, A kind of group is divided into (001) face and preferentially exposes, and another group is divided into (100) face and preferentially exposes, and specifically includes following preparation step:
Step 1, by a certain amount of Bi (NO3)3•5H2O is dissolved in nitric acid solution, KI solution is added, wherein Bi (NO3)3•5H2O It is 1:1 with the ratio between KI moles, then pH value is adjusted with NaOH solution, until pH=5.5~6.0 of mixed solution;
Step 2, in the solution investment reaction kettle step 1 obtained, hydro-thermal reaction 12 ~ 18 hours at 140~180oC, The BiOI powder of (100) face exposure will be obtained after precipitating filtering, cleaning;
Step 3, it weighs a certain amount of five water bismuth nitrate to be dissolved in the mixed solution of nitric acid and citric acid, then uses NaOH solution The pH for adjusting pH value to solution is 6~7, makes 0.35~0.75mol/L of concentration of five water bismuth nitrates;
Step 4, will the solution that obtained in the step 3 it is dry after obtain colloidal sol, be dried, grind, sieving, 400~ 3~5h is calcined at 450 DEG C, obtains bismuth oxide powder;
Step 5, bismuth oxide powder is mixed with BiOI powder obtained in step 2, ultrasonic disperse after deionized water is added, then Hydrochloric acid solution is added in above-mentioned system, wherein BiOI powder and bismuth oxide powder molar ratio are 1:(0 ~ 0.5), bismuth oxide with Hydrochloric acid molar ratio is 1:(7 ~ 9), precipitating is washed 3 times repeatedly using ethyl alcohol and deionized water, obtained after dry BiOI (100)/ BiOI (001) is the same as phase homojunction.
2. Bi (NO in the step 13)3•5H2The concentration of O is 0.2~0.5mol/L, and the concentration of KI solution is 0.2~0.5mol/ L。
3. hydrothermal temperature is 140~180oC in the step 2, the hydro-thermal time is 12 ~ 18 hours.
4. the pH of solution is 6~7 in the step 3, the concentration of five water bismuth nitrates is 0.35~0.75mol/L.
5. calcination temperature is 360~420 DEG C in the step 4, calcination time is 3~5h.
6. BiOI and bismuth oxide molar ratio are 1:(0 ~ 0.5 in the step 5), concentration of hydrochloric acid solution is 0.05~0.1 mol/L, Bismuth oxide and hydrochloric acid molar ratio are 1:(7 ~ 9).
7. the BiOI (100)/application of the BiOI (001) with phase homojunction in terms of photocatalysis.
CN201811085111.1A 2018-09-18 2018-09-18 A kind of BiOI (100)/BiOI (001) is the same as phase homojunction and preparation method Pending CN109289880A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109731563A (en) * 2019-02-25 2019-05-10 辽宁石油化工大学 It is a kind of to tie photochemical catalyst and its preparation method and application with phase
CN114160171A (en) * 2021-11-10 2022-03-11 中国电建集团成都勘测设计研究院有限公司 CeO2-La3+Preparation method of/BiOI composite material and method for removing sulfadiazine in water

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109731563A (en) * 2019-02-25 2019-05-10 辽宁石油化工大学 It is a kind of to tie photochemical catalyst and its preparation method and application with phase
CN109731563B (en) * 2019-02-25 2022-01-21 辽宁石油化工大学 In-phase junction photocatalyst and preparation method and application thereof
CN114160171A (en) * 2021-11-10 2022-03-11 中国电建集团成都勘测设计研究院有限公司 CeO2-La3+Preparation method of/BiOI composite material and method for removing sulfadiazine in water

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Application publication date: 20190201