CN107837813A - Chlorine oxygen bismuth/modified montmorillonoid composite photo-catalyst and its preparation method and application - Google Patents
Chlorine oxygen bismuth/modified montmorillonoid composite photo-catalyst and its preparation method and application Download PDFInfo
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- CN107837813A CN107837813A CN201711167331.4A CN201711167331A CN107837813A CN 107837813 A CN107837813 A CN 107837813A CN 201711167331 A CN201711167331 A CN 201711167331A CN 107837813 A CN107837813 A CN 107837813A
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- modified montmorillonoid
- bismuth
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- bismuth nitrate
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- 239000002131 composite material Substances 0.000 title claims abstract description 31
- AHUBLGVDRKDHAT-UHFFFAOYSA-N [Bi]=O.[Cl] Chemical compound [Bi]=O.[Cl] AHUBLGVDRKDHAT-UHFFFAOYSA-N 0.000 title claims abstract description 27
- 239000011941 photocatalyst Substances 0.000 title claims abstract description 27
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims abstract description 51
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 28
- 238000006243 chemical reaction Methods 0.000 claims abstract description 23
- 239000012153 distilled water Substances 0.000 claims abstract description 21
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 claims abstract description 18
- RXPAJWPEYBDXOG-UHFFFAOYSA-N hydron;methyl 4-methoxypyridine-2-carboxylate;chloride Chemical compound Cl.COC(=O)C1=CC(OC)=CC=N1 RXPAJWPEYBDXOG-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000000725 suspension Substances 0.000 claims abstract description 14
- 235000011164 potassium chloride Nutrition 0.000 claims abstract description 9
- 239000001103 potassium chloride Substances 0.000 claims abstract description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000013019 agitation Methods 0.000 claims abstract description 8
- 239000012065 filter cake Substances 0.000 claims abstract description 8
- 238000003760 magnetic stirring Methods 0.000 claims abstract description 8
- IQUPABOKLQSFBK-UHFFFAOYSA-N 2-nitrophenol Chemical compound OC1=CC=CC=C1[N+]([O-])=O IQUPABOKLQSFBK-UHFFFAOYSA-N 0.000 claims description 24
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 claims description 22
- BTJIUGUIPKRLHP-UHFFFAOYSA-N 4-nitrophenol Chemical compound OC1=CC=C([N+]([O-])=O)C=C1 BTJIUGUIPKRLHP-UHFFFAOYSA-N 0.000 claims description 16
- 229910052797 bismuth Inorganic materials 0.000 claims description 15
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 claims description 15
- 238000012986 modification Methods 0.000 claims description 8
- 239000005416 organic matter Substances 0.000 claims description 4
- 230000000593 degrading effect Effects 0.000 claims description 2
- 230000001699 photocatalysis Effects 0.000 abstract description 9
- 238000007146 photocatalysis Methods 0.000 abstract description 6
- 238000005516 engineering process Methods 0.000 abstract description 5
- 238000003889 chemical engineering Methods 0.000 abstract description 2
- 239000003256 environmental substance Substances 0.000 abstract description 2
- KZBUYRJDOAKODT-UHFFFAOYSA-N Chlorine Chemical compound ClCl KZBUYRJDOAKODT-UHFFFAOYSA-N 0.000 abstract 1
- 239000000460 chlorine Substances 0.000 abstract 1
- 229910052801 chlorine Inorganic materials 0.000 abstract 1
- CJJMLLCUQDSZIZ-UHFFFAOYSA-N oxobismuth Chemical compound [Bi]=O CJJMLLCUQDSZIZ-UHFFFAOYSA-N 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 37
- 239000003054 catalyst Substances 0.000 description 17
- 238000006731 degradation reaction Methods 0.000 description 11
- 238000000034 method Methods 0.000 description 10
- BWOROQSFKKODDR-UHFFFAOYSA-N oxobismuth;hydrochloride Chemical compound Cl.[Bi]=O BWOROQSFKKODDR-UHFFFAOYSA-N 0.000 description 9
- 230000015556 catabolic process Effects 0.000 description 8
- 238000010521 absorption reaction Methods 0.000 description 6
- 239000003795 chemical substances by application Substances 0.000 description 6
- GUJOJGAPFQRJSV-UHFFFAOYSA-N dialuminum;dioxosilane;oxygen(2-);hydrate Chemical compound O.[O-2].[O-2].[O-2].[Al+3].[Al+3].O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O GUJOJGAPFQRJSV-UHFFFAOYSA-N 0.000 description 6
- 239000000463 material Substances 0.000 description 6
- 229910052901 montmorillonite Inorganic materials 0.000 description 6
- 230000000694 effects Effects 0.000 description 5
- 230000003647 oxidation Effects 0.000 description 5
- 238000007254 oxidation reaction Methods 0.000 description 5
- OEHNVKBOQOXOJN-UHFFFAOYSA-N 2-(4-nitrophenyl)phenol Chemical compound OC1=CC=CC=C1C1=CC=C([N+]([O-])=O)C=C1 OEHNVKBOQOXOJN-UHFFFAOYSA-N 0.000 description 4
- 238000006555 catalytic reaction Methods 0.000 description 4
- 230000008859 change Effects 0.000 description 4
- 239000007788 liquid Substances 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- 239000004065 semiconductor Substances 0.000 description 4
- 239000007787 solid Substances 0.000 description 4
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- 238000002835 absorbance Methods 0.000 description 3
- 239000002253 acid Substances 0.000 description 3
- 239000007864 aqueous solution Substances 0.000 description 3
- PPNKDDZCLDMRHS-UHFFFAOYSA-N dinitrooxybismuthanyl nitrate Chemical class [Bi+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O PPNKDDZCLDMRHS-UHFFFAOYSA-N 0.000 description 3
- 238000002474 experimental method Methods 0.000 description 3
- 238000005286 illumination Methods 0.000 description 3
- 238000001179 sorption measurement Methods 0.000 description 3
- 238000002336 sorption--desorption measurement Methods 0.000 description 3
- 238000000870 ultraviolet spectroscopy Methods 0.000 description 3
- MPVDXIMFBOLMNW-ISLYRVAYSA-N 7-hydroxy-8-[(E)-phenyldiazenyl]naphthalene-1,3-disulfonic acid Chemical compound OC1=CC=C2C=C(S(O)(=O)=O)C=C(S(O)(=O)=O)C2=C1\N=N\C1=CC=CC=C1 MPVDXIMFBOLMNW-ISLYRVAYSA-N 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000005342 ion exchange Methods 0.000 description 2
- 239000002957 persistent organic pollutant Substances 0.000 description 2
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 230000009257 reactivity Effects 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- PYWVYCXTNDRMGF-UHFFFAOYSA-N rhodamine B Chemical compound [Cl-].C=12C=CC(=[N+](CC)CC)C=C2OC2=CC(N(CC)CC)=CC=C2C=1C1=CC=CC=C1C(O)=O PYWVYCXTNDRMGF-UHFFFAOYSA-N 0.000 description 2
- 229940043267 rhodamine b Drugs 0.000 description 2
- 239000002689 soil Substances 0.000 description 2
- 239000002351 wastewater Substances 0.000 description 2
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 1
- WGKMWBIFNQLOKM-UHFFFAOYSA-N [O].[Cl] Chemical compound [O].[Cl] WGKMWBIFNQLOKM-UHFFFAOYSA-N 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000004927 clay Substances 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000005518 electrochemistry Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000000383 hazardous chemical Substances 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000010842 industrial wastewater Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 229910052976 metal sulfide Inorganic materials 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 230000007096 poisonous effect Effects 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000001338 self-assembly Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000008961 swelling Effects 0.000 description 1
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/06—Halogens; Compounds thereof
- B01J27/08—Halides
- B01J27/10—Chlorides
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/34—Organic compounds containing oxygen
- C02F2101/345—Phenols
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/38—Organic compounds containing nitrogen
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Health & Medical Sciences (AREA)
- Toxicology (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Catalysts (AREA)
Abstract
The invention belongs to environmental chemical engineering photocatalysis water-treatment technology field, and in particular to a kind of chlorine oxygen bismuth/modified montmorillonoid composite photo-catalyst and its preparation method and application.Chlorine oxygen bismuth/modified montmorillonoid composite photo-catalyst of the present invention, is prepared by following steps：(1) bismuth nitrate and potassium chloride are placed in ethylene glycol, reaction under magnetic stirring forms settled solution；Modified montmorillonoid is added into above-mentioned settled solution, and 0.5~1.5h of ultrasonic disperse, forms bismuth nitrate modified montmorillonoid suspension；(2) distilled water is added under the conditions of magnetic agitation in bismuth nitrate modified montmorillonoid suspension obtained by step (1), continues 1~2h of reaction, standby aaerosol solution is made；(3) the standby aaerosol solution for obtaining step (2) is filtered, and filter cake is washed 3~5 times with distilled water and absolute ethyl alcohol, then dried at a temperature of 40~50 DEG C, that is, chlorine oxygen bismuth/modified montmorillonoid composite photo-catalyst is made.
Description
Technical field
The invention belongs to environmental chemical engineering photocatalysis water-treatment technology field, and in particular to a kind of chlorine oxygen bismuth/modified montmorillonoid
Composite photo-catalyst and its preparation method and application.
Background technology
With the development of modern industry, it is dirty currently the most important water body has been turned into organic pollution caused by its production
One of dye source.The complicated component of industrial wastewater containing organic pollution, difficult thoroughly degraded and TOC values are higher, and give ecological environment band
To seriously endanger.Method of the processing containing organic pollutant wastewater mainly has at present：Physisorphtion, membrane separation process, electrochemistry oxygen
Change method and ultrasonic degradation technology etc..Compared with these technologies, semiconductor-based photocatalysis oxidation technique developed in recent years
Have the characteristics that energy consumption is low, environment-friendly and degradable thorough.In numerous semiconductor materials applied to photocatalysis oxidation technique
In material, chlorine oxygen bismuth (BiOCl) shows the reactivity of good photocatalysis degradation organic contaminant, and this is primarily due to
The layer structure and built in field of BiOCl high anisotropies.But BiOCl specific surface area is smaller, and absorption property compared with
Difference, this limits BiOCl light-catalyzed reaction activity to a certain extent.Therefore, how photocatalytic semiconductor material pair is strengthened
The absorption property of organic pollution turns into the focus of people's research.Montmorillonite --- a kind of layered silicate material --- is because its is big
Specific surface area, excellent swelling behavior, absorption property and ion-exchange performance etc., turn into a kind of good solid matrix.By
Advantage in terms of preparation and immobilization of the montmorillonite in nano particle, has prepared many montmorillonite-semiconductor composites,
Including metal (Catalysis Letters, 1990,6:401-407), metal oxide (Materials Letters 2011,
65:657-660) and metal sulfide (Materials Letters 2008,62:3722-3723) composite nano materials.Mesh
Before, the research of some existing BiOX/ montmorillonite Composite photochemical catalysts is reported.Xu etc., which reports BiOBr/ under ultrasonic wave added and covered, to be taken off
The preparation of native composite photo-catalyst, the catalyst show good absorption and photocatalytic activity, catalyst amount to rhodamine B
For 1gL-1 when, 98.96% rhodamine B solution (40mgL-1) was degraded (Journal of in 120 minutes
Hazardous Materials,2014,275:185-192).Xu etc. is prepared for BiOCl/ montmorillonite Composite photochemical catalysts, and this is urged
Agent increases substantially to the degrading activity of orange G than the activity of BiOCl catalyst.When catalyst amount is 0.15gL-1,
40mgL-1 orange G solution be completely degraded in 60 minutes (Applied Clay Science, 2017,147:28-
35)。
The content of the invention
A kind of chlorine oxygen bismuth/preparation of modified montmorillonoid composite photo-catalyst of the present invention and the purpose of application process are to be directed to
The problem of BiOCl is to Organic Pollutants in Wastewater adsorption capacity and low photocatalytic activity, propose a kind of using modified montmorillonoid
Bigger serface, strong absorption property and ion-exchange performance, make BiOCl photochemical catalysts and modified montmorillonoid compound, urged with enhancing
Agent improves BiOCl photo-generated carriers separative efficiency and its adsorption capacity to organic pollution to the utilization ratio of luminous energy, and
Strengthen its light-catalyzed reaction activity.Using bismuth nitrate, potassium chloride and modified montmorillonoid as raw material, ethylene glycol is solvent, prepares chlorine oxygen
The method of bismuth/modified montmorillonoid composite photo-catalyst.This method can improve absorption and photocatalysis of the catalyst to organic pollution
Degradation capability, and the problem of can solve the problem that environmental pollution.
The present invention to achieve the above object and the technical scheme taken is：
A kind of chlorine oxygen bismuth/modified montmorillonoid composite photo-catalyst, is prepared by following steps：
(1) it is 1 in molar ratio by bismuth nitrate and potassium chloride：1~3 is placed in ethylene glycol, mole of ethylene glycol and bismuth nitrate
Than for 9~15：1, reaction under magnetic stirring forms settled solution；Modified montmorillonoid is added into above-mentioned settled solution, it is modified to cover
The mol ratio of de- soil and bismuth nitrate is 1：25~80, and 0.5~1.5h of ultrasonic disperse, form bismuth nitrate-modified montmorillonoid and suspend
Liquid；
(2) distilled water is added to by bismuth nitrate-modification obtained by step (1) with 1mL/min speed under the conditions of magnetic agitation
In montmorillonite suspension liquid, continue 1~2h of reaction, reaction temperature is controlled at 20~25 DEG C, standby aaerosol solution is made, wherein distilling
The volume ratio of water and ethylene glycol is 1：1~4；
(3) the standby aaerosol solution for obtaining step (2) is filtered, and filter cake is washed 3~5 times with distilled water and absolute ethyl alcohol,
Then dried at a temperature of 40~50 DEG C, that is, chlorine oxygen bismuth/modified montmorillonoid composite photo-catalyst is made.
The preparation method of chlorine oxygen bismuth/modified montmorillonoid composite photo-catalyst of the present invention, comprises the following steps：
(1) it is 1 in molar ratio by bismuth nitrate and potassium chloride：1~3 is placed in ethylene glycol, mole of ethylene glycol and bismuth nitrate
Than for 9~15：1, reaction under magnetic stirring forms settled solution；Modified montmorillonoid is added into above-mentioned settled solution, it is modified to cover
The mol ratio of de- soil and bismuth nitrate is 1：25~80, and 0.5~1.5h of ultrasonic disperse, form bismuth nitrate-modified montmorillonoid and suspend
Liquid；
(2) distilled water is added to by bismuth nitrate-modification obtained by step (1) with 1mL/min speed under the conditions of magnetic agitation
In montmorillonite suspension liquid, continue 1~2h of reaction, reaction temperature is controlled at 20~25 DEG C, standby aaerosol solution is made, wherein distilling
The volume ratio of water and ethylene glycol is 1：1~4；
(3) the standby aaerosol solution for obtaining step (2) is filtered, and filter cake is washed 3~5 times with distilled water and absolute ethyl alcohol,
Then dried at a temperature of 40~50 DEG C, that is, chlorine oxygen bismuth/modified montmorillonoid composite photo-catalyst is made.
The application of chlorine oxygen bismuth/modified montmorillonoid composite photo-catalyst of the present invention, for the organic matter in degradation water.
Organic matter of the present invention is phenol, o-nitrophenol or p-nitrophenol.
Compared with prior art, the invention has the advantages that：
1st, by compound with modified montmorillonoid, the specific surface area of catalyst is added, meanwhile, it has been self-assembly of bouquet
Shape structure, utilization ratio of the catalyst to luminous energy is enhanced, the combined efficiency of catalyst photo-generated carrier is reduced, improves and urge
Agent is to the adsorption capacity of organic pollution and its light-catalyzed reaction activity；
2nd, preparing raw material is cheap and easy to get, and preparation condition is gentle, and preparation process is simple, is not required to high-temperature roasting, reaction time
It is short；The preparation method is environmentally friendly simultaneously, does not produce poisonous and harmful accessory substance；
3rd, chlorine oxygen bismuth/modified montmorillonoid composite photo-catalyst has good photocatalytic degradation benzene under Single wavelength LED light
The reactivity of phenol, o-nitrophenol or p-nitrophenol, this utilizes significant to environmental improvement and green energy resource.
Brief description of the drawings
Fig. 1 is the XRD of chlorine oxygen bismuth/modified montmorillonoid composite photo-catalyst prepared by embodiment of the present invention 1.
Embodiment
Embodiment 1
4.85g bismuth nitrates and 0.74g potassium chloride are weighed respectively, are dispersed in 40mL ethylene glycol, under magnetic stirring
Form settled solution；Modified montmorillonoid is added into above-mentioned settled solution, and ultrasonic disperse 1h, forms bismuth nitrate-modified montmorillonoid
Suspension.20mL distilled water is added to above-mentioned gained bismuth nitrate-modification and covered with 1mL/min speed under the conditions of magnetic agitation and is taken off
In native suspension, continue to react 1.5h, reaction temperature is controlled at 20 DEG C, and aaerosol solution is made, aaerosol solution is filtered, and filter cake is used
Distilled water and absolute ethyl alcohol wash 3 times, are then dried at a temperature of 50 DEG C, that is, chlorine oxygen bismuth/modified montmorillonoid complex light is made and urges
Agent, the XRD spectrum of gained composite photo-catalyst are as shown in Figure 1.
Gained photochemical catalyst is used for oxidation processes phenol, o-nitrophenol or the p-nitrophenol aqueous solution.
Further to prove the degradation capability of the present embodiment catalyst Pyrogentisinic Acid, o-nitrophenol or p-nitrophenol, this
Invention has carried out following experiments：
Step (1)：10mg phenol, o-nitrophenol or p-nitrophenol solid accurately are weighed, is dissolved in distilled water,
And 1000mL is settled to, 10mgL-1 phenol, o-nitrophenol or p-nitrophenyl phenol solution is made；
Step (2)：Phenol, o-nitrophenol or p-nitrophenol that 100mL steps (1) obtain accurately are pipetted with pipette
Solution adds 0.1g chlorine oxygen bismuth/modified montmorillonoid composite photo-catalyst, temperature of reaction system control into solution into reactor
System first adsorbs 0.5h at 25 DEG C under half-light, reaches adsorption/desorption balance；
Step (3)：Using 360nm Single wavelengths LED as light source, step (2) resulting solution is subjected to light under light illumination and urged
Change degradation reaction, sampled at interval of 120min, and sieve phenol, o-nitrophenol or right are measured with UV-VIS spectrophotometry
The absorbance of nitrophenol solution simultaneously calculates its conversion ratio.
Embodiment 2
2.43g bismuth nitrates and 0.38g potassium chloride are weighed respectively, are dispersed in 20mL ethylene glycol, under magnetic stirring
Form settled solution；Modified montmorillonoid is added into above-mentioned settled solution, and ultrasonic disperse 0.5h, it is de- to form bismuth nitrate-modification illiteracy
Native suspension.10mL distilled water is added into above-mentioned gained bismuth nitrate-modification with 1mL/min speed under the conditions of magnetic agitation to cover
Take off in native suspension, continue to react 1h, reaction temperature is controlled at 25 DEG C, and aaerosol solution is made.Aaerosol solution is filtered, filter cake is used
Distilled water and absolute ethyl alcohol wash 5 times, are then dried at a temperature of 45 DEG C, that is, chlorine oxygen bismuth/modified montmorillonoid complex light is made and urges
Agent.
Gained photochemical catalyst is used for oxidation processes phenol, o-nitrophenol or the p-nitrophenol aqueous solution.
Further to prove the degradation capability of the present embodiment catalyst Pyrogentisinic Acid, o-nitrophenol or p-nitrophenol, this
Invention has carried out following experiments：
Step (1)：10mg phenol, o-nitrophenol or p-nitrophenol solid accurately are weighed, is dissolved in distilled water,
And 1000mL is settled to, 10mgL-1 phenol, o-nitrophenol or p-nitrophenyl phenol solution is made；
Step (2)：Phenol, o-nitrophenol or p-nitrophenol that 100mL steps (1) obtain accurately are pipetted with pipette
Solution adds 0.15g chlorine oxygen bismuth/modified montmorillonoid composite photo-catalyst, temperature of reaction system into solution into reactor
Control first adsorbs 1h at 20 DEG C under half-light, reaches adsorption/desorption balance；
Step (3)：Using 360nm Single wavelengths LED as light source, step (2) resulting solution is subjected to light under light illumination and urged
Change degradation reaction, sampled at interval of 120min, and phenol, o-nitrophenol are measured or to nitre with UV-VIS spectrophotometry
The absorbance of base phenol solution simultaneously calculates its conversion ratio.
Embodiment 3
4.85g bismuth nitrates and 0.74g potassium chloride are weighed respectively, are dispersed in 40mL ethylene glycol, under magnetic stirring
Form settled solution；Modified montmorillonoid is added into above-mentioned settled solution, and ultrasonic disperse 1h, forms bismuth nitrate-modified montmorillonoid
Suspension.20mL distilled water is added to above-mentioned gained bismuth nitrate-modification and covered with 1mL/min speed under the conditions of magnetic agitation and is taken off
In native suspension, continue to react 1.5h, reaction temperature is controlled at 25 DEG C, and aaerosol solution is made.Aaerosol solution is filtered, filter cake is used
Distilled water and absolute ethyl alcohol wash 4 times, are then dried at a temperature of 40 DEG C, that is, chlorine oxygen bismuth/modified montmorillonoid complex light is made and urges
Agent.
Gained photochemical catalyst is used for oxidation processes phenol, o-nitrophenol or the p-nitrophenol aqueous solution.
Further to prove the degradation capability of the present embodiment catalyst Pyrogentisinic Acid, o-nitrophenol or p-nitrophenol, this
Invention has carried out following experiments：
Step (1)：10mg phenol, o-nitrophenol or p-nitrophenol solid accurately are weighed, is dissolved in distilled water,
And 1000mL is settled to, 10mgL-1 phenol, o-nitrophenol or p-nitrophenyl phenol solution is made；
Step (2)：Phenol, o-nitrophenol or p-nitrophenol that 100mL steps (1) obtain accurately are pipetted with pipette
Solution adds 0.1g chlorine oxygen bismuth/modified montmorillonoid into phenol, o-nitrophenol or p-nitrophenyl phenol solution into reactor
Composite photo-catalyst, temperature of reaction system are controlled at 25 DEG C, and 1h is first adsorbed under half-light, reach adsorption/desorption balance；
Step (3)：Using 360nm Single wavelengths LED as light source, step (2) resulting solution is subjected to light under light illumination and urged
Change degradation reaction, sampled at interval of 240min, and phenol, o-nitrophenol are measured or to nitre with UV-VIS spectrophotometry
The absorbance of base phenol solution simultaneously calculates its conversion ratio.
Medicine and reagent used is that analysis is pure in embodiment of above.
The degradation rate of phenol, o-nitrophenol or p-nitrophenol is shown in Table 1 in each embodiment.
The chlorine oxygen bismuth of table 1/degraded situation of the modified montmorillonoid composite photo-catalyst under different embodiments：
Claims (4)
1. a kind of chlorine oxygen bismuth/modified montmorillonoid composite photo-catalyst, it is characterised in that be prepared by following steps：
(1) it is 1 in molar ratio by bismuth nitrate and potassium chloride：1~3 is placed in ethylene glycol, and the mol ratio of ethylene glycol and bismuth nitrate is 9
~15：1, reaction under magnetic stirring forms settled solution；Modified montmorillonoid is added into above-mentioned settled solution, modified montmorillonoid with
The mol ratio of bismuth nitrate is 1：25~80, and 0.5~1.5h of ultrasonic disperse, form bismuth nitrate-modified montmorillonoid suspension；
(2) distilled water is added to bismuth nitrate-modification obtained by step (1) and covered with 1mL/min speed under the conditions of magnetic agitation and taken off
In native suspension, continue 1~2h of reaction, reaction temperature is controlled at 20~25 DEG C, is made standby aaerosol solution, wherein distilled water with
The volume ratio of ethylene glycol is 1：1~4；
(3) the standby aaerosol solution obtained step (2) filters, and filter cake washs 3~5 times with distilled water and absolute ethyl alcohol, then
Dried at a temperature of 40~50 DEG C, that is, chlorine oxygen bismuth/modified montmorillonoid composite photo-catalyst is made.
A kind of 2. preparation method of chlorine oxygen bismuth/modified montmorillonoid composite photo-catalyst described in claim 1, it is characterised in that including
Following steps：
(1) it is 1 in molar ratio by bismuth nitrate and potassium chloride：1~3 is placed in ethylene glycol, and the mol ratio of ethylene glycol and bismuth nitrate is 9
~15：1, reaction under magnetic stirring forms settled solution；Modified montmorillonoid is added into above-mentioned settled solution, modified montmorillonoid with
The mol ratio of bismuth nitrate is 1：25~80, and 0.5~1.5h of ultrasonic disperse, form bismuth nitrate-modified montmorillonoid suspension；
(2) distilled water is added to bismuth nitrate-modification obtained by step (1) and covered with 1mL/min speed under the conditions of magnetic agitation and taken off
In native suspension, continue 1~2h of reaction, reaction temperature is controlled at 20~25 DEG C, is made standby aaerosol solution, wherein distilled water with
The volume ratio of ethylene glycol is 1：1~4；
(3) the standby aaerosol solution obtained step (2) filters, and filter cake washs 3~5 times with distilled water and absolute ethyl alcohol, then
Dried at a temperature of 40~50 DEG C, that is, chlorine oxygen bismuth/modified montmorillonoid composite photo-catalyst is made.
3. a kind of application of chlorine oxygen bismuth/modified montmorillonoid composite photo-catalyst described in claim 1, it is characterised in that for degrading
Organic matter in water.
A kind of 4. application of chlorine oxygen bismuth/modified montmorillonoid composite photo-catalyst according to claim 3, it is characterised in that institute
The organic matter stated is phenol, o-nitrophenol or p-nitrophenol.
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