CN108686656A - A kind of α-Fe2O3/ gangue composite photo-catalyst and its preparation method and application - Google Patents

A kind of α-Fe2O3/ gangue composite photo-catalyst and its preparation method and application Download PDF

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CN108686656A
CN108686656A CN201810403670.6A CN201810403670A CN108686656A CN 108686656 A CN108686656 A CN 108686656A CN 201810403670 A CN201810403670 A CN 201810403670A CN 108686656 A CN108686656 A CN 108686656A
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gangue
catalyst
molysite
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aqueous solution
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CN108686656B (en
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谢娟
许永权
杜红霞
张国刚
赵树春
曹亚鹏
康文通
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Hebei University of Science and Technology
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
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    • 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
    • B01J23/00Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/70Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
    • B01J23/74Iron group metals
    • B01J23/745Iron
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J29/00Catalysts comprising molecular sieves
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
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    • B01J35/60Catalysts, in general, characterised by their form or physical properties characterised by their surface properties or porosity
    • B01J35/61Surface area
    • 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
    • C02F1/32Treatment of water, waste water, or sewage by irradiation with ultraviolet light
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00Nature of the contaminant
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    • C02F2101/36Organic compounds containing halogen
    • 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 α-Fe2O3/ gangue composite photo-catalyst comprising the following raw material is prepared through boiling reflux:The aqueous solution of pretreated gangue and molysite;The aqueous solution of the molysite is with α-Fe2O3The mass ratio of quality meter and pretreated gangue is 0.5 ~ 5:100.The invention further relates to the method and its application for preparing above-mentioned composite photo-catalyst.The present invention product can under ultraviolet irradiation condition effective degrading chlorophenol class compound.The preparation method of the present invention has the characteristics that raw material is few, simple for process, the reaction time is short, condition is relatively mild, environmentally safe, is a kind of green synthesis process, industrialization easy to implement.

Description

A kind of α-Fe2O3/ gangue composite photo-catalyst and its preparation method and application
Technical field
The invention belongs to photochemical catalyst preparation fields, and in particular to a kind of α-Fe2O3/ gangue composite photo-catalyst, its system Preparation Method and its application in degrading chlorophenol class compound.
Background technology
It is at normal temperatures and pressures inorganic molecules by organic pollutant degradation that photocatalysis technology, which can directly utilize luminous energy, and And have the characteristics that low energy consumption, easy to operate, reaction condition is mild, secondary pollution is small, it is a kind of ideal environmental pollution improvement Technology.Be becoming tight fossil energy day, today of environmental pollution getting worse, the importance of photocatalysis technology is self-evident, Core is exactly to research and develop the photochemical catalyst of function admirable.
Common catalysis material is mainly TiO2,SnO2,CdS,WO3,ZrO2And Fe2O3Deng some n-type semiconductor chemical combination Object.α-Fe2O3Not only energy gap is relatively narrow, and light abstraction width extends to visible region, can be good at utilizing sunlight, and And with the nontoxic good characteristics such as inexpensive of high chemical stability, resistance to acid and alkali, fast light burn into, only photocatalysis efficiency needs to be carried It is high.
Because the activity of photochemical catalyst is in close relations with its granule size, granularity is smaller, and specific surface area is bigger, and photocatalysis is lived Property is higher, so semiconductor light-catalyst is micro-/ nano particle mostly.But during photocatalysis degradation organic contaminant, micro-/ Nano particle also can cause secondary agglomeration because of undersized, and deposit and be difficult to recycle after use, easily form the disadvantage of secondary pollution. This, which has become, restricts the big technical bottleneck that micro-/ nano semiconductor light-catalyst promotes and applies.
As a kind of effective ways to solve the above problems, micro-/ nano semiconductor light-catalyst it is immobilized in recent years by Domestic and foreign scholars have been arrived more and more to pay close attention to.Currently, common solid support method is generally divided into, film forming is immobilized and carrier is solid Two kinds of loadization, the latter's multiselect use activated carbon, carbon nanotube etc. with flourishing pore structure and large specific surface area to do carrier.By More expensive in their prices, process of industrialization is very slow.
Gangue is grey black rock lower than coal with a kind of phosphorus content of coal seam association, symbiosis in coal forming process. The solid waste discharged in this coal mining, washing and process accounts for about the 15% ~ 20% of coal production.It is a large amount of not sharp Gangue is arbitrarily accumulated, not only land occupation, but also pollution environment.Carrying out the comprehensive utilization of gangue in a deep going way has become China The fundamental way of coal industry in-depth transition and sustainable development.Natural gangue complicated component, compact structure, but it is modified Afterwards, the inorganic mineral in gangue is partially converted into amorphous state by crystalline state, and structure becomes loose, specific surface area increases, hole Gap structure is flourishing, and absorption property significantly improves.
So far there is not yet related α-Fe2O3The report of/gangue composite photo-catalyst.If being that absorption carries with modified gangue Body loads micro-/ nano α-Fe2O3Particle forms α-Fe2O3/ gangue composite photo-catalyst, can not only gangue become give up into Treasured realizes efficiently using for resource, also will be helpful to improve micro-/ nano α-Fe2O3Photocatalysis efficiency.Therefore, a kind of work is found Skill is simple, the at low cost, α-Fe of energy consumption less, environmentally protective2O3/ gangue composite photo-catalyst preparation method has important show Sincere justice.
Invention content
The object of the present invention is to provide a kind of α-Fe2O3/ gangue composite photo-catalyst and preparation method thereof.The preparation side Method has the characteristics that raw material is few, simple for process, the reaction time is short, condition is relatively mild, environmentally safe, is a kind of green conjunction At technique, industrialization easy to implement.Prepared product can under ultraviolet irradiation condition effective degrading chlorophenol class compound.
The present invention adopts the following technical scheme that:
A kind of α-Fe2O3/ gangue composite photo-catalyst comprising the following raw material is prepared through boiling reflux:Pretreated coal The aqueous solution of spoil and molysite;The aqueous solution of the molysite is with α-Fe2O3Quality meter and the mass ratio of pretreated gangue are 0.5~5:100。
The aqueous solution parameter of the molysite is calculated by following formula:
m α-Fe2O3= C The aqueous solution of molysite×V The aqueous solution of molysite×M α-Fe2O3
In formula,C- molar concentration, mol/L;V- volume, L;M- molal weight, g/mol;m- quality, g.
Further, the pretreated gangue be gangue through crush, ground 150 ~ 300 mesh sieve after, in 700 It is spare after ~ 900 DEG C of 1.5 ~ 3 h of calcining.
Preferably, the pretreated gangue is forged for gangue through crushing, after ground 200 mesh sieve in 800 DEG C It burns spare after 2 h.
Further, the molysite includes ferric nitrate, iron chloride or ferric sulfate.
Further, Fe in the aqueous solution of the molysite3+A concentration of 0.4 mol/L of ion.
A kind of above-mentioned α-Fe2O3The preparation method of/gangue composite photo-catalyst comprising following steps:
(1)Gangue is taken, 150 ~ 300 mesh sieve is crossed after crushing, grinding, 1.5 ~ 3 h is calcined in 700 ~ 900 DEG C, is pre-processed Gangue afterwards;
(2)Prepare Fe3+Ion concentration is the aqueous solution of the molysite of 0.4 mol/L;
(3)Take step(2)5 mL of aqueous solution of prepared molysite is added distilled water and is settled to 100 mL, then adds into solution Enter step(1)Obtained pretreated gangue, 1 h of magnetic agitation;
The aqueous solution of the molysite is with α-Fe2O3Quality meter, α-Fe2O3Mass ratio with pretreated gangue is 0.5 ~ 5: 100;
(4)Regulating step(3)3 h of boiling reflux after the pH to 9 ~ 11 of obtained reaction system;
(5)Through filtering, water washing and after natural drying is distilled, α-Fe are obtained2O3/ gangue composite photo-catalyst.
Wherein, the step(1)In, gangue crosses 200 mesh sieve after crushing, grinding, and calcination temperature is 800 DEG C, calcining Time is 2 h.
Wherein, the step(2)In, the molysite is ferric nitrate, iron chloride or ferric sulfate.
Wherein, the step(3)In, the α-Fe2O3Mass ratio with pretreated gangue is 1 ~ 4:100, preferably It is 3:100.
Wherein, the step(4)In, the pH value of the reaction system is 10.
Wherein, the step(4)In, adjust reaction system using the sodium hydrate aqueous solution of 6 mol/L and 0.1 mol/L PH value.
A kind of above-mentioned α-Fe2O3Application of/gangue the composite photo-catalyst in degrading chlorophenol class compound.
The beneficial effects of the present invention are:Natural gangue granularity is larger, quality is hard, compact structure, it is difficult to directly answer With.Usually first it is crushed, be ground up, sieved and calcination processing.It crushes, grinding makes the grain size of natural gangue become rapidly Small, lattice is distorted, and specific surface area accordingly becomes larger, but the structure of coal gangue particle still densification at this time, and adsorptivity is still very Difference does not show activity substantially when being chemically reacted.After high-temperature calcination processing, gangue not only has certain ingredient to volatilize, and one A little inorganic compounds also occur that crystalline state changes, and then the short texture degree of gangue and chemism is made to greatly improve.Although Above-mentioned processing can be played the role of improving gangue performance, but this for gangue is used as adsorbent, effect is remote It is not nearly enough.Gangue after calcining will be further processed with substances such as acid or alkali again.
Acid solution can dissolve the oxide of Al, Fe, Ca in gangue, increase the porosity of coal gangue particle, to enhance The adsorption capacity of gangue.Aqueous slkali can not only then dissolve some metal oxides in gangue, increase coal gangue particle Porosity, suitable alkali can also react with the oxide of Si in gangue and Al, generate the boiling with preferable adsorption capacity Stone molecular sieve.
It is well known that photochemical catalyst absorption is degraded, the ability of object is to influence a key factor of its photocatalysis efficiency. Modified gangue large specific surface area, more micropores have good adsorptivity, are not only advantageous to chemically load α-Fe2O3Light Catalyst, the α-Fe of formation2O3/ gangue composite photo-catalyst can also realize α-Fe2O3, both gangues synergistic effect, So that catalyst surface is remained higher pollutant concentration, promotes α-Fe2O3With the electronics transfer between the object molecule that is degraded, Improve α-Fe2O3Photocatalysis efficiency.
Our early-stage study is found, using molysite and alkali as reactant, using boiling reflux, under the conditions of 9 ~ 11 pH It can obtain the good micro-/ nano α-Fe of photocatalysis performance2O3Particle, this discovery make a step prepare α-Fe2O3/ gangue Compound is possibly realized.The alkali being present in reaction system can be modified gangue and be adsorbed with modified gangue Fe3+Ion reacts to obtain α-Fe2O3, thus by α-Fe2O3It is supported on modified gangue.Raw material needed for this method is few, It is simple for process, the reaction time is short, condition is relatively mild, environmentally safe, be a kind of green synthesis process.
Description of the drawings
Fig. 1 is modified gangue, pure α-Fe2O3And α-Fe2O3The XRD spectra of/gangue compound.
In Fig. 1, a is modified gangue, and b is pure α-Fe2O3, c is α-Fe2O3/ gangue compound.
Fig. 2 is pure α-Fe2O3And different quality ratio α-Fe2O3/ gangue compound photocatalytic degradation pentachlorophenol efficiency is at any time Between the curve that changes.
Specific implementation mode
In order to deepen the understanding of the present invention, the present invention is described in detail below with reference to the accompanying drawings and embodiments, should Embodiment is exemplary, and is only used for explaining the present invention, is not constituted and is limited to protection domain.
Embodiment 1
The gangue of Shanxi riding comfort model is derived from after crushing and being fully ground, crosses 200 mesh sieve, and it is spare to calcine 2 h in 700 DEG C. Meanwhile preparing Fe3+Ion concentration is the molysite aqueous solution of 0.4 mol/L, and the sodium hydroxide of 6 mol/L and 0.1 mol/L are water-soluble Liquid is spare.
By 5 mL iron nitrate aqueous solutions(Fe3+Ion concentration is 0.4 mol/L)It is introduced into three-necked flask, with distilled water constant volume 100 mL, are added the pretreated bastard coal mountain flour of calculation amount, after 1 h of magnetic agitation, be slowly added dropwise into bottle 6 mol/L and The sodium hydrate aqueous solution of 0.1 mol/L, the pH value that the addition by controlling sodium hydrate aqueous solution adjusts reaction system are 9,3 h of boiling reflux.Through filtering, distilling water washing, naturally dry, α-Fe are obtained2O3/ gangue composite photo-catalyst.
Embodiment 2 ~ 6 and comparative example 1 ~ 2
Embodiment 2 ~ 6 and comparative example 1 ~ 2 are identical as the operating procedure of embodiment 1, differ only in type, the bastard coal of molysite used Stone calcination temperature, gangue dosage and pH value of reaction system, it is specific as shown in table 1.
1 embodiment 2 ~ 6 of table and comparative example 1 ~ 2
1 XRD characterization of effect example
Fig. 1 is modified gangue, pure α-Fe2O3And α-Fe2O3The XRD spectra of/gangue compound.Occur 2 simultaneously in Fig. 1 cθThe diffraction maximum of modified gangue at=21.18 °, 26.64 °(Fig. 1 a)With 2θ=24.08 °, 33.19 °, 35.67 °, 40.84 °, hexagonal structure α-Fe at 49.47 °, 53.97 °, 57.46 °, 62.39 °, 63.96 °2O3(JCPDS 33-0664)Diffraction Peak(Fig. 1 b), it was demonstrated that product is really α-Fe2O3/ gangue compound.Because of α-Fe2O3It is covered on the surface of modified gangue, So α-Fe2O3Belong to α-Fe in/gangue compound2O3The purer α-Fe of each diffraction peak intensity2O3Variation is little, and belongs to and change The diffraction peak intensity of property gangue more unsupported α-Fe2O3It significantly reduces before.
2 α-Fe of effect example2O3The photocatalysis performance of/gangue compound is evaluated
Chlorophenols compound is a kind of typical " three causes(Carcinogenic, teratogenesis, mutagenesis)" organic pollution, it is widely used in giving birth to Produce preservative, dyestuff, herbicide and agrochemical.Meanwhile during incineration of waste, association with pulp bleaching, Creation During Chlorination in Domestic Water It is possible that generating chlorophenols by-product.Common chlorophenols compound has 2,4- Dichlorophenols, 2,4,6- trichlorophenols, 2,3,4,6- tetra- Chlorophenol and pentachlorophenol etc..This kind of a large amount of of organic compound use, are insufficient and adjoint to the understanding of its toxicity and harm in early days And come long-standing neglect, result in its continuous accumulation in the environment, to water environment and human health cause directly destroy and Potential threat.However, conventional method for treating water and biotechnology is difficult effective degrading chlorophenol class compound.In recent years, with light Catalysis is that the high-level oxidation technology of representative is quickly grown in terms of pollutant environmental improvement, is applied to degrading chlorophenol class compound Research also achieve notable achievement.
Photocatalysis performance evaluation experimental is the results show that made α-Fe2O3/ gangue compound is to above-mentioned chlorophenols compound There is preferable degradation effect.The photocatalysis performance evaluation experimental step and data carried out using pentachlorophenol as target degradation product is as follows:
100 mL pentachlorophenol solutions are added in beaker(10 mg/L, pH 9 ~ 10)With 0.1 g α-Fe2O3/ gangue compound Powder is protected from light 30 min of strong stirring, and pentachlorophenol is made to reach adsorption-desorption balance in catalyst surface.Then in magnetic agitation Under, using 125 W high voltage mercury lamp radiations(Lamp and 10 cm of liquid level distance)And start timing.Interval sampling, centrifuges, takes Clear liquid measures it in pentachlorophenol maximum absorption wavelength through filtering with microporous membrane, with ultraviolet-visible spectrophotometer(λ max = 220 nm)The absorbance at place, and according to the degradation rate of following formula calculating pentachlorophenol(η):
η=(A 0A t)/A 0×100%
In formula,A 0For the absorbance of pentachlorophenol solution before illumination;A tFor the absorbance of pentachlorophenol solution after light application time t.
Fig. 2 is pure α-Fe2O3And different quality ratio α-Fe2O3/ gangue compound photocatalytic degradation pentachlorophenol efficiency is at any time Between the curve that changes.Blank assay shows, when ultraviolet light, pentachloro- Phenol degradation rate is only 46.92% after 180 min, the phenomenon For the selfdecomposition of pentachlorophenol.While ultraviolet light, pure α-Fe are put into2O3Or α-Fe2O3/ gangue composite photo-catalyst, phase With in light application time, the degradation rate of pentachlorophenol significantly improves.It has been observed that all α-Fe2O3The photocatalysis of/gangue compound Activity is above pure α-Fe2O3, this confirms α-Fe2O3α-Fe in/gangue compound2O3It is implicitly present in and cooperates between gangue Effect.However, α-Fe2O3It is not the bigger the better with the mass ratio of gangue, mass ratio 3:100 α-Fe2O3/ gangue is multiple It closes object and shows highest photocatalytic activity, pentachloro- Phenol degradation rate is close to 90% in 180 min.
Embodiment described above is only that the preferred embodiment of the present invention is described, and but it is not limited to this, this The technical staff in field is easy to understand the spirit of the present invention according to above-described embodiment, and makes different amplification and variation, but Without departing from the spirit of the present invention, all within protection scope of the present invention.

Claims (10)

1. a kind of α-Fe2O3/ gangue composite photo-catalyst, which is characterized in that it includes that the following raw material is prepared through boiling reflux: The aqueous solution of molysite and pretreated gangue;The aqueous solution of the molysite is with α-Fe2O3Quality meter and pretreated bastard coal The mass ratio of stone is 0.5 ~ 5:100.
2. α-Fe according to claim 12O3/ gangue composite photo-catalyst, which is characterized in that described pretreated Gangue be gangue through crush, ground 150 ~ 300 mesh sieve after, in 700 ~ 900 DEG C calcine 1.5 ~ 3 h after it is spare.
3. α-Fe according to claim 12O3/ gangue composite photo-catalyst, which is characterized in that the molysite includes nitre Sour iron, iron chloride or ferric sulfate.
4. α-Fe according to claim 12O3/ gangue composite photo-catalyst, which is characterized in that the molysite it is water-soluble Fe in liquid3+A concentration of 0.4 mol/L of ion.
5. a kind of claim 1 ~ 4 any one of them α-Fe2O3The preparation method of/gangue composite photo-catalyst, feature exist In comprising following steps:
(1)Gangue is taken, 150 ~ 300 mesh sieve is crossed after crushing, grinding, 1.5 ~ 3 h is calcined in 700 ~ 900 DEG C, is pre-processed Gangue afterwards;
(2)Prepare Fe3+Ion concentration is the aqueous solution of the molysite of 0.4 mol/L;
(3)Take step(2)5 mL of aqueous solution of prepared molysite is added distilled water and is settled to 100 mL, then adds into solution Enter step(1)Obtained pretreated gangue, 1 h of magnetic agitation;
The aqueous solution of the molysite is with α-Fe2O3Quality meter, α-Fe2O3Mass ratio with pretreated gangue is 0.5 ~ 5: 100;
(4)Regulating step(3)3 h of boiling reflux after the pH to 9 ~ 11 of obtained reaction system;
(5)Through filtering, water washing and after natural drying is distilled, α-Fe are obtained2O3/ gangue composite photo-catalyst.
6. preparation method according to claim 5, which is characterized in that the step(1)In, gangue is through crushing, grinding 200 mesh sieve is crossed afterwards, and calcination temperature is 800 DEG C, and calcination time is 2 h.
7. preparation method according to claim 5, which is characterized in that the step(2)In, the molysite be ferric nitrate, Iron chloride or ferric sulfate.
8. preparation method according to claim 5, which is characterized in that the step(3)In, the α-Fe2O3With pretreatment The mass ratio of gangue afterwards is 1 ~ 4:100, preferably 3:100.
9. preparation method according to claim 5, which is characterized in that the step(4)In, the pH value of the reaction system It is 10.
10. a kind of α-Fe as described in claim 1 ~ 42O3/ gangue composite photo-catalyst is in degrading chlorophenol class compound Using.
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CN115414964A (en) * 2022-08-26 2022-12-02 陕西科技大学 Polymer modified coal gangue composite Ag-series photocatalyst and preparation method thereof
CN115414964B (en) * 2022-08-26 2024-03-22 陕西科技大学 Polymer modified gangue composite Ag-based photocatalyst and preparation method thereof
CN115477948A (en) * 2022-09-22 2022-12-16 昆明理工大学 Method for preparing FeOOH modified coal gangue by utilizing red mud
CN116139921A (en) * 2023-04-24 2023-05-23 太原理工大学 Preparation method and application of tail coal-based zeolite@CDs-TiO 2 composite photocatalyst

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