CN109894073A - A kind of BiOBr/SiO2Composite aerogel catalysis material and its preparation method and application - Google Patents
A kind of BiOBr/SiO2Composite aerogel catalysis material and its preparation method and application Download PDFInfo
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- CN109894073A CN109894073A CN201811356598.2A CN201811356598A CN109894073A CN 109894073 A CN109894073 A CN 109894073A CN 201811356598 A CN201811356598 A CN 201811356598A CN 109894073 A CN109894073 A CN 109894073A
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Abstract
The present invention relates to a kind of BiOBr/SiO2Composite aerogel catalysis material, the material are prepared using soda acid two-step method.Firstly, bismuth source and bromine source are dissolved separately in preparation SiO2Solvent needed for composite aerogel (dehydrated alcohol or ethylene glycol) He Shuizhong.Secondly, being 4:2:1 according to the volume ratio of dehydrated alcohol or ethylene glycol, ethyl orthosilicate and water, BiOBr/SiO is synthetically prepared using soda acid two-step method2Composite aerogel.This method simple process, prepared BiOBr/SiO2Composite aerogel had not only had high visible light catalytic activity specific to BiOBr, but also the advantages that have both high-specific surface area possessed by aerosil, high adsorption.It is expected to be applied to organic sewage process field as catalysis material.
Description
Technical field
The present invention relates to physical absorptions and chemical catalyst technical field, and in particular to a kind of BiOBr/SiO2Compound airsetting
Glue catalysis material and preparation method thereof.
Background technique
It is also increasingly tight along with the environmental pollution of generation with the development of society and the continuous improvement of living standards of the people
Weight.The organic pollutant category and content detected in water environment is increasing, and wherein most is persistent organic pollutants.
The long-term accumulation in water of a large amount of organic matter, eventually enters into biological chain, generates huge threat to the health of the mankind.Therefore it opens
The sewage disposal technology of green-emitting environmental protection becomes particularly important.In numerous sewage treatment process, photocatalysis technology is due to it
With efficient, non-selectivity, stability is high, green non-poisonous, without secondary pollution, low energy consumption, easy to operate and inexpensive etc. prominent
Advantage, it is considered to be most effective one of the energy saving means for solving problem of environmental pollution.
Research finds BiOX (X=Cl, Br, I) type photochemical catalyst under visible light illumination, and it is living to show stronger photocatalysis
Property, BiOX type semiconductor can be applied to the catalytic degradation of organic pollutant.Especially BiOBr catalyst has Br layers double
What alternate crystallization was formed contains [Bi2O2]2+The layer structure of component.It is wide that this special structure makes it have suitable forbidden band
Degree, stable photocatalysis performance inspire stronger photocatalytic activity under the conditions of visible light-inducing.
SiO2Aeroge, English abbreviation SiO2(AG), the unique three-dimensional network pore structure having, shows translucency
The good feature of good, porosity height, large specific surface area, absorption property, is commonly used for catalyst carrier, to improve the adsorptivity of catalyst
Energy.
Aiming at the problem that especially BiOBr limited sorption capacity present in photocatalysis technology application field, from raising
From the point of view of catalyst is to object adsorptivity and selectivity, development and design BiOBr and SiO2Composite material, can be abundant
Photocatalysis and SiO using BiOBr2Organic pollutant in the thorough environment purification of the absorption property of aeroge.The present invention
Theoretical research to photocatalysis technology and its there is certain directive significance and ginseng in the practical application of field of environment pollution control
Examine value.
Summary of the invention
The first purpose of this invention is to overcome the deficiencies of the prior art and provide a kind of BiOBr/SiO2Composite aerogel
Catalysis material.Make full use of the high visible light catalytic activity and SiO of BiOBr2The high absorption property of aeroge thoroughly purifies ring
Organic pollutant in border.So that BiOBr low absorbability problem present in photocatalysis technology application field is effectively solved
Certainly.
Second object of the present invention is to provide BiOBr/SiO2The preparation method of composite aerogel catalysis material, should
Simple process, at low cost, low energy consumption.
In order to realize that above-mentioned purpose of the invention, technical solution of the present invention are specific as follows:
(1), by a certain amount of bismuth source ultrasonic dissolution in solvent；It is mixed after to be dissolved with a certain amount of ethyl orthosilicate, in magnetic
Some time is stirred in power blender；
(2), a certain amount of bromine source is weighed to be dissolved in the water；
(3), the solution of step (2) is slowly dropped in step 1), magnetic agitation for a period of time after, a certain concentration is slowly added dropwise
Hydrochloric acid regulation system pH and continue magnetic agitation certain time；
(4), heating water bath for a period of time after, natural cooling.Under magnetic stirring, with certain density ammonia water conditioning system pH,
Rotor is taken out when solution becomes sticky, it is static to make its gel.
(5), dehydrated alcohol aging is added after gel, then carries out solvent displacement a period of time with n-hexane.Then trimethyl
It is modified that the mixed solution of chlorosilane, n-hexane and dehydrated alcohol carries out surface.After the completion of modified using room temperature gradient seasoning into
Row drying obtains sample after the completion of dry.
(6), the hydrophilic treated of sample.Sample in step (5) is placed in Muffle furnace, is calcined at a certain temperature.
In the step (1), the bismuth source is Bi (NO3)3·5H2O and Bi2O3One of；The solvent is anhydrous second
Alcohol or ethylene glycol；Behind bismuth source and ethyl orthosilicate mixing, the magnetic agitation time is 30~60 min；
In the step (2), bromine source is one of KBr, NaBr or CTAB (cetyl trimethylammonium bromide)；
In the step (3), the magnetic agitation time is 10~30 min；The concentration of hydrochloric acid is 0.1~0.5 mol/L；Salt used
PH=2~4 of sour regulation system；System pH continues the magnetic agitation time as 10~30 min after stablizing；
In the step (4), the heating water bath time is 3~6 h；Use the adjusting body for the ammonium hydroxide that concentration is 0.1~0.5 mol/L
It is pH=8~10；
In the step (5), use dehydrated alcohol ageing time for 10~24 h；Use n-hexane carry out solvent time swap for
24~36 h；The molar ratio of trim,ethylchlorosilane, n-hexane and dehydrated alcohol is (0.5~1): (0.5~1): 1, modification time
For 10~24 h；The dosage of the dehydrated alcohol, n-hexane and trim,ethylchlorosilane, n-hexane and dehydrated alcohol mixed solvent
For 20~30 mL；Room temperature gradient seasoning is respectively to take 3 time points within the scope of 50~120 DEG C, be separately dried 20~30 min；
In the step (6), calcination temperature is 300~450 DEG C, and soaking time is 30~60 min；
In the step (1) and step (2), the volume ratio of dehydrated alcohol or ethylene glycol, ethyl orthosilicate and water is 4:2:1.
BiOBr/SiO as described above2Composite aerogel catalysis material in terms of as photochemical catalyst in application.
BiOBr/SiO as described above2Composite aerogel catalysis material in organic wastewater in terms of processing in application.
The advantages of present invention obtains and good effect are as follows:
1, using simple soda acid two-step method, bismuth source and bromine source are directly dissolved separately in preparation SiO2Needed for composite aerogel
Solvent (dehydrated alcohol or ethylene glycol) He Shuizhong, simplifies production procedure；
2, using air drying method, sample obtained is dried.Compared to other drying means (supercritical dryings, freezing
It is dry etc.), have many advantages, such as low energy consumption, low risk, low cost；
3, there is high adsorption to organic pollutants such as RhB, adsorption efficiency can reach 65% or more；In simulated visible light condition
Under, photocatalytic degradation efficiency can reach 100% in 30 min；
4, circulation degradation experiment shows that sample obtained has excellent Repeatability, has in practical applications centainly
Potentiality；
5, using BiOBr as composite object, BiOBr/SiO is prepared2Catalytic composite material compensates for the adsorptivity of BiOBr not
The disadvantage of foot enhances the degradation capability to organic pollutant.
6, the present invention prepares BiOBr/SiO using using simple soda acid two-step method2Composite aerogel catalysis material.It is first
First, bismuth source and bromine source are dissolved separately in preparation SiO2Solvent needed for composite aerogel (dehydrated alcohol or ethylene glycol) and water
In.Secondly, being 4:2:1 according to the volume ratio of dehydrated alcohol or ethylene glycol, ethyl orthosilicate and water, synthesized using soda acid two-step method
Prepare BiOBr/SiO2Composite aerogel.This method simple process, prepared BiOBr/SiO2Composite aerogel both had
High visible light catalytic activity specific to BiOBr, and have both high-specific surface area, high adsorption possessed by aerosil
The advantages that.It is expected to be applied to organic sewage process field as catalysis material.
7, preparation method of the invention is simple, low in cost, is suitble to industrialized production；Prepared composite photocatalyst material
Visible light photocatalysis active with higher has wide application in terms for the treatment of of Organic Wastewater.
Detailed description of the invention
Fig. 1 is 1 gained BiOBr/SiO of embodiment2The XRD diagram of catalytic composite material；
Fig. 2 is 1 gained BiOBr/SiO of embodiment2The FT-IR of catalytic composite material schemes；
Fig. 3 is 1 gained BiOBr/SiO of embodiment2The nitrogen adsorption of catalytic composite material-desorption isothermal curve；
Fig. 4 is BiOBr/SiO2Absorption degradation figure of the composite catalyst to 30 mg/L rhodamine Bs.
Specific embodiment
The embodiment of the present invention is described in detail below, it should be noted that the present embodiment is narrative, is not limited
, this does not limit the scope of protection of the present invention.
Raw material used in the present invention is unless otherwise specified conventional commercial product；Used in the present invention
Method is unless otherwise specified the conventional method of this field.
Embodiment 1
Following embodiment will the present invention is further illustrated in conjunction with attached drawing.
(1), by the Bi (NO of 3 mol3)3·5H2O ultrasonic dissolution is in 10 mL ethylene glycol；After to be dissolved just with 20 mL
Silester mixing, stirs 30 min in magnetic stirring apparatus；
(2), 3 mol KBr are weighed to be dissolved in 5 mL water；
(3), the solution of step (2) is slowly dropped in step 1), after 30 min of magnetic agitation, 0.1 mol/L is slowly added dropwise
Simultaneously continue 20 min of magnetic agitation in hydrochloric acid regulation system pH=4；
(4), after 4 h of heating water bath, natural cooling.Under magnetic stirring, with ammonia water conditioning system pH=8 of 0.1 mol/L, to
Rotor is taken out when solution becomes sticky, it is static to make its gel.
(5), 20 mL dehydrated alcohol aging, 15 h is added after gel, then carries out solvent with 20 mL n-hexanes and replaces 15 h.
Then the mixed solution of 30 mL trim,ethylchlorosilanes, n-hexane and dehydrated alcohol carries out surface modified 24.After the completion of modified respectively
Dry 30 min at 60 DEG C, 80 DEG C, 100 DEG C and 120 DEG C, obtain sample after the completion of dry.
(6), the hydrophilic treated of sample.Sample in step 5) is placed in Muffle furnace, calcines 30 under the conditions of 350 DEG C
min。
Embodiment 2
Following embodiment will the present invention is further illustrated in conjunction with attached drawing.
(1), by the Bi (NO of 5 mol3)3·5H2O ultrasonic dissolution is in 10 mL ethylene glycol；After to be dissolved just with 20 mL
Silester mixing, stirs 30 min in magnetic stirring apparatus；
(2), 5 mol KBr are weighed to be dissolved in 5 mL water；
(3), the solution of step 2) is slowly dropped in step 1), after 30 min of magnetic agitation, 0.1 mol/L salt is slowly added dropwise
Simultaneously continue 20 min of magnetic agitation in sour regulation system pH=4；
(4), after 4 h of heating water bath, natural cooling.Under magnetic stirring, with ammonia water conditioning system pH=8 of 0.1 mol/L, to
Rotor is taken out when solution becomes sticky, it is static to make its gel.
(5), 20 mL dehydrated alcohol aging, 15 h is added after gel, then carries out solvent with 20 mL n-hexanes and replaces 15 h.
Then the mixed solution of 30 mL trim,ethylchlorosilanes, n-hexane and dehydrated alcohol carries out surface modified 24.After the completion of modified respectively
Dry 30 min at 60 DEG C, 80 DEG C, 100 DEG C and 120 DEG C, obtain sample after the completion of dry.
(6), the hydrophilic treated of sample.Sample in step 5) is placed in Muffle furnace, calcines 30 under the conditions of 350 DEG C
min。
Embodiment 3
Following embodiment will the present invention is further illustrated in conjunction with attached drawing.
(1), by the Bi (NO of 1 mol3)3·5H2O ultrasonic dissolution is in 10 mL ethylene glycol；After to be dissolved just with 20 mL
Silester mixing, stirs 30 min in magnetic stirring apparatus；
(2), 1 mol KBr is weighed to be dissolved in 5 mL water；
(3), the solution of step (2) is slowly dropped in step 1), after 30 min of magnetic agitation, 0.1 mol/L is slowly added dropwise
Simultaneously continue 20 min of magnetic agitation in hydrochloric acid regulation system pH=4；
(4), after 4 h of heating water bath, natural cooling.Under magnetic stirring, with ammonia water conditioning system pH=8 of 0.1 mol/L, to
Rotor is taken out when solution becomes sticky, it is static to make its gel.
(5), 20 mL dehydrated alcohol aging, 15 h is added after gel, then carries out solvent with 20 mL n-hexanes and replaces 15 h.
Then the mixed solution of 30 mL trim,ethylchlorosilanes, n-hexane and dehydrated alcohol carries out surface modified 24.After the completion of modified respectively
Dry 30 min at 60 DEG C, 80 DEG C, 100 DEG C and 120 DEG C, obtain sample after the completion of dry.
(6), the hydrophilic treated of sample.Sample in step 5) is placed in Muffle furnace, calcines 30 under the conditions of 350 DEG C
min。
Coherent detection of the invention:
XRD test is carried out to the sample obtained of example 1, result is as shown in Figure 1.The diffraction peak intensity of sample is high and clear,
Without mixed and disorderly peak, there is good crystallinity.The diffraction maximum of sample and standard four directions BiOBr structure (JCPDS No.09-0393) and
SiO2Phase (JCPDS No.39-1425) is well matched with.
FT-IR test is carried out to the sample obtained of example 1, result is as shown in Figure 2.Infrared spectroscopy is commonly used to determine
The chemical bonding state of material.In 1091.5 cm-1The strong and wide Si-O vibrating mode at place represents SiO2Network structure
Si-O-Si link.796.6 cm-1With 1384.6 cm-1The place peak Si-C confirmed Si-CH3The presence of functional group.3433 cm-1Place
The peak of appearance is the stretching vibration of Si-OH.466.8 cm-1The peak at place is the stretching vibration of Bi-O.
Specific area measuring is carried out to present invention material sample obtained.Its nitrogen adsorption-desorption isothermal curve such as Fig. 3
It is shown.By calculating, it is 280 m that the specific surface area of sample, which reaches,2g -1.Biggish specific surface area would generally its Surface absorption more
More active materials and reactant provides more active sites for photochemical catalyst.
Photocatalytic degradation experiment is carried out to present invention material sample obtained, result is as shown in Figure 4.As figure shows,
Obtained sample can reach 65% to the adsorption efficiency of rhodamine B (30 mg/L) in 60 min；Corresponding photocatalysis drop
It solves efficiency and reaches 100% in 30 min or so.
Although disclosing the embodiment of the present invention for the purpose of illustration, it will be appreciated by those skilled in the art that: not
Be detached from the present invention and spirit and scope of the appended claims in, various substitutions, changes and modifications be all it is possible, therefore, this
The range of invention is not limited to the embodiment and attached drawing disclosure of that.
Claims (9)
1. a kind of BiOBr/SiO2Composite aerogel catalysis material, it is characterised in that: the high visible of BiOBr is made full use of to urge
Change activity and SiO2Organic pollutant in the thorough environment purification of the high absorption property of aeroge.
2. a kind of BiOBr/SiO as described in claim 12The preparation method of composite aerogel catalysis material, feature exist
In: steps are as follows:
(1), by a certain amount of bismuth source ultrasonic dissolution in solvent；It is mixed after to be dissolved with a certain amount of ethyl orthosilicate, in magnetic
Some time is stirred in power blender；
(2), a certain amount of bromine source is weighed to be dissolved in the water；
(3), the solution of step (2) is slowly dropped in step (1), magnetic agitation for a period of time after, be slowly added dropwise certain dense
The hydrochloric acid regulation system pH of degree simultaneously continues magnetic agitation certain time；
(4), heating water bath for a period of time after, natural cooling.Under magnetic stirring, with certain density ammonia water conditioning system pH,
Rotor is taken out when solution becomes sticky, it is static to make its gel.
(5), dehydrated alcohol aging is added after gel, then carries out solvent displacement a period of time with n-hexane.Then trimethylchloro-silicane
It is modified that the mixed solution of alkane, n-hexane and dehydrated alcohol carries out surface.It is done after the completion of modification using room temperature gradient seasoning
It is dry, sample is obtained after the completion of dry.
(6), the hydrophilic treated of sample.Sample in step (5) is placed in Muffle furnace, is calcined at a certain temperature.
3. bismuth source is Bi (NO according in claim 2 (1)3)3·5H2O and Bi2O3One of；The solvent is anhydrous second
Alcohol or ethylene glycol；Behind bismuth source and ethyl orthosilicate mixing, the magnetic agitation time is 30~60 min.
4. bromine source is one in KBr, NaBr or CTAB (cetyl trimethylammonium bromide) according in claim 2 (2)
Kind.
5. the magnetic agitation time is 10~30 min according in claim 2 (3)；The concentration of hydrochloric acid is 0.1~0.5 mol/
L；PH=2~4 of hydrochloric acid regulation system used；System pH continues the magnetic agitation time as 10~30 min after stablizing.
6. the heating water bath time is 3~6 h according in claim 2 (4)；The ammonium hydroxide for the use of concentration being 0.1~0.5 mol/L
Regulation system pH=8~10.
7. using dehydrated alcohol ageing time for 10~24 h according in claim 2 (5)；Solvent is carried out using n-hexane to set
Changing the time is 24~36 h；The molar ratio of trim,ethylchlorosilane, n-hexane and dehydrated alcohol is (0.5~1): (0.5~1): 1,
Modification time is 10~24 h；The dehydrated alcohol, n-hexane and trim,ethylchlorosilane, n-hexane mix molten with dehydrated alcohol
The dosage of agent is 20~30 mL；Room temperature gradient seasoning is respectively to take 3 time points within the scope of 50~120 DEG C, be separately dried 20
~30 min.
8. calcination temperature is 300~450 DEG C according in claim 2 (6), soaking time is 30~60 min.
9. the volume ratio of dehydrated alcohol or ethylene glycol, ethyl orthosilicate and water is 4:2 according in claim 2 (1) and (2):
1。
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111604067A (en) * | 2020-06-02 | 2020-09-01 | 河北大学 | Halogen silicon oxide bismuth material and preparation method and application thereof |
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