CN107570135A - Mullite for photochemical catalytic oxidation loads TiO2And preparation method and applications - Google Patents
Mullite for photochemical catalytic oxidation loads TiO2And preparation method and applications Download PDFInfo
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- CN107570135A CN107570135A CN201710750614.5A CN201710750614A CN107570135A CN 107570135 A CN107570135 A CN 107570135A CN 201710750614 A CN201710750614 A CN 201710750614A CN 107570135 A CN107570135 A CN 107570135A
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Abstract
The invention discloses a kind of mullite for photochemical catalytic oxidation to load TiO2And preparation method and applications, mullite load TiO2Including absolute ethyl alcohol, butyl titanate and mullite.Preparation method is：First pass through absolute ethyl alcohol and butyl titanate mixes, with nitre acid for adjusting pH to 23, TiO is made2Colloidal sol；With distilled water immersion mullite, mullite suspension is obtained, takes appropriate TiO2Colloidal sol is added in mullite suspension, stirring, is stood, precipitation, is then dried, calcined 13 hours at 300 DEG C 500 DEG C, obtains mullite load TiO2.The present invention prepares TiO in gained mullite2Addition be more than 20% when, mullite load TiO2More preferable catalytic oxidation effect is respectively provided with to nitrogen oxides and methyl orange, when the catalysis oxidation time is 420min, mullite load TiO290% is reached to methyl orange degradation rate；With pure TiO2Compare, mullite load TiO280% TiO can be saved2Dosage, reduce cost of material.Its preparation method is simple, cost is cheap, suitable for industrialized production.
Description
Technical field
The present invention relates to the environmental protection technical field for removing pollutant, and in particular to the mullite for photochemical catalytic oxidation
Load TiO2And preparation method and applications.
Background technology
Waste water from dyestuff, discharged nitrous oxides can all pollute into environment, pollutant process method master common at present
There are membrane separation process, extraction, radiation method, oxidizing process, Coagulation Method, absorption method etc..Wherein, membrane separation process is held high due to film price
Expensive, concentration polarization causes the factors such as fouling membrane so that its large-scale application is restricted；Extraction extract consumption is big,
Cost is higher；Radiation method power consumption is high, and radiation appliance is expensive, and can produce harm to human body, need to additionally configure protector,
It is unable to wide popularization and application；Coagulation Method is widely used, but the problem of existence and stability difference；Absorption method easily causes absorption easily up to full
With, it is inefficient, be not easily recycled the problems such as.Oxidizing process has deep oxidation under high temperature method, chemical oxidization method and photocatalytic oxidation.It is high
Temperature aoxidizes improper for wastewater treatment, and chemical oxidization method easily produces oxidant secondary pollution, and photochemical catalytic oxidation is applied to
Dyestuff it is useless and and the governance process of nitrogen oxides pollution thing in, without adding oxidant to system, avoid the secondary of oxidant
Pollution, have the advantages that no chemical agent addition, cost are low and pollution-free, have broad application prospects.
TiO2As a kind of the most frequently used photochemical catalyst, oxygen can be effectively catalyzed to dyestuff, nitrogen oxides under ultraviolet light
Change, but its photocatalytic oxidation efficiency is not high.
The content of the invention
It is an object of the invention to solve above-mentioned technical problem, there is provided a kind of mullite for photochemical catalytic oxidation loads
TiO2And preparation method and applications, mullite load TiO2Photochemical catalytic oxidation speed faster, effect is more preferable, property is stable, right
Environment is nuisanceless, and to the regulation effect of dyestuff and nitrogen oxides more preferably；Its preparation method is simple, cost is cheap, suitable for work
Industry metaplasia is produced.
In order to achieve the above object, the present invention is achieved using following technical scheme.
(1) the mullite load TiO for photochemical catalytic oxidation2, including following raw material：Absolute ethyl alcohol, butyl titanate and not
Carry out stone.
Preferably, the usage ratio of the absolute ethyl alcohol, butyl titanate and mullite is：(10-20)mL：(4-8)mL：
(1-45g)。
(2) the mullite load TiO for photochemical catalytic oxidation2Preparation method, including following operating procedure：
Step 1, TiO is prepared2Colloidal sol：
Step 1a, absolute ethyl alcohol is taken, add butyl titanate, mixed, obtain transparent yellow solution；
Step 1b, the pH to 2-3 of the yellow solution is adjusted, continues to stir, obtains TiO2Colloidal sol；
Step 2, mullite load TiO is prepared2：
Step 2a, takes mullite to be added in distilled water, immersion, obtains mullite suspension；
Step 2b, take the TiO2Colloidal sol, the mullite suspension is added thereto, stir, obtain mixing suspension；
Step 2c, the mixing suspension is stood, precipitation, obtain sediment；
Step 2d, by sediment drying, calcining, obtain mullite load TiO2。
Preferably, in step 1a, the mixing is mechanical agitation.
Preferably, in step 1a, the temperature of the mixing is 18-25 DEG C, and the time of mixing is small for 0.5-1
When.
Preferably, in step 1b, the regulation is adjusted using 1mol/L salpeter solution.
Preferably, in step 1b, the rotating speed of the stirring is 300-600 revs/min, and the time of stirring is 1.5-3 hours.
Preferably, in step 2a, the mullite is 200-400 mesh powders.
Preferably, in step 2a, the mullite and the distilled water ratio are (1-3) g：(10-30)mL.
Preferably, in step 2a, the time of the immersion is 0.8-1.2 hours.
Preferably, in step 2b, the TiO2The usage ratio of colloidal sol and mullite is：(1-9)mL：(1-3)g.
Preferably, in step 2b, the rotating speed of the stirring is 400-600 revs/min, and the time of the stirring is small for 6-10
When.
Preferably, in step 2d, the temperature of the drying is 40 DEG C -200 DEG C.
It is further preferred that in step 2d, the temperature of the drying is 120 DEG C.
Preferably, in step 2d, the temperature of the calcining is 300 DEG C -500 DEG C, and the time of calcining is 1-3 hours.
(3) the mullite load TiO for photochemical catalytic oxidation2Application in photochemical catalytic oxidation nitrogen oxides.
The different TiO of equivalent are weighed respectively2Addition mullite load TiO2, different TiO2Addition saponite
Load TiO2, pure mullite and pure TiO2, it is respectively placed in simulation sunlight device, is filled with nitrogen oxides thereto, is surveyed
Determine and calculate nitrogen oxides remnants rates in different time, be i.e. the residual concentration of nitrogen oxides and initial concentration ratio, using the time as
Abscissa, nitrogen oxides remnants rates are ordinate, draw curve comparison figure.
(4) the mullite load TiO for photochemical catalytic oxidation2Application in photochemical catalytic oxidation methyl orange.
Take beaker several, the methyl orange solution of equivalent be separately added into it, then be separately added into successively equivalent pure mullite,
Mullite loads TiO2, genuine soap stone, saponite load TiO2And pure TiO2, then it is placed on the camera bellows irradiated under ultraviolet light
In, with magnetic stirrer, take a supernatant liquor to be positioned in cuvette with light splitting light into beaker at regular intervals
Degree measures respective absorbance, and calculates methyl orange degradation rate according to absorbance, and using the time as abscissa, degradation rate is sat to be vertical
Mark, draw curve comparison figure.
Compared with prior art, beneficial effects of the present invention are：
(1) mullite load TiO2Not soluble in water, property is stable, nuisanceless to environment.(2) when mullite loads TiO2In
TiO2When addition is more than 20%, mullite load TiO2The catalysis oxidation efficiency of nitrogen oxides and methyl orange is better than pure
TiO2, pure mullite, genuine soap stone and saponite load TiO2.(3) when mullite loads TiO2With pure TiO2Catalysis to nitrogen oxides
When effect reaches identical, mullite load TiO280%TiO can at least be saved2Dosage, reduce cost of material.(4) with it is pure
TiO2TiO is loaded with saponite2Compare, mullite load TiO2Photochemical catalytic oxidation speed faster.(5) when mullite loads TiO2
Middle TiO2Addition be more than 20% when, when the catalysis oxidation time be 420min, mullite load TiO2Methyl orange degradation rate is reached
To 90%.
Brief description of the drawings
The present invention is described in further details with specific embodiment below in conjunction with the accompanying drawings.
Fig. 1 is that mullite loads TiO2, pure mullite and pure TiO2To the catalysis oxidation rate curve comparison figure of nitrogen oxides；
Wherein, abscissa is the time, unit min；Ordinate is nitrogen oxides remnants rates, i.e., nitrogen oxides in catalysis oxidation product
Residual concentration and initial concentration ratio；A curves are catalysis oxidation rate curve of the pure mullite to nitrogen oxides, and b curves are not next
Stone loads TiO2Middle TiO2Addition be 10% when mullite load TiO2To the catalysis oxidation rate curve of nitrogen oxides, c curves
TiO is loaded for mullite2Middle TiO2Addition be 20% when mullite load TiO2It is bent to the catalysis oxidation rate of nitrogen oxides
Line, d curves are that mullite loads TiO2Middle TiO2Addition be 30% when mullite load TiO2Catalysis oxygen to nitrogen oxides
Rate curve, e curves are pure TiO2To the catalysis oxidation rate curve of nitrogen oxides；
Fig. 2 is that saponite loads TiO2, genuine soap stone and pure TiO2To the catalysis oxidation rate curve comparison figure of nitrogen oxides；Wherein,
Abscissa is the time, unit min；Ordinate is nitrogen oxides remnants rates, i.e., the remnants of nitrogen oxides in catalysis oxidation product
Concentration and initial concentration ratio；A curves are catalysis oxidation rate curve of the genuine soap stone to nitrogen oxides, and b curves load for saponite
TiO2Middle TiO2Addition be 5% when saponite load TiO2To the catalysis oxidation rate curve of nitrogen oxides, c curves are born for saponite
Carry TiO2Middle TiO2Addition be 15% when saponite load TiO2To the catalysis oxidation rate curve of nitrogen oxides, d curves are saponite
Load TiO2Middle TiO2Addition be 20% when saponite load TiO2To the catalysis oxidation rate curve of nitrogen oxides, e curves are soap
Stone loads TiO2Middle TiO2Addition be 30% when saponite load TiO2To the catalysis oxidation rate curve of nitrogen oxides, f curves are
Pure TiO2To the catalysis oxidation rate curve of nitrogen oxides；
Fig. 3 is pure mullite, mullite load TiO2, genuine soap stone and saponite load TiO2To methyl orange degradation rate comparison diagram；
Wherein, abscissa is the time, unit min；Ordinate is degradation rate, unit %；A curves are that mullite loads TiO2To first
Base orange inhales degradation rate curve, and b curves are that saponite loads TiO2To methyl orange degradation rate curve, c curves are pure mullite to methyl
Orange degradation rate curve, d curves are genuine soap stone to methyl orange degradation rate curve；
Fig. 4 is that mullite loads TiO2With pure TiO2To methyl orange degradation rate comparison diagram；Wherein, abscissa is the time, unit
For min；Ordinate is degradation rate, unit %；A curves are that mullite loads TiO2Middle TiO2Addition be 10% when not come
Stone loads TiO2To the degradation rate curve of methyl orange, b curves are that mullite loads TiO2Middle TiO2Addition be 15% when not come
Stone loads TiO2To the degradation rate curve of methyl orange, c curves are that mullite loads TiO2Middle TiO2Addition be 20% when not come
Stone loads TiO2To the degradation rate curve of methyl orange, d curves are that mullite loads TiO2Middle TiO2Addition be 30% when not come
Stone loads TiO2To the degradation rate curve of methyl orange, e curves are pure TiO2To the degradation rate curve of methyl orange.
Embodiment
Embodiment of the present invention is described in detail below in conjunction with embodiment, but those skilled in the art will
It will be appreciated that the following example is merely to illustrate the present invention, and it is not construed as limiting the scope of the present invention.
Embodiment 1：
Mullite for photochemical catalytic oxidation loads TiO2, including following raw material：Absolute ethyl alcohol 100mL, butyl titanate
80mL and mullite 20g.
The above-mentioned mullite for photochemical catalytic oxidation loads TiO2Preparation method, including following preparation process：
Step 1, TiO is prepared2Colloidal sol：
Step 1a, absolute ethyl alcohol is taken, add butyl titanate, mechanical agitation 0.5 hour at 21.5 DEG C, obtain transparent yellow
Solution；
Step 1b, the pH to 2 of yellow solution is adjusted using 1mol/L salpeter solution, is 300 revs/min of conditions in rotating speed
Under continue stirring 2 hours, obtain TiO2Colloidal sol；
Step 2, mullite load TiO is prepared2：
Step 2a, take 200 mesh Mullite Powders to be added in 100mL distilled water, soak 1 hour, obtain mullite suspension；
Step 2b, take 10mL TiO2Colloidal sol, mullite suspension is added thereto, stirred under being 500 revs/min in rotating speed
Mix 8 hours, obtain mixing suspension；
Step 2c, mixing suspension is stood, precipitated, obtains sediment；
Step 2d, sediment is dried under the conditions of 120 DEG C, then calcine 2 hours, obtained not under 400 DEG C of temperature conditionss
Carry out stone load TiO2, wherein TiO2Content account for mullite load TiO25%.
Embodiment 2：
Mullite for photochemical catalytic oxidation loads TiO2, including following raw material：Absolute ethyl alcohol 100mL, butyl titanate
80mL and mullite 20g.
The above-mentioned mullite for photochemical catalytic oxidation loads TiO2Preparation method, including following preparation process：
Step 1, TiO is prepared2Colloidal sol：
Step 1a, absolute ethyl alcohol is taken, add butyl titanate, mechanical agitation 1 hour at 18 DEG C, it is molten to obtain transparent yellow
Liquid；
Step 1b, the pH to 2 of yellow solution is adjusted using 1mol/L salpeter solution, is 300 revs/min of conditions in rotating speed
Under continue stirring 2 hours, obtain TiO2Colloidal sol；
Step 2, mullite load TiO is prepared2：
Step 2a, take 200 mesh Mullite Powders to be added in 200mL distilled water, soak 0.8 hour, obtain mullite suspension
Liquid；
Step 2b, take 20mL TiO2Colloidal sol, mullite suspension is added thereto, stirred under being 600 revs/min in rotating speed
Mix 6 hours, obtain mixing suspension；
Step 2c, mixing suspension is stood, precipitated, obtains sediment；
Step 2d, sediment is dried under the conditions of 120 DEG C, then calcine 1 hour, obtained not under 500 DEG C of temperature conditionss
Carry out stone load TiO2, wherein TiO2Content account for mullite load TiO210%.
Embodiment 3：
Mullite for photochemical catalytic oxidation loads TiO2, including following raw material：Absolute ethyl alcohol 100mL, butyl titanate
80mL and mullite 20g.
The above-mentioned mullite for photochemical catalytic oxidation loads TiO2Preparation method, including following preparation process：
Step 1, TiO is prepared2Colloidal sol：
Step 1a, absolute ethyl alcohol is taken, add butyl titanate, mechanical agitation 0.5 hour at 25 DEG C, it is molten to obtain transparent yellow
Liquid；
Step 1b, the pH to 2 of yellow solution is adjusted using 1mol/L salpeter solution, is 300 revs/min of conditions in rotating speed
Under continue stirring 2 hours, obtain TiO2Colloidal sol；
Step 2, mullite load TiO is prepared2：
Step 2a, take 400 mesh Mullite Powders to be added in 300mL distilled water, soak 1.2 hours, obtain mullite suspension
Liquid；
Step 2b, take 34mL TiO2Colloidal sol, mullite suspension is added thereto, stirred under being 400 revs/min in rotating speed
Mix 10 hours, obtain mixing suspension；
Step 2c, mixing suspension is stood, precipitated, obtains sediment；
Step 2d, sediment is dried under the conditions of 80 DEG C, then calcined 3 hours under 300 DEG C of temperature conditionss, obtained and do not come
Stone loads TiO2, wherein TiO2Content account for mullite load TiO215%.
Embodiment 4：
Mullite for photochemical catalytic oxidation loads TiO2, including following raw material：Absolute ethyl alcohol 100mL, butyl titanate
80mL and mullite 20g.
The above-mentioned mullite for photochemical catalytic oxidation loads TiO2Preparation method, including following preparation process：
Step 1, TiO is prepared2Colloidal sol：
Step 1a, absolute ethyl alcohol is taken, add butyl titanate, mechanical agitation 0.75 hour at 21.5 DEG C, obtain transparent Huang
Color solution；
Step 1b, the pH to 3 of yellow solution is adjusted using 1mol/L salpeter solution, is 600 revs/min of conditions in rotating speed
Under continue stirring 1.5 hours, obtain TiO2Colloidal sol；
Step 2, mullite load TiO is prepared2：
Step 2a, take 300 mesh Mullite Powders to be added in 100mL distilled water, soak 1.2 hours, obtain mullite suspension
Liquid；
Step 2b, take 48mL TiO2Colloidal sol, mullite suspension is added thereto, stirred under being 500 revs/min in rotating speed
Mix 10 hours, obtain mixing suspension；
Step 2c, mixing suspension is stood, precipitated, obtains sediment；
Step 2d, sediment is dried under the conditions of 200 DEG C, then calcine 3 hours, obtained not under 300 DEG C of temperature conditionss
Carry out stone load TiO2, wherein TiO2Content account for mullite load TiO220%..
Embodiment 5：
Mullite for photochemical catalytic oxidation loads TiO2, including following raw material：Absolute ethyl alcohol 100mL, butyl titanate
80mL and mullite 20g.
The above-mentioned mullite for photochemical catalytic oxidation loads TiO2Preparation method, including following preparation process：
Step 1, TiO is prepared2Colloidal sol：
Step 1a, absolute ethyl alcohol is taken, add butyl titanate, mechanical agitation 1 hour at 21.5 DEG C, it is molten to obtain transparent yellow
Liquid；
Step 1b, the pH to 2.5 of yellow solution is adjusted using 1mol/L salpeter solution, is 400 revs/min of bars in rotating speed
Continue stirring 3 hours under part, obtain TiO2Colloidal sol；
Step 2, mullite load TiO is prepared2：
Step 2a, take 200 mesh Mullite Powders to be added in 300mL distilled water, soak 1 hour, obtain mullite suspension；
Step 2b, take 82mL TiO2Colloidal sol, mullite suspension is added thereto, stirred under being 400 revs/min in rotating speed
Mix 8 hours, obtain mixing suspension；
Step 2c, mixing suspension is stood, precipitated, obtains sediment；
Step 2d, sediment is dried under the conditions of 200 DEG C, then calcine 2 hours, obtained not under 400 DEG C of temperature conditionss
Carry out stone load TiO2, wherein TiO2Content account for mullite load TiO230%.
Embodiment 1-5 is the TiO that 20g mullites load different volumes2Different TiO obtained by colloidal sol2The mullite of addition
Load TiO2, specific conversion scale is as shown in table 1：
Table 1TiO2Sol volume and mullite load TiO2Middle TiO2The substitution ratio of mass percent
Embodiment 6：
Mullite for photochemical catalytic oxidation loads TiO2, including following raw material：Absolute ethyl alcohol 200mL, butyl titanate
40mL and mullite 30g.
The above-mentioned mullite for photochemical catalytic oxidation loads TiO2Preparation method, including following preparation process：
Step 1, TiO is prepared2Colloidal sol：Step 1a, absolute ethyl alcohol is taken, add butyl titanate, the mechanical agitation at 21.5 DEG C
0.5 hour, obtain transparent yellow solution；
Step 1b, using 1mol/L salpeter solution adjust yellow solution pH to 2, after being added dropwise to complete rotating speed be 600
Continue stirring 2 hours under the conditions of rev/min, obtain TiO2Colloidal sol；
Step 2, mullite load TiO is prepared2：
Step 2a, take 270 mesh Mullite Powders to be added in 200mL distilled water, soak 0.8 hour, obtain mullite suspension
Liquid；
Step 2b, take 50mL TiO2Colloidal sol, mullite suspension is added thereto, stirred under being 600 revs/min in rotating speed
Mix 6 hours, obtain mixing suspension；
Step 2c, mixing suspension is stood, precipitated, obtains sediment；
Step 2d, sediment is dried under the conditions of 120 DEG C, then calcine 2 hours, obtained not under 500 DEG C of temperature conditionss
Carry out stone load TiO2。
Embodiment 7：
Mullite for photochemical catalytic oxidation loads TiO2, including following raw material：Absolute ethyl alcohol 150mL, butyl titanate
60mL and mullite 30g.
The above-mentioned mullite for photochemical catalytic oxidation loads TiO2Preparation method, including following preparation process：
Step 1, TiO is prepared2Colloidal sol：
Step 1a, absolute ethyl alcohol is taken, add butyl titanate, mechanical agitation 0.5 hour at 18 DEG C, it is molten to obtain transparent yellow
Liquid；
Step 1b, the pH to 3 of yellow solution is adjusted using 1mol/L salpeter solution, is 300 revs/min of conditions in rotating speed
Under continue stirring 2 hours, obtain TiO2Colloidal sol；
Step 2, mullite load TiO is prepared2：
Step 2a, take 325 mesh Mullite Powders to be added in 200mL distilled water, soak 1 hour, obtain mullite suspension；
Step 2b, take 90mL TiO2Colloidal sol, mullite suspension is added thereto, stirred under being 500 revs/min in rotating speed
Mix 8 hours, obtain mixing suspension；
Step 2c, mixing suspension is stood, precipitated, obtains sediment；
Step 2d, sediment is dried under the conditions of 80 DEG C, then calcined 3 hours under 400 DEG C of temperature conditionss, obtained and do not come
Stone loads TiO2。
Embodiment 8：
Mullite for photochemical catalytic oxidation loads TiO2, including following raw material：Absolute ethyl alcohol 100mL, butyl titanate
60mL and mullite 10g.
The above-mentioned mullite for photochemical catalytic oxidation loads TiO2Preparation method, including following preparation process：
Step 1, TiO is prepared2Colloidal sol：
Step 1a, absolute ethyl alcohol is taken, add butyl titanate, mechanical agitation 1 hour at 25 DEG C, it is molten to obtain transparent yellow
Liquid；
Step 1b, the pH to 2 of yellow solution is adjusted using 1mol/L salpeter solution, is 600 revs/min of conditions in rotating speed
Under continue stirring 1.5 hours, obtain TiO2Colloidal sol；
Step 2, mullite load TiO is prepared2：
Step 2a, take 200 mesh Mullite Powders to be added in 100mL distilled water, soak 1.2 hours, obtain mullite suspension
Liquid；
Step 2b, take 10mL TiO2Colloidal sol, mullite suspension is added thereto, stirred under being 400 revs/min in rotating speed
Mix 10 hours, obtain mixing suspension；
Step 2c, mixing suspension is stood, precipitated, obtains sediment；
Step 2d, sediment is dried under the conditions of 40 DEG C, then calcined 1 hour under 500 DEG C of temperature conditionss, obtained and do not come
Stone loads TiO2。
Embodiment 9：
Mullite for photochemical catalytic oxidation loads TiO2, include the raw material of following ratio：Absolute ethyl alcohol 150mL, metatitanic acid
Butyl ester 60mL and mullite 200g.
The above-mentioned mullite for photochemical catalytic oxidation loads TiO2Preparation method, including following preparation process：
Step 1, TiO is prepared2Colloidal sol：
Step 1a, absolute ethyl alcohol is taken, add butyl titanate, mechanical agitation 0.5 hour at 25 DEG C, it is molten to obtain transparent yellow
Liquid；
Step 1b, the pH to 2 of yellow solution is adjusted using 1mol/L salpeter solution, is 300 revs/min of conditions in rotating speed
Under continue stirring 2 hours, obtain TiO2Colloidal sol；
Step 2, mullite load TiO is prepared2：
Step 2a, take 400 mesh Mullite Powders to be added in 300mL distilled water, soak 0.8 hour, obtain mullite suspension
Liquid；
Step 2b, take 50mL TiO2Colloidal sol, mullite suspension is added thereto, stirred under being 400 revs/min in rotating speed
Mix 6 hours, obtain mixing suspension；
Step 2c, mixing suspension is stood, precipitated, obtains sediment；
Step 2d, sediment is dried under the conditions of 120 DEG C, then calcine 2 hours, obtained not under 400 DEG C of temperature conditionss
Carry out stone load TiO2。
Embodiment 10：
Mullite for photochemical catalytic oxidation loads TiO2, including following raw material：Absolute ethyl alcohol 150mL, butyl titanate
40mL and mullite 450g.
The above-mentioned mullite for photochemical catalytic oxidation loads TiO2Preparation method, including following preparation process：
Step 1, TiO is prepared2Colloidal sol：
Step 1a, absolute ethyl alcohol is taken, add butyl titanate, mechanical agitation 0.5 hour at 21.5 DEG C, obtain transparent yellow
Solution；
Step 1b, the pH to 2 of yellow solution is adjusted using 1mol/L salpeter solution, is 300 revs/min of conditions in rotating speed
Under continue stirring 2 hours, obtain TiO2Colloidal sol；
Step 2, mullite load TiO is prepared2：
Step 2a, take 300 mesh Mullite Powders to be added in 100mL distilled water, soak 1.2 hours, obtain mullite suspension
Liquid；
Step 2b, take 90mL TiO2Colloidal sol, mullite suspension is added thereto, stirred under being 500 revs/min in rotating speed
Mix 8 hours, obtain mixing suspension；
Step 2c, mixing suspension is stood, precipitated, obtains sediment；
Step 2d, sediment is dried under the conditions of 200 DEG C, then calcine 2 hours, obtained not under 300 DEG C of temperature conditionss
Carry out stone load TiO2。
Embodiment 11：
Mullite for photochemical catalytic oxidation loads TiO2, including following raw material：Absolute ethyl alcohol 150mL, butyl titanate
40mL and mullite 30g.
The above-mentioned mullite for photochemical catalytic oxidation loads TiO2Preparation method, including following preparation process：
Step 1, TiO is prepared2Colloidal sol：
Step 1a, absolute ethyl alcohol is taken, add butyl titanate, mechanical agitation 0.75 hour at 18 DEG C, obtain transparent yellow
Solution；
Step 1b, the pH to 2 of yellow solution is adjusted using 1mol/L salpeter solution, is 300 revs/min of conditions in rotating speed
Under continue stirring 2 hours, obtain TiO2Colloidal sol；
Step 2, mullite load TiO is prepared2：
Step 2a, take 300 mesh Mullite Powders to be added in 200mL distilled water, soak 0.8 hour, obtain mullite suspension
Liquid；
Step 2b, take 10mL TiO2Colloidal sol, mullite suspension is added thereto, stirred under being 500 revs/min in rotating speed
Mix 6 hours, obtain mixing suspension；
Step 2c, mixing suspension is stood, precipitated, obtains sediment；
Step 2d, sediment is dried under the conditions of 120 DEG C, then calcine 3 hours, obtained not under 300 DEG C of temperature conditionss
Carry out stone load TiO2。
Experiment 1
The mullite that above-described embodiment is prepared loads TiO2For photochemical catalytic oxidation nitrogen oxides, nitrogen oxygen herein
Compound refers mainly to NO2, the admixture of gas such as NO.
1) test method：
1g embodiment 2, embodiment 4, the gained mullite of embodiment 5 load TiO is weighed respectively2, its mullite load TiO2
Middle TiO2Addition be respectively 10%, 20% and 30%, be respectively placed in simulation sunlight device in, be filled with thereto
NO, determine and calculate NO residual concentrations and initial concentration ratio in different time；Weigh 1g pure mullite and pure respectively again
TiO2, it is respectively placed in simulation sunlight device, is filled with NO thereto, is determined and to calculate NO remnants in different time dense
Degree and initial concentration ratio；Mullite loads TiO2, pure mullite and pure TiO2To catalytic oxidation effect such as Fig. 1 of nitrogen oxides
It is shown.
1g saponite load TiO is weighed respectively2, its saponite load TiO2Middle TiO2Addition be respectively 5%, 15%,
20% and 30%, it is respectively placed in simulation sunlight device, is filled with NO thereto, determines and calculate NO in different time
Residual concentration and initial concentration ratio；Weigh 1g genuine soap stone and pure TiO respectively again2, it is respectively placed in simulation sunlight
In device, NO is filled with thereto, is determined and is calculated NO residual concentrations and initial concentration ratio in different time；Saponite loads
TiO2, genuine soap stone and pure TiO2It is as shown in Figure 2 to the catalytic oxidation effect of nitrogen oxides.
2) result of the test：Result of the test is as depicted in figs. 1 and 2
Fig. 1 is that mullite loads TiO2, pure mullite and pure TiO2To the catalysis oxidation rate curve comparison figure of nitrogen oxides；
Fig. 2 is that saponite loads TiO2, genuine soap stone and pure TiO2To the catalysis oxidation rate curve comparison figure of nitrogen oxides.
As shown in Figure 1, compared with pure mullite, mullite load TiO2Middle different TiO2The catalysis oxidation product of addition
Middle nitrogen oxides remnants rates are below the pure mullite of homogenous quantities, illustrate that mullite loads TiO2Than not loading TiO2To nitrogen oxidation
Thing has more preferable photochemical catalytic oxidation effect.With pure TiO2Compare, when mullite loads TiO2Middle TiO2Addition is more than 20%
When, nitrogen oxides remnants rates are less than the pure TiO of homogenous quantities in its catalysis oxidation product2, illustrate that mullite loads TiO2Middle TiO2Add
Photochemical catalytic oxidation effect when dosage is more than 20% to nitrogen oxides is more preferable；In addition, as seen from the figure, when nitrogen oxides remnants rate phases
Deng when, mullite load TiO2Oxidation catalysis time and pure TiO2Shorten compared to obvious.
Thus illustrate, when mullite loads TiO2With pure TiO2When reaching identical to the catalytic effect of nitrogen oxides, mullite
Load TiO280%TiO can at least be saved2Dosage, cost of material is reduced, because internal TiO2Particle seldom with pollution
Thing contacts, so not having the effect of catalysis oxidation；In addition, the mullite load TiO of same quality2With pure TiO2Compare, Mo Lai
Stone loads TiO2To the catalytic oxidation effect of nitrogen oxides more preferably, this is due to TiO2In mullite particle Surface coating, improve
TiO2With the contact area of pollutant, accelerate the progress to nitrogen oxides catalytic oxidation.
As shown in Figure 2, in the range of experimental measuring, compared with genuine soap stone, saponite load TiO2Middle different TiO2Addition
Nitrogen oxides remnants rates are below the genuine soap stone of homogenous quantities in catalysis oxidation product, illustrate that saponite loads TiO2Than not loading TiO2
There is more preferable photochemical catalytic oxidation effect to nitrogen oxides.Saponite loads TiO2Nitrogen oxides remnants rates are equal in catalysis oxidation product
Higher than the pure TiO of homogenous quantities2, illustrate that saponite loads TiO2Photochemical catalytic oxidation effect to nitrogen oxides is not so good as pure TiO2It is good.Soap
Soil load TiO2Although TiO can be improved2Specific surface area, but due to bentonite load TiO2In TiO2Mainly it is inserted into
Bentonite mineral lattice interlayer, substantially reduces TiO2To the catalytic oxidation effect of nitrogen oxides.
It follows that as mullite load TiO2Middle TiO2When addition is more than 20%, mullite load TiO2To nitrogen oxidation
The catalysis oxidation efficiency highest of thing, next to that pure TiO2, it is finally saponite load TiO2, and pure mullite and genuine soap stone are to nitrogen oxygen
The catalytic oxidation effect of compound is poor.Mullite (3Al2O3·2SiO2) and conventional silicate carrier mineral facies ratio, it has
There is higher alumina silica ratio, possess more alumina octahedrals；Mullite lattice charge balances, and being not susceptible to ion with cation hands over
Change absorption.Alumina octahedral surface typically exhibits electropositive, and common are organic pollutants ion and nitrogen oxides is easier to inhale
It is attached to electropositive carrier surface.Therefore, mullite has higher as catalyst carrier than other silicates carrier minerals
The catalysis oxidation efficiency.
Mullite load TiO obtained by other embodiment2The same experiment 1 of catalytic oxidation effect to nitrogen oxides.
Experiment 2：
The mullite that above-described embodiment is prepared loads TiO2For photochemical catalytic oxidation methyl orange.
1) test method：
400ml 4, beaker is taken, concentration is separately added into it and is 10mg/L methyl orange solution 200ml, then is distinguished successively
Add 2g pure mullite, mullite load TiO2, genuine soap stone and saponite load TiO2, wherein mullite load TiO2To implement
The TiO of the gained of example 42The mullite that addition is 20% loads TiO2.Then it is placed on the camera bellows irradiated under ultraviolet light
In, with magnetic stirrer, take a supernatant liquor to be positioned in cuvette into beaker every 10min and use spectrophotometer
Respective absorbance is measured, and methyl orange degradation rate is calculated according to absorbance, as a result as shown in Figure 3.
400ml 5, beaker is taken, concentration is separately added into it and is 10mg/L methyl orange solution 200ml, then is distinguished successively
Add the mullite load TiO obtained by embodiment 2-52With pure TiO2.Then it is placed on the camera bellows irradiated under ultraviolet light
In, with magnetic stirrer, take a supernatant liquor to be positioned in cuvette into beaker every 10min and use spectrophotometer
Respective absorbance is measured, and methyl orange degradation rate is calculated according to absorbance, as a result as shown in Figure 4.
2) result of the test：Result of the test is as shown in Figure 3 and Figure 4
Fig. 3 is pure mullite, mullite load TiO2, genuine soap stone and saponite load TiO2To methyl orange degradation rate comparison diagram；
Fig. 4 mullites load TiO2Different TiO2Addition and pure TiO2To methyl orange degradation rate comparison diagram.
From the figure 3, it may be seen that pure mullite is less than 20% to methyl orange degradation rate, genuine soap stone is less than to methyl orange degradation rate
20%；Mullite loads TiO2TiO is loaded higher than pure mullite, genuine soap stone and saponite to the degradation rate of methyl orange2To methyl orange
Degradation rate, illustrate mullite load TiO2The best results of degraded to methyl orange；As shown in Figure 4, when mullite loads TiO2
Middle TiO2When addition is more than 20%, its degradation rate to methyl orange is apparently higher than pure TiO2, when its catalysis oxidation to methyl orange
When time is 420min, degradation rate reaches 90%.
It follows that mullite loads TiO2There is good catalytic oxidation effect to methyl orange.
Mullite load TiO obtained by other embodiment2The same experiment 2 of degradation effect to methyl orange.
Although the present invention is described in detail with a general description of the specific embodiments in this specification,
But on the basis of the present invention, it can be made some modifications or improvements, this will be apparent to those skilled in the art.
Therefore, these modifications or improvements without departing from theon the basis of the spirit of the present invention, belong to claimed model
Enclose.
Claims (10)
1. the mullite load TiO for photochemical catalytic oxidation2, it is characterised in that including following raw material：Absolute ethyl alcohol, butyl titanate
And mullite.
2. the mullite according to claim 1 for photochemical catalytic oxidation loads TiO2, it is characterised in that the anhydrous second
The usage ratio of alcohol, butyl titanate and mullite is (10-20) mL：(4-8)mL：20mL：(1-45)g.
3. the mullite load TiO for photochemical catalytic oxidation2Preparation method, it is characterised in that including following operating procedure：
Step 1, TiO is prepared2Colloidal sol：
Step 1a, absolute ethyl alcohol is taken, add butyl titanate, mixed, obtain transparent yellow solution；
Step 1b, the pH to 2-3 of the yellow solution is adjusted, continues to stir, obtains TiO2Colloidal sol；
Step 2, mullite load TiO is prepared2：
Step 2a, takes mullite to be added in distilled water, immersion, obtains mullite suspension；
Step 2b, take the TiO2Colloidal sol, the mullite suspension is added thereto, stir, obtain mixing suspension；
Step 2c, the mixing suspension is stood, precipitation, obtain sediment；
Step 2d, by sediment drying, calcining, obtain mullite load TiO2。
4. the mullite according to claim 3 for photochemical catalytic oxidation loads TiO2Preparation method, it is characterised in that
In step 1a, the temperature of the mixing is 18-25 DEG C, and the time of mixing is 0.5-1 hours.
5. the mullite according to claim 3 for photochemical catalytic oxidation loads TiO2Preparation method, it is characterised in that
In step 2a, the mullite and the distilled water ratio are (1-3) g：(10-30)mL.
6. the mullite according to claim 3 for photochemical catalytic oxidation loads TiO2Preparation method, it is characterised in that
In step 2b, the TiO2The usage ratio of colloidal sol and mullite is：(1-9)mL：(1-3)g.
7. the mullite according to claim 3 for photochemical catalytic oxidation loads TiO2Preparation method, it is characterised in that
In step 2b, the rotating speed of the stirring is 400-600 revs/min, and the time of the stirring is 6-10 hours.
8. the mullite according to claim 3 for photochemical catalytic oxidation loads TiO2Preparation method, it is characterised in that
In step 2d, the temperature of the drying is 40 DEG C -200 DEG C.
9. the mullite according to claim 3 for photochemical catalytic oxidation loads TiO2Preparation method, it is characterised in that
In step 2d, the temperature of the calcining is 300 DEG C -500 DEG C, and the time of calcining is 1-3 hours.
10. the mullite load TiO for photochemical catalytic oxidation2Application in photochemical catalytic oxidation nitrogen oxides or methyl orange.
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