CN102145280B - Method for preparing rice hull active carbon/silicon dioxide/titanium dioxide composite material - Google Patents
Method for preparing rice hull active carbon/silicon dioxide/titanium dioxide composite material Download PDFInfo
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Abstract
The invention discloses a method for preparing a rice hull active carbon/silicon dioxide/titanium dioxide composite material in the technical field of preparation of nano titanium dioxide photocatalysts. The method comprises the following steps of: carrying out acid cleaning on rice hull powder; adding an NaOH solution into the rice hull powder which is subjected to acid cleaning and carrying out alkali cooking to obtain mixed size consisting of rice hulls and sodium silicate; preparing a rice hull/silicon dioxide/titanium dioxide precursor; and finally carrying out carbonization and activating treatment to prepare the rice hull active carbon/silicon dioxide/titanium dioxide composite material. The rice hulls and nano titanium dioxide are combined in a chemical bond mode by silicon dioxide. The rice hull active carbon/silicon dioxide/titanium dioxide composite material not only has excellent adsorption performance of rice hull active carbon, but also has excellent photocatalysis performance of the nano titanium dioxide. The problem that the nano titanium dioxide is easy to fall off on the surface of a vector is effectively avoided. The stability of the composite material is greatly improved. The method has the advantages of simple preparation process, low price of raw materials, low cost and low pollution.
Description
Technical field
The invention belongs to the preparing technical field of nano titanium dioxide photocatalyst, be specifically related to the preparation method of a kind of rice hull active carbon/earth silicon/titanic oxide optic catalytic composite material.
Background technology
Nano titanium oxide is a kind of typical photochemical catalyst, but in traditional preparation method and application process, has shortcomings such as photocatalysis efficiency is low, recovery difficulty, thereby has limited its industrialized application.In recent years, for improving the photocatalysis effect and the recovery utilization rate of nano titanium oxide, people utilize various preparing carriers fixed titanium dioxide optical catalysts; Wherein active carbon has obtained extensive application as catalyst carrier; Active carbon has following advantage as carrier: cheap, and ability acid and alkali-resistance, stable in properties; Have flourishing pore structure, huge specific area and good absorption property, and can recycle.At present; Preparing the most frequently used method of activated carbon supported type nano titanium oxide is sol-gel process; But the defective that this method exists is: the bond strength of nano titanium oxide and absorbent charcoal carrier is lower, and nano titanium oxide is prone to come off at carrier surface, and it is not high to recycle value.Chinese patent CN 101053845A discloses the method that a kind of sol-gel process prepares active carbon-titanium dioxide composite photocatalyst; Butyl titanate is mixed with absolute ethyl alcohol and stirring; The catalyst that dropping water, acetate, absolute ethyl alcohol are made under brute force stirs obtains TiO 2 sol; In the colloidal sol process, add active carbon then, after fully stirring, heat treatment obtains active carbon-titanium dioxide composite photocatalyst; The weak point of this method mainly is: 1. the bond strength of titanium dioxide and carrier is not high after this composite photo-catalyst load; Titanium dioxide is prone to come off at carrier surface, thereby composite using the back catalytic performance to descend repeatedly, and reuse is relatively poor; 2. in the preparation process, used a large amount of organic solvents, increased production cost, and be unfavorable for environmental protection.
Summary of the invention
In view of the existing problem of background technology; The object of the present invention is to provide a kind of simple, preparation method of rice hull active carbon/earth silicon/titanic oxide composite cheaply; With rice hull active carbon loaded with nano silica and nanometer titanium dioxide composite material; With the photocatalytic activity of raising nano titanium oxide, and effectively solve be prone to the come off problem of nano titanium oxide at carrier surface.
The technical scheme that the present invention adopts comprises the steps: 1, the preliminary treatment of rice husk: rice husk use the clear water cleaning, drying, pulverizing; Cross 100 ~ 250 mesh sieves; The adding mass percentage concentration is 3% ~ 10% hydrochloric acid, and the mass ratio of rice husk and hydrochloric acid solution is 0.1 ~ 1:1, under 40 ~ 85 ℃ of temperature, stirs 1 ~ 7 hour; Washing obtains the pickling powdered rice hulls to neutral; 2, soda boiling: the NaOH solution that in said pickling powdered rice hulls, adds 0.5-3mol/L; Wherein the mass ratio of pickling powdered rice hulls and NaOH is 0.5 ~ 2:1; Constantly stir down the soda boiling temperature maintenance at 50 ~ 95 ℃, and insulation soda boiling 2 ~ 8 hours, obtaining the mixed serum of rice husk and sodium metasilicate composition; 3, the preparation of rice husk/earth silicon/titanic oxide precursor: the TiCl that under constantly stirring, in said mixed serum, adds 0.5-3.5mol/L earlier
4Solution, reaction temperature remain on 45 ~ 90 ℃; PH value to 5.5 ~ 7.5 of conditioned reaction system then, TiCl
4The solution adding finishes, and continues to stir insulation slaking 0.5 ~ 3 hour; At last with the dope filtration of gained, with the electrical conductivity≤260 μ S/cms of deionized water cyclic washing, the filter cake of gained 70 ~ 140 ℃ of vacuum drying 5 ~ 12 hours, is pulverized to filtrating, make rice husk/earth silicon/titanic oxide composite; 4, charing: said rice husk/earth silicon/titanic oxide composite under nitrogen atmosphere, in 300 ~ 550 ℃ of roastings 2 ~ 6 hours, is naturally cooled to room temperature, make rice hull carbon/earth silicon/titanic oxide composite; 5, activation: it is 30 ~ 60% ZnCl that said rice hull carbon/earth silicon/titanic oxide composite is immersed in mass percentage concentration
2Stir in the aqueous solution, wherein composite and ZnCl
2Mass ratio be 0.2 ~ 0.8:1, dip time is 12 ~ 24 hours, dry back in 400 ~ 650 ℃ of activation 1 ~ 4 hour, naturally cools to room temperature and obtains activation products under nitrogen atmosphere; 6, post processing: it is 4 ~ 20% chlorohydric acid pickling that said activation products are used mass percentage concentration earlier, then with the electrical conductivity≤260 μ S/cms of deionized water cyclic washing to filtrating, and drying, pulverizing makes rice hull active carbon/earth silicon/titanic oxide composite.
The present invention at first carries out pickling to rice husk; Then through soda boiling with the amorphous silica in the rice husk with the stripping of sodium metasilicate form; With the precipitation method technology nano silicon and nano titanium oxide are deposited on the rice husk surface equably again; Utilize silica that rice husk and the nano titanium oxide form with chemical bond is combined, prepare rice hull active carbon/earth silicon/titanic oxide composite through charing, activation at last, its advantage is:
1, utilizes the absorption property and the good photocatalysis performance of nano titanium oxide of excellence of the rice hull active carbon/earth silicon/titanic oxide composite material concurrent rice hull active carbon of precipitation method prepared.
2, between rice hull active carbon and nano titanium oxide, introduce nano silicon; Silica combines rice hull active carbon and nano titanium oxide through chemical bond securely; Avoided be prone to the come off problem of nano titanium oxide effectively, significantly improved the stability of composite at carrier surface.
3, rice hull active carbon in the composite and nano silicon all come from the agricultural wastes rice husk, and the present invention has made full use of rice husk raw material self characteristics and this renewable resource of rice husk, have solved rice husk and have piled up the environmental problem of bringing.
4, the preparation process is simple, low in raw material cost, and cost is low, not with an organic solvent, pollutes few.
The specific embodiment
Earlier rice husk is carried out preliminary treatment, pretreated method is that rice husk is used the clear water cleaning, drying; Pulverize, cross 100 ~ 250 mesh sieves, add mass percentage concentration and be 3% ~ 10% hydrochloric acid and carry out pickling; Wherein the mass ratio of rice husk and hydrochloric acid solution is 0.1 ~ 1:1; Under 40 ~ 85 ℃ of temperature, stirred 1 ~ 7 hour, washing obtains the pickling powdered rice hulls to neutral.In the pickling powdered rice hulls of gained, add in the NaOH solution of 0.5-3mol/L; Wherein the mass ratio of pickling powdered rice hulls and NaOH is 0.5 ~ 2:1, and under constantly stirring, the soda boiling temperature maintenance is at 50 ~ 95 ℃; And be incubated soda boiling 2 ~ 8 hours, obtain the mixed serum that rice husk and sodium metasilicate are formed.Prepare rice husk/earth silicon/titanic oxide precursor again, promptly under constantly stirring, in the mixed serum of rice husk that obtains and sodium metasilicate composition, add the TiCl of 0.5-3.5mol/L
4Solution, reaction temperature remain on 45 ~ 90 ℃, pH value to 5.5 ~ 7.5 of conditioned reaction system, TiCl when reaction system pH is adjusted to 5.5 ~ 7.5
4The solution adding finishes; Continue to stir, insulation slaking 0.5 ~ 3 hour is with the dope filtration of gained; With the electrical conductivity≤260 μ S/cms of deionized water cyclic washing to filtrating; The filter cake of gained 70 ~ 140 ℃ of vacuum drying 5 ~ 12 hours, is pulverized, made rice husk/earth silicon/titanic oxide composite.Carry out charing then and handle, the rice husk/earth silicon/titanic oxide composite that is about to gained in 300 ~ 550 ℃ of roastings 2 ~ 6 hours, naturally cools to room temperature under nitrogen atmosphere, make rice hull carbon/earth silicon/titanic oxide composite.Carry out activation processing again: it is 30 ~ 60% ZnCl that the rice hull carbon/earth silicon/titanic oxide composite that is about to gained is immersed in mass percentage concentration
2Stir in the aqueous solution, wherein composite and ZnCl
2Mass ratio be 0.2 ~ 0.8:1, dip time is 12 ~ 24 hours, dry back in 400 ~ 650 ℃ of activation 1 ~ 4 hour, naturally cools to room temperature and obtains activation products under nitrogen atmosphere.Be post processing at last; The activation products elder generation use mass percentage concentration that is about to gained is 4 ~ 20% chlorohydric acid pickling, then with the electrical conductivity≤260 μ S/cms of deionized water cyclic washing to filtrating, drying; Pulverize, make rice hull active carbon/earth silicon/titanic oxide composite.
Below provide 4 embodiment and 3 comparative examples to further specify the present invention:
Embodiment 1
Earlier use the clear water cleaning, drying to 1 kilogram of rice husk, pulverize, cross 250 mesh sieves, the mass percentage concentration that adds 10 kilograms is that 85 ℃ were stirred 7 hours in 3% the hydrochloric acid solution, and washing is neutrality extremely, obtains the pickling powdered rice hulls.In the pickling powdered rice hulls, add 16.7 liters of the NaOH solution of 3mol/L, constantly stirring down, the soda boiling temperature maintenance is at 95 ℃, and the insulation soda boiling obtained the mixed serum of rice husk and sodium metasilicate composition in 8 hours.Under constantly stirring, in the mixed serum that the rice husk and the sodium metasilicate of gained are formed, add the TiCl of 3.5mol/L again
4Solution, reaction temperature remain on 90 ℃, the pH value of conditioned reaction system then, and when the pH of reaction system is adjusted to 5.5, TiCl
4The solution adding finishes, and continues to stir insulation slaking 3 hours; Filter, with the deionized water cyclic washing to the electrical conductivity≤260 μ S/cm that filtrate, with the filter cake of gained 140 ℃ of vacuum drying 12 hours; Pulverize, make rice husk/earth silicon/titanic oxide composite.Again with the rice husk/earth silicon/titanic oxide composite of gained under nitrogen atmosphere, in 550 ℃ of roastings 6 hours, naturally cool to room temperature, make rice hull carbon/earth silicon/titanic oxide composite.In the rice hull carbon/earth silicon/titanic oxide composite of gained, add mass percentage concentration again and be 60% ZnCl
2The aqueous solution stirs, and wherein the mass ratio of composite and zinc chloride is 0.8:1, floods 24 hours, and dry back in 650 ℃ of activation 4 hours, naturally cools to room temperature and obtains activation products under nitrogen atmosphere.At last the activation products of gained being used mass percentage concentration is 4% hydrochloric acid solution pickling, then with the electrical conductivity≤260 μ S/cms of deionized water cyclic washing to filtrating, and drying, pulverizing makes rice hull active carbon/earth silicon/titanic oxide composite.
Embodiment 2
Earlier use the clear water cleaning, drying to 1 kilogram of rice husk, pulverize, cross 100 mesh sieves, the mass percentage concentration that adds 1 kilogram is that 40 ℃ were stirred 1 hour in 10% the hydrochloric acid solution, and washing is neutrality extremely, obtains the pickling powdered rice hulls.In the pickling powdered rice hulls, add 25 liters of the NaOH solution of 0.5mol/L, constantly stirring down, the soda boiling temperature maintenance is at 50 ℃, and the insulation soda boiling obtained the mixed serum of rice husk and sodium metasilicate composition in 2 hours.Under constantly stirring, in the mixed serum that the rice husk and the sodium metasilicate of gained are formed, add the TiCl of 0.5mol/L again
4Solution, reaction temperature remain on 45 ℃, the pH value of conditioned reaction system then, and when reaction system pH is adjusted to 7.5, TiCl
4The solution adding finishes, and continues to stir insulation slaking 0.5 hour; Filter, with the deionized water cyclic washing to the electrical conductivity≤260 μ S/cm that filtrate, with the filter cake of gained 70 ℃ of vacuum drying 5 hours; Pulverize, make rice husk/earth silicon/titanic oxide composite.Again with the rice husk/earth silicon/titanic oxide composite of gained under nitrogen atmosphere, in 300 ℃ of roastings 2 hours, naturally cool to room temperature, make rice hull carbon/earth silicon/titanic oxide composite.In the rice hull carbon/earth silicon/titanic oxide composite of gained, add mass percentage concentration again and be 30% ZnCl
2The aqueous solution stirs, and wherein the mass ratio of composite and zinc chloride is 0.2:1, floods 12 hours, and dry back in 400 ℃ of activation 1 hour, naturally cools to room temperature and obtains activation products under nitrogen atmosphere.At last the activation products of gained being used mass percentage concentration is 20% hydrochloric acid solution pickling, then with the electrical conductivity≤260 μ S/cms of deionized water cyclic washing to filtrating, and drying, pulverizing makes rice hull active carbon/silica
/Composite titania material.
Embodiment 3
Earlier use the clear water cleaning, drying to 1 kilogram of rice husk, pulverize, cross 200 mesh sieves, the mass percentage concentration that adds 5 kilograms is that 70 ℃ were stirred 5 hours in 5% the hydrochloric acid solution, and washing is neutrality extremely, obtains the pickling powdered rice hulls.In the pickling powdered rice hulls, add 12.5 liters of the NaOH solution of 2mol/L, constantly stirring down, the soda boiling temperature maintenance is at 80 ℃, and the insulation soda boiling obtained the mixed serum of rice husk and sodium metasilicate composition in 6 hours.Under constantly stirring, in the mixed serum that the rice husk and the sodium metasilicate of gained are formed, add the TiCl of 2.5mol/L again
4Solution, reaction temperature remain on 75 ℃, the pH value of conditioned reaction system then, and when reaction system pH is adjusted to 7, TiCl
4The solution adding finishes, and continues to stir insulation slaking 2 hours; Filter, with the deionized water cyclic washing to the electrical conductivity≤260 μ S/cm that filtrate, with the filter cake of gained 120 ℃ of vacuum drying 10 hours; Pulverize, make rice husk/earth silicon/titanic oxide composite.Again with the rice husk/earth silicon/titanic oxide composite of gained under nitrogen atmosphere, in 450 ℃ of roastings 5 hours, naturally cool to room temperature, make rice hull carbon/earth silicon/titanic oxide composite.In the rice hull carbon/earth silicon/titanic oxide composite of gained, add mass percentage concentration again and be 50% ZnCl
2The aqueous solution stirs, and wherein the mass ratio of composite and zinc chloride is 0.5:1, floods 18 hours, and dry back in 600 ℃ of activation 3 hours, naturally cools to room temperature and obtains activation products under nitrogen atmosphere.At last the activation products of gained being used mass percentage concentration is 10% hydrochloric acid solution pickling, then with the electrical conductivity≤260 μ S/cms of deionized water cyclic washing to filtrating, and drying, pulverizing makes rice hull active carbon/earth silicon/titanic oxide composite.
Embodiment 4
Earlier use the clear water cleaning, drying to 1 kilogram of rice husk, pulverize, cross 150 mesh sieves, the mass percentage concentration that adds 4 kilograms is that 60 ℃ were stirred 3 hours in 7% the hydrochloric acid solution, and washing is neutrality extremely, obtains the pickling powdered rice hulls.In the pickling powdered rice hulls, add 11.1 liters of the NaOH solution of 1.5mol/L, constantly stirring down, the soda boiling temperature maintenance is at 70 ℃, and the insulation soda boiling obtained the mixed serum of rice husk and sodium metasilicate composition in 5 hours.Under constantly stirring, in the mixed serum that the rice husk and the sodium metasilicate of gained are formed, add the TiCl of 2mol/L again
4Solution, reaction temperature remain on 55 ℃, the pH value of conditioned reaction system then, and when reaction system pH is adjusted to 6, TiCl
4The solution adding finishes, and continues to stir insulation slaking 1.5 hours; Filter, with the deionized water cyclic washing to the electrical conductivity≤260 μ S/cm that filtrate, with the filter cake of gained 110 ℃ of vacuum drying 8 hours; Pulverize, make rice husk/earth silicon/titanic oxide composite.Again with the rice husk/earth silicon/titanic oxide composite of gained under nitrogen atmosphere, in 400 ℃ of roastings 2 hours, naturally cool to room temperature, make rice hull carbon/earth silicon/titanic oxide composite.In the rice hull carbon/earth silicon/titanic oxide composite of gained, add mass percentage concentration again and be 35% ZnCl
2The aqueous solution stirs, and wherein the mass ratio of composite and zinc chloride is 0.3:1, floods 18 hours, and dry back in 550 ℃ of activation 2 hours, naturally cools to room temperature under nitrogen atmosphere.At last the activation products of gained being used mass percentage concentration is 15% hydrochloric acid solution pickling, then with the electrical conductivity≤260 μ S/cms of deionized water cyclic washing to filtrating, and drying, pulverizing makes rice hull active carbon/earth silicon/titanic oxide composite.
Comparative example 1
In comparative example 1,, be about to " use the clear water cleaning, drying to 1 kilogram of rice husk earlier; pulverize, cross 200 mesh sieves, the mass percentage concentration that adds 5 kilograms is that 70 ℃ were stirred 5 hours; washing obtains the pickling powdered rice hulls to neutral in 5% the hydrochloric acid solution " this step deletion with the rice husk pickling process among the embodiment 3 deletion, other operations are all identical with embodiment 3, and the concrete operations step is following: elder generation is clean with clear water 1 kilogram of rice husk; Drying is pulverized, and crosses 200 mesh sieves, obtains powdered rice hulls; In powdered rice hulls, add 12.5 liters of the NaOH solution of 2mol/L, constantly stirring down, the soda boiling temperature maintenance is at 80 ℃, and the insulation soda boiling obtained the mixed serum of rice husk and sodium metasilicate composition in 6 hours.Under constantly stirring, in the mixed serum that the rice husk and the sodium metasilicate of gained are formed, add the TiCl of 2.5mol/L again
4Solution, reaction temperature remain on 75 ℃, when reaction system pH is adjusted to 6.5, and TiCl
4The solution adding finishes, and continues to stir insulation slaking 2 hours; Filter, with the deionized water cyclic washing to the electrical conductivity≤260 μ S/cm that filtrate, with the filter cake of gained 120 ℃ of vacuum drying 10 hours; Pulverize, make rice husk/earth silicon/titanic oxide composite.Again with the rice husk/earth silicon/titanic oxide composite of gained under nitrogen atmosphere, in 450 ℃ of roastings 5 hours, naturally cool to room temperature, make rice hull carbon/earth silicon/titanic oxide composite.In the rice hull carbon/earth silicon/titanic oxide composite of gained, add mass percentage concentration again and be 50% ZnCl
2The aqueous solution stirs, and wherein the mass ratio of composite and zinc chloride is 0.5:1, floods 18 hours, and dry back in 600 ℃ of activation 3 hours, naturally cools to room temperature and obtains activation products under nitrogen atmosphere.At last the activation products of gained being used mass percentage concentration is 10% hydrochloric acid solution pickling, then with the electrical conductivity≤260 μ S/cms of deionized water cyclic washing to filtrating, and drying, pulverizing makes rice hull active carbon/earth silicon/titanic oxide composite.
Comparative example 2
In comparative example 2; With the rice husk among the embodiment 4/earth silicon/titanic oxide composite under nitrogen atmosphere in 400 ℃ of roastings 2 hours; Naturally cool to room temperature, make this operation deletion of rice hull carbon/earth silicon/titanic oxide composite, other operations are all identical with embodiment 3.
Comparative example 3
In comparative example 3, the rice husk pickling process of " use the clear water cleaning, drying to 1 kilogram of rice husk; pulverize, cross 200 mesh sieves, the mass percentage concentration that adds 5 kilograms is in 5% the hydrochloric acid solution; 80 ℃ were stirred 5 hours, and washing obtains the pickling powdered rice hulls to neutral " among the embodiment 3 and " with the rice husk/earth silicon/titanic oxide composite of gained under nitrogen atmosphere; in 450 ℃ of roastings 5 hours; naturally cool to room temperature, make rice hull carbon/earth silicon/titanic oxide composite " step to be deleted, other operations are all identical with embodiment 3.
Carry out the photocatalytic activity evaluation in the face of rice hull active carbon/earth silicon/titanic oxide composite down, result of the test is as shown in table 1.
Rice hull active carbon/earth silicon/titanic oxide the composite that in the photochemical reaction appearance, adds 0.2 gram; The reactive red M-2B solution that adds 500 milliliters of 20mg/L again open to stir and feeds from the bottom air of flow 0.02L/min, opens uviol lamp (power 15W, wavelength 254nm); Reacting took a sample after 4 hours places centrifuge tube to centrifugalize; Get supernatant liquor and test, under its maximum absorption wavelength, measure solution absorbency through spectrophotometer, degradation rate is calculated as follows:
ηFor the dyestuff degradation rate (
%);
A 0,
A tBe respectively the degraded before,
tDye solution absorbance after time;
C 0,
C tBe respectively the degraded before,
tDyes concentration after time (mg/L).
Can find out that by table 1 photocatalytic activity of rice hull active carbon/earth silicon/titanic oxide composite that the present invention is prepared significantly improves.
The photocatalysis test of table 1 rice hull active carbon/earth silicon/titanic oxide composite
| Title | Dyestuff degradation rate (%) |
| The pure titinium dioxide P25 of company (German Degussa) | 70.69 |
| Embodiment 1 | 91.23 |
| Embodiment 2 | 92.88 |
| Embodiment 3 | 97.67 |
| Embodiment 4 | 93.36 |
| Comparative example 1 | 78.44 |
| Comparative example 2 | 75.22 |
| Comparative example 3 | 73.75 |
Claims (1)
1. the preparation method of rice hull active carbon/earth silicon/titanic oxide composite is characterized in that comprising the steps:
(1) preliminary treatment of rice husk:, pulverize with rice husk clear water cleaning, drying; Cross 100 ~ 250 mesh sieves, the adding mass percentage concentration is 3 ~ 10% hydrochloric acid, and the mass ratio of rice husk and hydrochloric acid solution is 0.1 ~ 1:1; Under 40 ~ 85 ℃ of temperature, stirred 1 ~ 7 hour, be washed to neutrality, obtain the pickling powdered rice hulls;
(2) soda boiling: the NaOH solution that in said pickling powdered rice hulls, adds 0.5-3mol/L; Wherein the mass ratio of pickling powdered rice hulls and NaOH is 0.5 ~ 2:1; Constantly stir down the soda boiling temperature maintenance at 50 ~ 95 ℃, and insulation soda boiling 2 ~ 8 hours, obtaining the mixed serum of rice husk and sodium metasilicate composition;
(3) preparation of rice husk/earth silicon/titanic oxide precursor: the TiCl that under constantly stirring, in said mixed serum, adds 0.5-3.5mol/L earlier
4Solution, reaction temperature remain on 45 ~ 90 ℃; TiCl when reaction system pH is adjusted to 5.5 ~ 7.5
4The solution adding finishes, and continues to stir insulation slaking 0.5 ~ 3 hour; At last with the dope filtration of gained, with the electrical conductivity≤260 μ S/cms of deionized water cyclic washing, the filter cake of gained 70 ~ 140 ℃ of vacuum drying 5 ~ 12 hours, is pulverized to filtrating, make rice husk/earth silicon/titanic oxide composite;
(4) charing: said rice husk/earth silicon/titanic oxide composite under nitrogen atmosphere, in 300 ~ 550 ℃ of roastings 2 ~ 6 hours, is naturally cooled to room temperature, make rice hull carbon/earth silicon/titanic oxide composite;
(5) activation: it is 30 ~ 60% ZnCl that said rice hull carbon/earth silicon/titanic oxide composite is immersed in mass percentage concentration
2Stir in the aqueous solution, wherein composite and ZnCl
2Mass ratio be 0.2 ~ 0.8:1, dip time is 12 ~ 24 hours, dry back in 400 ~ 650 ℃ of activation 1 ~ 4 hour, naturally cools to room temperature and obtains activation products under nitrogen atmosphere;
(6) post processing: it is 4 ~ 20% chlorohydric acid pickling that said activation products are used mass percentage concentration earlier; Then with the electrical conductivity≤260 μ S/cms of deionized water cyclic washing to filtrating; Drying is pulverized, and makes rice hull active carbon/earth silicon/titanic oxide composite.
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| 缪应纯等.以稻壳为模板合成Co-TiO2-SiO2光催化降解染料.《材料导报》.2010,第24卷185-191. * |
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