CN104084223A - Magnetically-separatable ferriferrous oxide/silver chloride photocatalyst and preparation method thereof - Google Patents

Magnetically-separatable ferriferrous oxide/silver chloride photocatalyst and preparation method thereof Download PDF

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CN104084223A
CN104084223A CN201410226373.0A CN201410226373A CN104084223A CN 104084223 A CN104084223 A CN 104084223A CN 201410226373 A CN201410226373 A CN 201410226373A CN 104084223 A CN104084223 A CN 104084223A
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photochemical catalyst
iron tetroxide
chloride
silver chlorate
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原弘
刘泽泞
刘永成
蔡木锦
徐飘飘
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Huazhong Agricultural University
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    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
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Abstract

The invention discloses a magnetically-separatable ferriferrous oxide/silver chloride photocatalyst and a preparation method thereof. The photocatalyst is composed of silver chloride and ferriferrous oxide, silver chloride is supported by the surface of ferriferrous oxide, and in the photocatalyst, ferriferrous oxide accounts for 20-40% by specific gravity of the photocatalyst. The preparation method comprises: respectively dissolving ferric chloride, ferrous chloride and silver nitrate in water, so as to prepare a ferric chloride solution, a ferrous chloride solution and a silver nitrate solution for usage; mixing the ferric chloride solution and the ferrous chloride solution under a constant-temperature condition, so as to obtain a reaction mixed solution containing ferriferrous oxide; and slowly dropwise adding the silver nitrate solution into the reaction mixed solution, so as to prepare the magnetically-separatable ferriferrous oxide/silver chloride photocatalyst. When being used to degrade organic dye wastewater, the light-responsive ferriferrous oxide/silver chloride photocatalyst exhibits good photocatalytic activity and stability compared with silver chloride, and also the photocatalyst has the magnetically separatable characteristic.

Description

There is tri-iron tetroxide/silver chlorate photochemical catalyst of Magnetic Isolation and preparation method thereof
Technical field
The present invention relates to photochemical catalyst field, refer to particularly a kind of tri-iron tetroxide/silver chlorate photochemical catalyst with Magnetic Isolation and preparation method thereof.
Background technology
Be accompanied by industrial expansion, environmental pollution has become the significant problem that survival and development of mankind need to solve, and the health that wherein water pollution directly threatens the mankind especially, therefore how the pollutant in efficient degradation water body just becomes the problem that whole world scientist need to capture.Compared with traditional water pollutant treatment technology, Photocatalitic Technique of Semiconductor has efficiently, low-carbon (LC), environmental protection, low toxicity, the advantage such as with low cost, particularly exploitation in recent years a series of have visible light-responded photochemical catalyst and make this technology have great application prospect utilizing in sunshine processing environment pollutant, and this class material also becomes the focus of photocatalysis research field.
The silver salt class materials such as AgCl are the common visible light-responded catalysis materials that has, although these materials have higher Photocatalytic activity to water pollutant under visible ray illumination condition, but they are Shortcomings aspect post processing and recycling, for example need high speed centrifugation, add precipitating reagent etc., be unfavorable for practical application, and carry out functional modification and obtain Magnetic Isolation function and just can address this problem thering is visible light-responded photochemical catalyst.
Summary of the invention
Technical problem to be solved by this invention is just to provide a kind of tri-iron tetroxide/silver chlorate photochemical catalyst with Magnetic Isolation and preparation method thereof, has solved the silver salt class catalysis materials such as existing silver chlorate and has been difficult for the problem reclaiming.
For solving the problems of the technologies described above, a kind of tri-iron tetroxide/silver chlorate photochemical catalyst with Magnetic Isolation provided by the invention, described catalyst is made up of silver chlorate and tri-iron tetroxide, and described silver chlorate loads on the surface of tri-iron tetroxide.
Further, in described photochemical catalyst, the percentage by weight that tri-iron tetroxide accounts for photochemical catalyst is 10～20%.
The present invention also provides a kind of preparation method of tri-iron tetroxide/silver chlorate photochemical catalyst with Magnetic Isolation, comprises the following steps:
1) by iron chloride, frerrous chloride, silver nitrate difference solution water, be prepared into ferric chloride solution, solution of ferrous chloride and liquor argenti nitratis ophthalmicus, for subsequent use;
2) ferric chloride solution and solution of ferrous chloride are placed in to mixing and stirring under the constant temperature of 65～75 DEG C; Add sodium hydrate aqueous solution highly basic to regulate pH to 6.5～7.0, and still aging at 65～75 DEG C of constant temperature, obtain the reaction mixture that contains tri-iron tetroxide; Ageing contributes to obtain ferroferric oxide nano granules.Wherein, under the condition of 70 DEG C, ageing can allow frerrous chloride and iron chloride fully be hydrolyzed for 1 hour.
3) to step 2) slowly drip liquor argenti nitratis ophthalmicus in the reaction mixture that obtains, fully stir, lucifuge leaves standstill 1～3h; Obtain tri-iron tetroxide/silver chlorate photochemical catalyst aqueous solution, then by tri-iron tetroxide/silver chlorate photochemical catalyst aqueous solution aqueous solution washing, dry, obtain tri-iron tetroxide/silver chlorate photochemical catalyst.Described tri-iron tetroxide/silver chlorate photochemical catalyst is that in silver nitride precipitation generative process, polymerization forms aggregate.
Further, described step 1) in, the mol ratio of iron chloride, frerrous chloride and silver nitrate is 1 ︰ 1～2 ︰ 5～40.
Again further, described step 1) in, the mol ratio of iron chloride, frerrous chloride and silver nitrate is: 1 ︰ 1 ︰ 20.
Again further, the concentration of described sodium hydrate aqueous solution is 0.1mol/L.Because the mixed solution of iron chloride and frerrous chloride is acid, but generating tri-iron tetroxide need to carry out approaching in neutral environment, so with the sodium hydroxide solution adjusting pH to 6.5 of 0.1mol/L, the reason of selecting sodium hydroxide solution to make conditioning agent is that the material in NaOH and system can not generate precipitated impurities, and sodium hydroxide solution cost is lower, regulate pH processing ease.
When the mol ratio of iron chloride, frerrous chloride and silver nitrate is: when 1 ︰ 1 ︰ 20, in reaction mixture, slowly drip after liquor argenti nitratis ophthalmicus, in solution, Ag +︰ Cl -content ratio is 4 ︰ 1.Due to the tri-iron tetroxide surface band negative electricity (ξ electromotive force-1.23mV) generating, so the Ag of positively charged +ion is easily adsorbed onto tri-iron tetroxide surface and Cl -, can there is particle aggregation in ion generation precipitation reaction, finally form micron-sized particle in this process.
Principle of the present invention:
In the present invention, magnetic Fe 3o 4can carry out compoundly with photochemical catalyst, realize the recycling to photochemical catalyst by externally-applied magnetic field, for solving, the problem of AgCl in recycling be significant.Utilize the prepared Fe of equation (1) 3o 4in magnetic-particle solution, contain abundant chlorion, silver ion is added after this solution to magnetic Fe 3o 4particle can be carried out enrichment silver ion and be formed silver nitride precipitation by electrostatic attraction, produces the compound of tri-iron tetroxide and silver chlorate, and this process is without by Fe 3o 4carry out purifying, also do not need to add any coating material.
What the photochemical catalyst obtaining by the method just had both the photocatalytic activity of silver chlorate and tri-iron tetroxide can Magnetic Isolation feature, can solve a difficult problem for AgCl recycling.
FeCl 2+ 2FeCl 3+ 8OH -=Fe 3o 4↓+4H 2o+8Cl -equation (1)
Beneficial effect of the present invention is:
1, photochemical catalyst of the present invention has feature that can Magnetic Isolation, and when adding magnet, described photochemical catalyst can be fast by attraction in 1min, and solution becomes clarification, shows that photochemical catalyst has magnetic.Although silver chlorate loads on the surface of tri-iron tetroxide, silver chlorate can not make the magnetic of tri-iron tetroxide disappear.
2, the present invention has visible light-responded tri-iron tetroxide/silver chlorate photochemical catalyst in the time of degrading organic dye waste water, compared with only thering is visible light-responded silver chlorate photochemical catalyst, except showing good photocatalytic activity and stability, this photochemical catalyst also has characteristic that can Magnetic Isolation simultaneously.
3, the invention provides a kind of environmental protection, preparation quickly and easily has the method for tri-iron tetroxide/silver chlorate photochemical catalyst of Magnetic Isolation, both can be used for laboratory operation, is conducive to again large-scale industrial production.
4, chlorion is the key factor of the stable existence of ferriferrous oxide nano colloidal sol, cause area load to have the tri-iron tetroxide of silver chlorate to assemble adding after silver ion because meeting generates silver nitride precipitation, form irregular, particle diameter and distribute from nanometer to micron-sized particle.The present invention is the regulation and control for pattern without price modification any surfactant etc., can simplify preparation process, make synthetic method more efficient, green.
Brief description of the drawings
Fig. 1 is transmission electron microscope (TEM) photo of tri-iron tetroxide/silver chlorate photochemical catalyst with Magnetic Isolation of the present invention.
Fig. 2 is X-ray diffraction (XRD) figure of tri-iron tetroxide/silver chlorate photochemical catalyst with Magnetic Isolation of the present invention.
Fig. 3 is saturated vibrations sample magnetometer (VSM) test curve of tri-iron tetroxide/silver chlorate photochemical catalyst with Magnetic Isolation of the present invention.
Fig. 4 is the curve map of tri-iron tetroxide/silver chlorate photochemical catalyst degradating organic dye rhodamine B under all band simulated solar illumination condition with Magnetic Isolation of the present invention.
Fig. 5 be tri-iron tetroxide/silver chlorate photochemical catalyst with Magnetic Isolation of the present invention (in building-up process, Ag +︰ Cl -content ratio is 4 ︰ 1) photocatalytic degradation rhodamine B cyclic test curve map and with the contrast of pure silver chlorate.
Fig. 6 is that embodiment 1～4 prepares and has tri-iron tetroxide/silver chlorate photochemical catalyst of Magnetic Isolation and other three kinds of mass degradation rhodamine B cyclic test curve maps and the contrast with pure silver chlorate thereof.
Detailed description of the invention
In order to explain better the present invention, further illustrate main contents of the present invention below in conjunction with specific embodiment, but content of the present invention is not only confined to following examples.
Embodiment 1
A preparation method with tri-iron tetroxide/silver chlorate photochemical catalyst of Magnetic Isolation, comprises the following steps:
1) take 2.982g FeCl 24H 2o is dissolved in 100mL deionized water, takes 8.150gFeCl 36H 2o is dissolved in 100mL deionized water, takes 4.247g AgNO 3be dissolved in 250mL deionized water, be prepared into the ferric chloride solution that molar concentration is 0.3mol/L (48.66g/L), solution of ferrous chloride and 0.1mol/L (16.98g/L) liquor argenti nitratis ophthalmicus of 0.15mol/L (19.0g/L), for subsequent use;
2) take mixing and stirring under the constant temperature that 2mL ferric chloride solution and 4mL solution of ferrous chloride be placed in 70 DEG C; The sodium hydrate aqueous solution that slowly drips 0.1mol/L (4g/L) regulates pH to 6.5, and under the constant temperature of 70 DEG C still aging 1h, obtain reaction mixture;
3) to step 2) slowly drip 120mL0.1mol/L (16.98g/L) liquor argenti nitratis ophthalmicus in the reaction mixture that obtains, in solution, Ag +︰ Cl -content ratio is 4 ︰ 1, fully stirs, and lucifuge leaves standstill 1h; Obtain tri-iron tetroxide/silver chlorate photochemical catalyst aqueous solution of pitchy, then tri-iron tetroxide/silver chlorate photochemical catalyst aqueous solution is washed, finally smoked 24h 65 DEG C of conditions, obtain having tri-iron tetroxide/silver chlorate photochemical catalyst of Magnetic Isolation.The percentage by weight that tri-iron tetroxide accounts for photochemical catalyst is 10～20%.
As shown in Figure 1, the present embodiment prepares the aggregate that photocatalyst granular polymerization forms, and is of a size of micron order; In the XRD figure of Fig. 2, there is Fe 3o 4with the characteristic peak of AgCl, show that its composition is Fe 3o 4and AgCl.
Embodiment 2
A preparation method with tri-iron tetroxide/silver chlorate photochemical catalyst of Magnetic Isolation, comprises the following steps:
1) iron chloride, frerrous chloride, silver nitrate are distinguished soluble in water, be prepared into the ferric chloride solution that molar concentration is 0.3mol/L (48.66g/L), solution of ferrous chloride and 0.1mol/L (16.98g/L) liquor argenti nitratis ophthalmicus of 0.15mol/L (19.0g/L), for subsequent use;
2) take mixing and stirring under the constant temperature that 2mL ferric chloride solution and 4mL solution of ferrous chloride be placed in 65 DEG C; The sodium hydrate aqueous solution that slowly drips 0.1mol/L (4g/L) regulates pH to 6.5, and under the constant temperature of 65 DEG C still aging 2h, obtain reaction mixture;
3) to step 2) slowly drip 30mL0.1mol/L (16.98g/L) liquor argenti nitratis ophthalmicus in the reaction mixture that obtains, in solution, Ag +︰ Cl -content ratio is 1 ︰ 1, fully stirs, and lucifuge leaves standstill 1h; Obtain tri-iron tetroxide/silver chlorate photochemical catalyst aqueous solution of pitchy, then tri-iron tetroxide/silver chlorate photochemical catalyst aqueous solution is washed, finally smoked 24h 65 DEG C of conditions, obtain having tri-iron tetroxide/silver chlorate photochemical catalyst of Magnetic Isolation.The percentage by weight that tri-iron tetroxide accounts for photochemical catalyst is 10～20%.
Embodiment 3
A preparation method with tri-iron tetroxide/silver chlorate photochemical catalyst of Magnetic Isolation, comprises the following steps:
1) by iron chloride, frerrous chloride, silver nitrate difference solution water, be prepared into the ferric chloride solution that molar concentration is 0.3mol/L (48.66g/L), solution of ferrous chloride and 0.1mol/L (16.98g/L) liquor argenti nitratis ophthalmicus of 0.15mol/L (19.0g/L), for subsequent use;
2) take mixing and stirring under the constant temperature that 2mL ferric chloride solution and 4mL solution of ferrous chloride be placed in 75 DEG C; The sodium hydrate aqueous solution that slowly drips 0.1mol/L (4g/L) regulates pH to 7.0, and under the constant temperature of 75 DEG C still aging 2h, obtain reaction mixture;
3) to step 2) slowly drip 60mL0.1mol/L (16.98g/L) liquor argenti nitratis ophthalmicus in the reaction mixture that obtains, in solution, Ag +︰ Cl -content ratio is 2 ︰ 1, fully stirs, and lucifuge leaves standstill 1h; Obtain tri-iron tetroxide/silver chlorate photochemical catalyst aqueous solution of pitchy, then tri-iron tetroxide/silver chlorate photochemical catalyst aqueous solution is washed, finally smoked 24h 65 DEG C of conditions, obtain having tri-iron tetroxide/silver chlorate photochemical catalyst of Magnetic Isolation.The percentage by weight that tri-iron tetroxide accounts for photochemical catalyst is 10～20%.
Embodiment 4
A preparation method with tri-iron tetroxide/silver chlorate photochemical catalyst of Magnetic Isolation, comprises the following steps:
1) by iron chloride, frerrous chloride, silver nitrate difference solution water, be prepared into the ferric chloride solution that molar concentration is 0.3mol/L (48.66g/L), solution of ferrous chloride and 0.1mol/L (16.98g/L) liquor argenti nitratis ophthalmicus of 0.15mol/L (19.0g/L), for subsequent use;
2) take mixing and stirring under the constant temperature that 2mL ferric chloride solution and 4mL solution of ferrous chloride be placed in 65 DEG C; The sodium hydrate aqueous solution that slowly drips 0.1mol/L (4g/L) regulates pH to 6.5, and under the constant temperature of 65 DEG C still aging 1h, obtain reaction mixture;
3) to step 2) slowly drip 240mL0.1mol/L (16.98g/L) liquor argenti nitratis ophthalmicus in the reaction mixture that obtains, in solution, Ag +︰ Cl -content ratio is 6 ︰ 1, fully stirs, and lucifuge leaves standstill 1h; Obtain tri-iron tetroxide/silver chlorate compound water solution of pitchy, then tri-iron tetroxide/silver chlorate photochemical catalyst aqueous solution is washed, finally smoked 24h 65 DEG C of conditions, obtain having tri-iron tetroxide/silver chlorate photochemical catalyst of Magnetic Isolation.The percentage by weight that tri-iron tetroxide accounts for photochemical catalyst is 10～20%.
Embodiment 5
A preparation method with tri-iron tetroxide/silver chlorate photochemical catalyst of Magnetic Isolation, comprises the following steps:
1) by iron chloride, frerrous chloride, silver nitrate difference solution water, be prepared into the ferric chloride solution that molar concentration is 0.3mol/L (48.66g/L), solution of ferrous chloride and 0.1mol/L (16.98g/L) liquor argenti nitratis ophthalmicus of 0.15mol/L (19.0g/L), for subsequent use;
2) take mixing and stirring under the constant temperature that 1mL ferric chloride solution and 4mL solution of ferrous chloride be placed in 65 DEG C; The sodium hydrate aqueous solution that slowly drips 0.1mol/L (4g/L) regulates pH to 6.5, and under the constant temperature of 65 DEG C still aging 1h, obtain reaction mixture;
3) to step 2) slowly drip 240mL0.1mol/L (16.98g/L) liquor argenti nitratis ophthalmicus in the reaction mixture that obtains, in solution, Ag +︰ Cl -content ratio is 6 ︰ 1, fully stirs, and lucifuge leaves standstill 1h; Obtain tri-iron tetroxide/silver chlorate photochemical catalyst aqueous solution of pitchy, then tri-iron tetroxide/silver chlorate photochemical catalyst aqueous solution is washed, finally smoked 24h 65 DEG C of conditions, obtain having tri-iron tetroxide/silver chlorate photochemical catalyst of Magnetic Isolation.The percentage by weight that tri-iron tetroxide accounts for photochemical catalyst is 10～20%.
Embodiment 1 is prepared to tri-iron tetroxide/silver chlorate photochemical catalyst with Magnetic Isolation and carry out verification experimental verification
1, tri-iron tetroxide/silver chlorate photochemical catalyst can Magnetic Isolation Performance Detection
As shown in Figure 3, the saturation magnetization of catalyst is 12.2emu/g, and pure tri-iron tetroxide particle saturation magnetization is 80.6emu/g.Although the saturation magnetization of catalyst has largely and weakens compared with pure tri-iron tetroxide, to find as contrasted photo in Fig. 3, catalyst can separate fast under additional magnetic fields from sewage.
2, tri-iron tetroxide/silver chlorate photocatalyst for degrading rhodamine B
Take 50mg tri-iron tetroxide/silver chlorate photochemical catalyst and add 50mL rhodamine B solution (1 × 10 -5molL -1), lucifuge stirs 30min, makes rhodamine B reach adsorption equilibrium at catalyst surface.Use 300W xenon lamp to carry out light-catalyzed reaction as light source, course of reaction continues to stir, and gets 3mL reactant liquor every 2min, centrifugal, the maximum absorbance of getting supernatant UV, visible light spectrophotometric determination solution detects the variation of solution concentration, and after reaction 6min, rhodamine B is completely degraded.
All band simulated solar photocatalytic degradation organic dyestuff rhodamine B tendency chart as shown in Figure 4, compare with tri-iron tetroxide with pure silver chlorate, tri-iron tetroxide/silver chlorate photochemical catalyst shows the advantage of obvious photocatalytic degradation rhodamine B, can fast degradation pollutant, and silver chlorate is can only degrade when 12min approximately 40% rhodamine B of reaction, and tri-iron tetroxide does not show the photocatalytic activity under this reaction condition.Tri-iron tetroxide/silver chlorate photochemical catalyst that as can be seen from Figure 4 prepared by the present invention has efficient photocatalysis performance under visible illumination condition.
Fig. 5 is the comparison diagram of pure silver chlorate and tri-iron tetroxide/silver chlorate photochemical catalyst cyclic test with Magnetic Isolation.Under all band simulated solar illumination condition, tri-iron tetroxide/silver chlorate photochemical catalyst with Magnetic Isolation all can be at 12min by the degraded of organic dyestuff rhodamine B thoroughly.Silver chlorate not only catalytic activity than composite catalyst a little less than, simultaneously the ability of pure silver chlorate photocatalytic degradation rhodamine B, also along with recycling occurs obviously to reduce, shows its less stable in photocatalytic degradation pollutant.The photocatalytic activity and the stability that contrast the tri-iron tetroxide/silver chlorate photochemical catalyst with Magnetic Isolation that shows prepared by the present invention by cyclic test are all better, and the recycling that can circulate, has a good application prospect.
3, the recycling of tri-iron tetroxide/silver chlorate photochemical catalyst
Tri-iron tetroxide/silver chlorate the photochemical catalyst that takes respectively 100mg, adds 50mL rhodamine B solution (1 × 10 -5molL -1) in, lucifuge stirs 30min, makes rhodamine B reach adsorption equilibrium at catalyst surface, use 300W xenon lamp to carry out light-catalyzed reaction as light source, course of reaction continues to stir, and gets 3mL reactant liquor every 2min, centrifugal, the maximum absorbance of getting supernatant UV, visible light spectrophotometric determination solution detects the variation of solution concentration, after reaction 12min, reclaims catalyst sample, washing, dry, for photocatalytic degradation rhodamine B test next time, in triplicate.
Tri-iron tetroxide/silver chlorate photochemical catalyst, silver chlorate, tri-iron tetroxide and titanium oxide rhodamine B degradation (method of operating is the same) that embodiment 1～4 is prepared
As shown in Figure 6, all band simulated solar photocatalytic degradation organic dyestuff rhodamine B tendency chart as shown in the figure.Compare with tri-iron tetroxide with pure silver chlorate, and tri-iron tetroxide/silver chlorate photochemical catalyst (in building-up process, Ag +︰ Cl -content ratio is 4 ︰ 1) show the advantage of obvious photocatalytic degradation rhodamine B, can fast degradation pollutant, and silver chlorate is can only degrade when 12min approximately 40% rhodamine B of reaction, and tri-iron tetroxide does not show the photocatalytic activity under this reaction condition.The catalytic activity of other ratio catalyst is also low compared with tri-iron tetroxide/silver chlorate photochemical catalyst.Tri-iron tetroxide/silver chlorate photochemical catalyst (in building-up process, Ag +︰ Cl -content ratio is 4 ︰ 1) show best photocatalytic activity: silver chloride content is too low, and photocatalytic activity is not high; Silver ion adds some metallic silver particles of too much meeting to generate, and suppresses photocatalytic activity thereby can become photo-generated carrier complex centre, thus tri-iron tetroxide/silver chlorate photochemical catalyst (in building-up process, Ag +︰ Cl -content ratio is 4 ︰ 1) activity is the highest.Tri-iron tetroxide/silver chlorate photochemical catalyst that as can be seen from Fig. prepared by the present invention has efficient photocatalysis performance under visible illumination condition.
Other unspecified part is prior art.Although above-described embodiment has been made detailed description to the present invention; but it is only the present invention's part embodiment; instead of whole embodiment, people can also obtain other embodiment according to the present embodiment under without creative prerequisite, and these embodiment belong to protection domain of the present invention.

Claims (6)

1. tri-iron tetroxide/silver chlorate photochemical catalyst with Magnetic Isolation, is characterized in that: described catalyst is made up of silver chlorate and tri-iron tetroxide, described silver chlorate loads on the surface of tri-iron tetroxide.
2. tri-iron tetroxide/silver chlorate photochemical catalyst according to claim 1 with Magnetic Isolation, is characterized in that: in described photochemical catalyst, the percentage by weight that tri-iron tetroxide accounts for photochemical catalyst is 10～20%.
3. a preparation method described in claim 1 with tri-iron tetroxide/silver chlorate photochemical catalyst of Magnetic Isolation, is characterized in that: comprise the following steps:
1) by iron chloride, frerrous chloride, silver nitrate difference solution water, be prepared into ferric chloride solution, solution of ferrous chloride and liquor argenti nitratis ophthalmicus, for subsequent use;
2) ferric chloride solution and solution of ferrous chloride are placed in to mixing and stirring under the constant temperature of 65～75 DEG C; Add sodium hydrate aqueous solution to regulate pH to 6.5～7.0, and still aging under the constant temperature of 65～75 DEG C, obtain the reaction mixture that contains tri-iron tetroxide;
3) to step 2) slowly drip liquor argenti nitratis ophthalmicus in the reaction mixture that obtains, fully stir, lucifuge leaves standstill 1～3h; Obtain tri-iron tetroxide/silver chlorate photochemical catalyst aqueous solution, then by tri-iron tetroxide/silver chlorate photochemical catalyst aqueous solution washing, dry, obtain having tri-iron tetroxide/silver chlorate photochemical catalyst of Magnetic Isolation.
4. the preparation method according to claim 3 with tri-iron tetroxide/silver chlorate photochemical catalyst of Magnetic Isolation, is characterized in that: described step 1) in, the mol ratio of iron chloride, frerrous chloride and silver nitrate is 1 ︰ 1～2 ︰ 5～40.
5. the preparation method according to claim 4 with tri-iron tetroxide/silver chlorate photochemical catalyst of Magnetic Isolation, is characterized in that: described step 1) in, the mol ratio of iron chloride, frerrous chloride and silver nitrate is: 1 ︰ 1 ︰ 20.
6. according to the preparation method of tri-iron tetroxide/silver chlorate photochemical catalyst described in any one in claim 3～5 with Magnetic Isolation, it is characterized in that: the concentration of described sodium hydrate aqueous solution is 0.1mol/L.
CN201410226373.0A 2014-05-27 2014-05-27 Magnetically-separatable ferriferrous oxide/silver chloride photocatalyst and preparation method thereof Pending CN104084223A (en)

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