CN102895980A - Ferro-chrome composite oxide and preparation method and application thereof - Google Patents
Ferro-chrome composite oxide and preparation method and application thereof Download PDFInfo
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- CN102895980A CN102895980A CN201210433318XA CN201210433318A CN102895980A CN 102895980 A CN102895980 A CN 102895980A CN 201210433318X A CN201210433318X A CN 201210433318XA CN 201210433318 A CN201210433318 A CN 201210433318A CN 102895980 A CN102895980 A CN 102895980A
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Abstract
The invention provides a ferro-chrome composite oxide, a preparation method thereof and application thereof. The ferro-chrome composite oxide has a general formula of Fe3-xCrxO4, and X-ray powder obtained through Cu-K alpha-ray measurement is diffracted at angles 2theta of 31 degrees, 36 degrees and 63 degrees and displays characteristic peak. When the ferro-chrome composite oxide serving as a catalyst performs sewage treatment, a pH value of the sewage is not required to be regulated, and the ferro-chrome composite oxide has the advantage of high sewage treatment efficiency; the ferro-chrome composite oxide is a solid catalyst and can be recycled, so that the sewage treatment cost can be reduced; and moreover, the preparation method for the ferro-chrome composite oxide is easy to operate.
Description
Technical field
The present invention relates to a kind of composite oxide of metal, be specifically related to a kind of siderochrome composite oxides, Preparation Method And The Use.
Background technology
In recent years, along with industrial boom, the sewage pollution problem is day by day serious.There is serious harm in the organic substance that contains a large amount of poisonous and harmful difficult degradations in the sewage to health and ecological environment.At present, a kind of effective ways of disposing of sewage are for adopting Fenton reagent to carry out sewage disposal, by all kinds of organic pollutions in the oxidation degradation of sewage of Fenton reagent, thereby make the processed sewage can be recycling.
But, when adopting Fenton reagent to carry out sewage disposal, need before the Fenton's reaction with sulfuric acid the pH of sewage to be adjusted to 3, also need after the reaction with NaOH pH to be adjusted to neutrality.Therefore, this kind processing method need to consume a large amount of sulfuric acid and NaOH, has strengthened cost of sewage disposal.
Summary of the invention
Defective for prior art exists the invention provides a kind of siderochrome composite oxides, and when adopting these siderochrome composite oxides to carry out sewage disposal, the pH value that does not need to regulate sewage has that sewage treating efficiency height, cost are low to reach advantage simple to operate.
The technical solution used in the present invention is as follows:
The invention provides a kind of siderochrome composite oxides, described siderochrome composite oxides have following general formula I:
Fe
3-xCr
xO
4 I；
Wherein, 0＜x＜3.
Preferably, the x value is 0.18,0.47,1.24,1.78,2.33,2.94.
Preferably, the described siderochrome composite oxides X-ray powder diffraction that uses the Cu-K alpha ray to measure is 31 °, 36 °, 63 ° at 2 θ and shows characteristic peak.
Preferably, described siderochrome composite oxides particle diameter is 20-32nm.
The present invention also provides a kind of preparation method of siderochrome composite oxides, may further comprise the steps:
S1 adds entry in the mixture of 16 weight portion NaOH and 7.65 weight portion sodium nitrate, be stirred to solid and all dissolve, and obtains the first mixed solution;
S2 stirs down, and dripping concentration in the mixture of 5.35665 weight portions, six hydrated chromium trichlorides and 0.1-91 weight portion green vitriol is the hydrochloric acid of 0.5-1.5mol/L, and being stirred to solid all dissolves, and obtains the second mixed solution;
S3 under the inert gas environment, heats the second mixed solution after 90-100 ℃, drips the first mixed solution that the S1 preparation obtains to dropwising with the speed of 5-15ml/min;
S4, the reactant liquor that S3 is obtained continue to keep 90-100 ℃ to be cooled to 20-30 ℃ after 2 hours, and centrifugal treating is isolated solid, then uses the washed with de-ionized water solid, and the solid drying after cleaning is namely got described siderochrome composite oxides.
Preferably, among the S1, in described the first mixed solution, the NaOH mass fraction is 0.32-1.6g/ml, and the sodium nitrate mass fraction is 0.153-0.765g/ml;
Among the S2, in described the second mixed solution, six hydrated chromium trichloride mass fractions are 0.107-0.535g/ml, and the green vitriol mass fraction is 0.1-91g/ml.
Preferably, among the S4, drying condition is drying overnight in 100 ℃ the vacuum drying chamber.
The present invention also provides a kind of purposes of siderochrome composite oxides, and described siderochrome composite oxides are used for the catalyst of hydrogen peroxide sewage treatment.
Preferably, described siderochrome composite oxides are specially for the catalyst of hydrogen peroxide sewage treatment:
Described siderochrome composite oxides and hydrogen peroxide are joined in the need sewage to be processed, and 20-30 ℃ was stirred 20 minutes-3 hours.
Preferably, the mol ratio of siderochrome composite oxides and hydrogen peroxide is 1.07～1.78.
Beneficial effect of the present invention is as follows:
The invention provides a kind of siderochrome composite oxides, when adopting these siderochrome composite oxides to carry out sewage disposal as catalyst, the pH value that does not need to regulate sewage has the high advantage of sewage treating efficiency; And the siderochrome composite oxide catalysts is solid, can reuse, so can reduce the cost of sewage disposal; And, also have advantage simple to operate.
Description of drawings
Fig. 1 is the X-ray powder diffraction pattern of the siderochrome composite oxides that prepare of the embodiment of the invention 1;
Fig. 2 is siderochrome composite oxides consumption and the column diagram of processing rear COD of sewage relation in the sewage disposal.
The specific embodiment
Siderochrome composite oxides Preparation Example 1
S1 adds 26ml water in the mixture of 16g NaOH and 7.65g sodium nitrate, be stirred to solid and all dissolve, and obtains the first mixed solution;
S2 stirs down, and dripping concentration in the mixture of 5.35665g six hydrated chromium trichloride 50.2358g green vitriols is the hydrochloric acid of 1.3mol/L, and being stirred to solid all dissolves, and obtains the second mixed solution;
S3, under the inert gas environment, heat the second mixed solution to 96 ℃ after, drip the first mixed solution that the S1 preparation obtains to dropwising with the speed of 11ml/min;
S4, the reactant liquor that S3 is obtained continue to keep 95 ℃ to be cooled to 25 ℃ after 2 hours, and centrifugal treating is isolated solid, then uses the washed with de-ionized water solid, and the solid drying after cleaning is namely got described siderochrome composite oxides.
Prepared siderochrome composite oxides particle diameter is 30nm.
Use 18KWX alpha cellulose a gage of science, at Cu-K α, λ=1.5418A, tube voltage 40kV, tube current 200mA, 10 °/min of sweep speed (10-90 °), step-length is under the test condition of 0.02 °/step product to be carried out XRD to characterize, and obtains X-ray powder diffraction pattern shown in Figure 1, and it is 31 °, 36 °, 63 ° at 2 θ and shows characteristic peak, the XRD characterization result shows that resulting product is Fe
2.33Cr
0.67O
4Reason is: with jade software XRD diffracting spectrum shown in Figure 1 is carried out the phase retrieval.Because there is not Fe in the reference material number of phases quantitative limitation in the PDF card in the jade software
2.33Cr
0.67O
4Phase.Be Fe at qualifications for certain element that exists, Cr, in the situation of O, in several phases that the most probable that retrieves exists, FeCr
2O
4Diffracted ray and the XRD diffracting spectrum of siderochrome composite oxides shown in Figure 1 have reasonable corresponding relation.As seen from Figure 1, three of the diffracting spectrum of siderochrome composite oxides enough and phase FeCr of strong peak energy
2O
4Three diffracted rays (220) (311) corresponding with (440).But, can find out at FeCr
2O
4Diffracted ray (511) locate, have unconspicuous diffraction maximum in the XRD collection of illustrative plates of the siderochrome composite oxides of surveying.This explanation the present invention prepare siderochrome composite oxides and FeCr
2O
4Similar, but be not FeCr
2O
4
Use the U.S. Optima 3300DV ICP of PERKIN ELMER company plasma emission spectrometer, at wavelength working range: 165-782nm, 2 road imaging optical paths are arranged, be furnished with under the condition of SCD detector product is carried out elementary analysis, test result shows Fe: Cr: O=2.33: 0.67: 4.
Siderochrome composite oxides Preparation Example 2
S1 adds 10ml water in the mixture of 16g NaOH and 7.65g sodium nitrate, be stirred to solid and all dissolve, and obtains the first mixed solution;
S2 stirs down, and dripping concentration in the mixture of 5.35665g six hydrated chromium trichloride 87.5422g green vitriols is the hydrochloric acid of 1.2mol/L, and being stirred to solid all dissolves, and obtains the second mixed solution;
S3, under the inert gas environment, heat the second mixed solution to 90 ℃ after, drip the first mixed solution that the S1 preparation obtains to dropwising with the speed of 5ml/min;
S4, the reactant liquor that S3 is obtained continue to keep 92 ℃ to be cooled to 23 ℃ after 2 hours, and centrifugal treating is isolated solid, then uses the washed with de-ionized water solid, and the solid drying after cleaning is namely got described siderochrome composite oxides.
Prepared siderochrome composite oxides particle diameter is 23nm, and structural formula is Fe
2.82Cr
0.18O
4
The X-ray powder diffraction pattern that uses the Cu-K alpha ray to measure is consistent with embodiment 1.
Siderochrome composite oxides Preparation Example 3
S1 adds 50ml water in the mixture of 16g NaOH and 7.65g sodium nitrate, be stirred to solid and all dissolve, and obtains the first mixed solution;
S2 stirs down, and dripping concentration in the mixture of 5.35665g six hydrated chromium trichloride 30.0790g green vitriols is the hydrochloric acid of 1.1mol/L, and being stirred to solid all dissolves, and obtains the second mixed solution;
S3, under the inert gas environment, heat the second mixed solution to 100 ℃ after, drip the first mixed solution that the S1 preparation obtains to dropwising with the speed of 15ml/min;
S4, the reactant liquor that S3 is obtained continue to keep 96 ℃ to be cooled to 27 ℃ after 2 hours, and centrifugal treating is isolated solid, then uses the washed with de-ionized water solid, and the solid drying after cleaning is namely got described siderochrome composite oxides.
Prepared siderochrome composite oxides particle diameter is 25m, and structural formula is Fe
2.53Cr
0.47O
4
The X-ray powder diffraction pattern that uses the Cu-K alpha ray to measure is consistent with embodiment 1.
Siderochrome composite oxides Preparation Example 4
S1 adds 40ml water in the mixture of 16g NaOH and 7.65g sodium nitrate, be stirred to solid and all dissolve, and obtains the first mixed solution;
S2 stirs down, and dripping concentration in the mixture of 5.35665g six hydrated chromium trichloride 7.9311g green vitriols is the hydrochloric acid of 1.5mol/L, and being stirred to solid all dissolves, and obtains the second mixed solution;
S3, under the inert gas environment, heat the second mixed solution to 96 ℃ after, drip the first mixed solution that the S1 preparation obtains to dropwising with the speed of 9ml/min;
S4, the reactant liquor that S3 is obtained continue to keep 100 ℃ to be cooled to 30 ℃ after 2 hours, and centrifugal treating is isolated solid, then uses the washed with de-ionized water solid, and the solid drying after cleaning is namely got described siderochrome composite oxides.
Prepared siderochrome composite oxides particle diameter is 30nm, and structural formula is Fe
1.76Cr
1.24O
4
The X-ray powder diffraction pattern that uses the Cu-K alpha ray to measure is consistent with embodiment 1.Siderochrome composite oxides Preparation Example 5
S1 adds 80ml water in the mixture of 16g NaOH and 7.65g sodium nitrate, be stirred to solid and all dissolve, and obtains the first mixed solution;
S2 stirs down, and dripping concentration in the mixture of 5.35665g six hydrated chromium trichloride 3.8298g green vitriols is the hydrochloric acid of 0.5mol/L, and being stirred to solid all dissolves, and obtains the second mixed solution;
S3, under the inert gas environment, heat the second mixed solution to 92 ℃ after, drip the first mixed solution that the S1 preparation obtains to dropwising with the speed of 13ml/min;
S4, the reactant liquor that S3 is obtained continue to keep 90 ℃ to be cooled to 20 ℃ after 2 hours, and centrifugal treating is isolated solid, then uses the washed with de-ionized water solid, and the solid drying after cleaning is namely got described siderochrome composite oxides.
Prepared siderochrome composite oxides particle diameter is 23nm, and structural formula is Fe
1.22Cr
1.78O
4
The X-ray powder diffraction pattern that uses the Cu-K alpha ray to measure is consistent with embodiment 1.
Siderochrome composite oxides Preparation Example 6
S1 adds 23ml water in the mixture of 16g NaOH and 7.65g sodium nitrate, be stirred to solid and all dissolve, and obtains the first mixed solution;
S2 stirs down, and dripping concentration in the mixture of 5.35665g six hydrated chromium trichloride 1.6068g green vitriols is the hydrochloric acid of 0.8mol/L, and being stirred to solid all dissolves, and obtains the second mixed solution;
S3, under the inert gas environment, heat the second mixed solution to 93 ℃ after, drip the first mixed solution that the S1 preparation obtains to dropwising with the speed of 13ml/min;
S4, the reactant liquor that S3 is obtained continue to keep 95 ℃ to be cooled to 24 ℃ after 2 hours, and centrifugal treating is isolated solid, then uses the washed with de-ionized water solid, and the solid drying after cleaning is namely got described siderochrome composite oxides.
Prepared siderochrome composite oxides particle diameter is 27nm, and structural formula is Fe
0.67Cr
2.33O
4
The X-ray powder diffraction pattern that uses the Cu-K alpha ray to measure is consistent with embodiment 1.Siderochrome composite oxides Preparation Example 7
S1 adds 48ml water in the mixture of 16g NaOH and 7.65g sodium nitrate, be stirred to solid and all dissolve, and obtains the first mixed solution;
S2 stirs down, and dripping concentration in the mixture of 5.35665g six hydrated chromium trichloride 0.1141g green vitriols is the hydrochloric acid of 0.7mol/L, and being stirred to solid all dissolves, and obtains the second mixed solution;
S3, under the inert gas environment, heat the second mixed solution to 92 ℃ after, drip the first mixed solution that the S1 preparation obtains to dropwising with the speed of 9ml/min;
S4, the reactant liquor that S3 is obtained continue to keep 98 ℃ to be cooled to 28 ℃ after 2 hours, and centrifugal treating is isolated solid, then uses the washed with de-ionized water solid, and the solid drying after cleaning is namely got described siderochrome composite oxides.
Prepared siderochrome composite oxides particle diameter is 33nm, and structural formula is Fe
0.06Cr
2.94O
4
The X-ray powder diffraction pattern that uses the Cu-K alpha ray to measure is consistent with embodiment 1.
Sewage water treatment method embodiment 1
Be 1.07 Fe with mol ratio
2.33Cr
0.67O
4Join in the need sewage to be processed with hydrogen peroxide, 26 ℃ were stirred 2.5 hours.The sewage color obviously becomes clear after processing.
Sewage water treatment method embodiment 2
Be 1.78 Fe with mol ratio
2.82Cr
0.18O
4Join in the need sewage to be processed with hydrogen peroxide, 29 ℃ were stirred 1.5 hours.The sewage color obviously becomes clear after processing.
Sewage water treatment method embodiment 3
Be 1.23 Fe with mol ratio
2.53Cr
0.47O
4Join in the need sewage to be processed with hydrogen peroxide, 21 ℃ were stirred 2 hours.The sewage color obviously becomes clear after processing.
Sewage water treatment method embodiment 4
Be 1.35 Fe with mol ratio
1.76Cr
1.24O
4Join in the need sewage to be processed with hydrogen peroxide, 28 ℃ were stirred 2 hours.The sewage color obviously becomes clear after processing.
Sewage water treatment method embodiment 5
Be 1.68 Fe with mol ratio
1.22Cr
1.78O
4Join in the need sewage to be processed with hydrogen peroxide, 25 ℃ were stirred 1 hour.The sewage color obviously becomes clear after processing.
Sewage water treatment method embodiment 6
Be 1.21 Fe with mol ratio
0.67Cr
2.33O
4Join in the need sewage to be processed with hydrogen peroxide, 30 ℃ were stirred 3 hours.The sewage color obviously becomes clear after processing.
Sewage water treatment method embodiment 7
Be 1.13 Fe with mol ratio
0.06Cr
2.94O
4Join in the need sewage to be processed with hydrogen peroxide, 20 ℃ were stirred 20 minutes.The sewage color obviously becomes clear after processing.
Test example 1
This test example is used for investigating the consumption of siderochrome composite oxides to the impact of wastewater treatment efficiency.
Get 50 milliliters of Shandong insecticide factory raw sewerages, add the siderochrome composite oxides that the embodiment 1 of 25ul hydrogen peroxide and investigation amount prepares in this sewage, stir after 1 hour, sewage color after measuring COD value, the total dissolved solidss TDS value of sewage and observing processing, result of the test sees Table 1.Wherein, the COD of sewage value is measured according to GB GB11914-1989 method; The TDS value is according to gravimetric detemination.
Table 1
Can find out from table 1 and Fig. 2, when adopting hydrogen peroxide that sewage is processed, add the siderochrome composite oxides and can improve sewage treating efficiency, effectively reduce COD, TDS and the Colority of Sewage Water of sewage; And siderochrome composite oxides use amount is larger, and wastewater treatment efficiency is better.Possible cause is: this catalyst is a kind of siderochrome composite oxides, can make decomposing hydrogen dioxide solution produce hydroxyl radical free radical OH, because OH has very strong oxidisability, energy oxidation majority of organic pollutants is so can play the effect of sewage purification.
Other siderochrome composite oxides of the present invention have also been carried out identical experiment, and experimental result is similar.
The above only is preferred embodiment of the present invention; should be pointed out that for those skilled in the art, under the prerequisite that does not break away from the principle of the invention; can also make some improvements and modifications, these improvements and modifications also should be looked protection scope of the present invention.
Claims (10)
1. siderochrome composite oxides is characterized in that, described siderochrome composite oxides have following general formula I:
Fe
3-xCr
xO
4 I；
Wherein, 0＜x＜3.
2. siderochrome composite oxides according to claim 1 is characterized in that, the x value is 0.18,0.47,1.24,1.78,2.33,2.94.
3. siderochrome composite oxides according to claim 1 is characterized in that, the X-ray powder diffraction that described siderochrome composite oxides use the Cu-K alpha ray to measure is 31 °, 36 °, 63 ° at 2 θ and shows characteristic peak.
4. each described siderochrome composite oxides is characterized in that according to claim 1-3, and described siderochrome composite oxides particle diameter is 20-32nm.
5. the preparation method of each described siderochrome composite oxides of claim 1-4 is characterized in that, may further comprise the steps:
S1 adds entry in the mixture of 16 weight portion NaOH and 7.65 weight portion sodium nitrate, be stirred to solid and all dissolve, and obtains the first mixed solution;
S2 stirs down, and dripping concentration in the mixture of 5.35665 weight portions, six hydrated chromium trichlorides and 0.1-91 weight portion green vitriol is the hydrochloric acid of 0.5-1.5mol/L, and being stirred to solid all dissolves, and obtains the second mixed solution;
S3 under the inert gas environment, heats the second mixed solution after 90-100 ℃, drips the first mixed solution that the S1 preparation obtains to dropwising with the speed of 5-15ml/min;
S4, the reactant liquor that S3 is obtained continue to keep 90-100 ℃ to be cooled to 20-30 ℃ after 2 hours, and centrifugal treating is isolated solid, then uses the washed with de-ionized water solid, and the solid drying after cleaning is namely got described siderochrome composite oxides.
6. preparation method according to claim 5 is characterized in that, among the S1, in described the first mixed solution, the NaOH mass fraction is 0.32-1.6g/ml, and the sodium nitrate mass fraction is 0.153-0.765g/ml;
Among the S2, in described the second mixed solution, six hydrated chromium trichloride mass fractions are 0.107-0.535g/ml, and the green vitriol mass fraction is 0.1-91g/ml.
7. preparation method according to claim 5 is characterized in that, among the S4, drying condition is drying overnight in 100 ℃ the vacuum drying chamber.
8. the purposes of each described siderochrome composite oxides of claim 1-4 is characterized in that, described siderochrome composite oxides are used for the catalyst of hydrogen peroxide sewage treatment.
9. purposes according to claim 8 is characterized in that, the catalyst that described siderochrome composite oxides are used for the hydrogen peroxide sewage treatment is specially:
Described siderochrome composite oxides and hydrogen peroxide are joined in the need sewage to be processed, and 20-30 ℃ was stirred 20 minutes-3 hours.
10. purposes according to claim 9 is characterized in that, the mol ratio of siderochrome composite oxides and hydrogen peroxide is 1.07～1.78.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105107522A (en) * | 2015-08-28 | 2015-12-02 | 威水星空（北京）环境技术有限公司 | Ferro-manganese composite oxide catalyst and preparation method thereof |
| CN107265515A (en) * | 2017-07-31 | 2017-10-20 | 苏州热工研究院有限公司 | A kind of High Content Chromium doped ferroferric oxide raw powder's production technology |
| CN115571966A (en) * | 2022-09-29 | 2023-01-06 | 暨南大学 | Hexavalent chromium removing method based on adjustment of iron circulation in green rust and preparation method of reduced layered iron-chromium oxide |
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| PL193145B1 (en) * | 2001-05-11 | 2007-01-31 | Politechnika Szczecinska | Novel phases of homogenous solid solution type in a ternary system of vanadium, iron and chromium oxides and method of obtaining them |
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| PL193145B1 (en) * | 2001-05-11 | 2007-01-31 | Politechnika Szczecinska | Novel phases of homogenous solid solution type in a ternary system of vanadium, iron and chromium oxides and method of obtaining them |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105107522A (en) * | 2015-08-28 | 2015-12-02 | 威水星空（北京）环境技术有限公司 | Ferro-manganese composite oxide catalyst and preparation method thereof |
| CN107265515A (en) * | 2017-07-31 | 2017-10-20 | 苏州热工研究院有限公司 | A kind of High Content Chromium doped ferroferric oxide raw powder's production technology |
| CN115571966A (en) * | 2022-09-29 | 2023-01-06 | 暨南大学 | Hexavalent chromium removing method based on adjustment of iron circulation in green rust and preparation method of reduced layered iron-chromium oxide |
| CN115571966B (en) * | 2022-09-29 | 2024-05-31 | 暨南大学 | Hexavalent chromium removal method based on adjustment of iron circulation in green rust and preparation method of reduced layered iron chromium oxide |
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