CN103241775B - Preparation method of Fe2O3/BiOCl nano-composite powder - Google Patents
Preparation method of Fe2O3/BiOCl nano-composite powder Download PDFInfo
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- CN103241775B CN103241775B CN201310179772.1A CN201310179772A CN103241775B CN 103241775 B CN103241775 B CN 103241775B CN 201310179772 A CN201310179772 A CN 201310179772A CN 103241775 B CN103241775 B CN 103241775B
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Abstract
The invention relates to a preparation method of composite powder, and in particular relates to a preparation method of Fe2O3/BiOCl nano-composite powder. The preparation method aims to solve the technical problem that when Fe2O3 or BiOCl is separately applied to catalyzing organics and serves as a coating additive, the pearl effect is not obvious. The method comprises the following steps of: 1, dissolving bismuth nitrate in nitric acid, uniformly stirring, diluting with water to obtain a bismuth nitrate solution; 2, preparing an ammonia water solution; 3, preparing a bismuth hydroxide colloid; 4, preparing a ferric chloride solution; 5, dissolving polyethylene glycol in water to obtain a polyethylene glycol water solution; and 6, mixing the bismuth hydroxide colloid, the ferric chloride solution and the polyethylene glycol water solution, pouring the mixture into a hydrothermal kettle, holding the temperature and obtaining the Fe2O3/BiOCl nano-composite powder after naturally cooling. The Fe2O3/BiOCl nano-composite powder obtained by adopting the method is simple in synthesis process, low in cost and good in pearl effect and can be recycled when serving as a photocatalyst.
Description
Technical field
The present invention relates to a kind of preparation method of composite granule.
Background technology
Dispersed development is in recent years very fast, is all widely used in catalyzer, function ceramics, sensor, superconductor, coating and medicine and makeup etc.Present stage, composite bead delustering pigment was mainly obtained by mixing by two kinds and two or more pigment, and because powder mixing is evenly unsuitable, acquisition composite granule aberration is comparatively large, thus affects pearl effect; In addition, Bi based compound, because having the energy gap of special laminate structure and suitable size, receives much concern in the process of research novel photocatalysis material.Organic pollutant can be decomposed into inorganic molecules by photocatalyst material, as water and carbonic acid gas, and has the advantages such as low cost, efficient, non-secondary pollution.Single application Fe
2o
3or during BiOCl catalyzing organic, photochemical catalysis absorbing wavelength frequency band is narrower, thermostability is poor, or when using as paint additive, the problems such as pearl effect is not obvious.
Summary of the invention
The object of the invention is to solve single application Fe
2o
3or during BiOCl catalyzing organic, when using as paint additive, the unconspicuous technical problem of pearl effect, provides a kind of Fe
2o
3the preparation method of/BiOCl composite nano-powder.
Fe
2o
3the preparation method of/BiOCl composite nano-powder carries out according to following steps:
One, be dissolved in nitric acid by Bismuth trinitrate, thin up after stirring, obtains bismuth nitrate solution, and in bismuth nitrate solution, the concentration of Bismuth trinitrate is 0.0001 ~ 0.02mol/L, and the concentration of nitric acid is 0.02 ~ 10mol/L;
Two, compound concentration is the ammonia soln of 0.001 ~ 2mol/L;
Three, ammoniacal liquor and bismuth nitrate solution are added drop-wise in the container be filled with water simultaneously and stir simultaneously, in dropping process, the pH value of the hierarchy of control is 7 ~ 10, obtains bismuth hydroxide colloid;
Four, iron(ic) chloride is dissolved in water, obtains the ferric chloride Solution that concentration is 0.005 ~ 0.02mol/L;
Five, be dissolved in water by polyoxyethylene glycol, obtain Aqueous Solutions of Polyethylene Glycol, described polyoxyethylene glycol is one or several the mixing in poly(oxyethylene glycol) 400, polyethylene glycol 1500, Macrogol 2000 and PEG 20000;
Six, after the Aqueous Solutions of Polyethylene Glycol of the ferric chloride Solution in the bismuth hydroxide colloid obtained in step 3, step 4 and step 5 being mixed, pour in water heating kettle, obtain mixed system, in mixed system, the concentration of polyoxyethylene glycol is 0.1 ~ 10g/L, the mol ratio of bismuth hydroxide and iron(ic) chloride is 1: 1 ~ 10, then be incubated 1 ~ 48h under the condition of 150 ~ 200 DEG C in holding temperature, with deionized water or alcohol washes 4 ~ 10 times after naturally cooling, obtain Fe
2o
3/ BiOCl composite nano-powder.
Fe of the present invention
2o
3the synthesis technique of/BiOCl composite nano-powder is simple, cost is low, pearl effect is good, when using as photocatalyst, recyclable recycling.
Accompanying drawing explanation
Fig. 1 is Fe prepared by test one
2o
3the material phase analysis XRD figure of/BiOCl composite nano-powder, in spectrogram, ★ represents BiOCl,
represent Fe
2o
3;
Fig. 2 is Fe prepared by test one
2o
3the thing phase SEM photo of/BiOCl composite nano-powder.
Embodiment
Technical solution of the present invention is not limited to following cited embodiment, also comprises the arbitrary combination between each embodiment.
Embodiment one: Fe in present embodiment
2o
3the preparation method of/BiOCl composite nano-powder carries out according to following steps:
One, be dissolved in nitric acid by Bismuth trinitrate, thin up after stirring, obtains bismuth nitrate solution, and in bismuth nitrate solution, the concentration of Bismuth trinitrate is 0.0001 ~ 0.02mol/L, and the concentration of nitric acid is 0.02 ~ 10mol/L;
Two, compound concentration is the ammonia soln of 0.001 ~ 2mol/L;
Three, ammoniacal liquor and bismuth nitrate solution are added drop-wise in the container be filled with water simultaneously and stir simultaneously, in dropping process, the pH value of the hierarchy of control is 7 ~ 10, obtains bismuth hydroxide colloid;
Four, iron(ic) chloride is dissolved in water, obtains the ferric chloride Solution that concentration is 0.005 ~ 0.02mol/L;
Five, be dissolved in water by polyoxyethylene glycol, obtain Aqueous Solutions of Polyethylene Glycol, described polyoxyethylene glycol is one or several the mixing in poly(oxyethylene glycol) 400, polyethylene glycol 1500, Macrogol 2000 and PEG 20000;
Six, after the Aqueous Solutions of Polyethylene Glycol of the ferric chloride Solution in the bismuth hydroxide colloid obtained in step 3, step 4 and step 5 being mixed, pour in water heating kettle, obtain mixed system, in mixed system, the concentration of polyoxyethylene glycol is 0.1 ~ 10g/L, the mol ratio of bismuth hydroxide and iron(ic) chloride is 1: 1 ~ 10, then be incubated 1 ~ 48h under the condition of 150 ~ 200 DEG C in holding temperature, with deionized water or alcohol washes 4 ~ 10 times after naturally cooling, obtain Fe
2o
3/ BiOCl composite nano-powder.
When in present embodiment, described in step 5, polyoxyethylene glycol is mixture, between each composition be arbitrarily than.
Embodiment two: present embodiment and embodiment one are 0.001 ~ 0.015mol/L unlike the concentration of Bismuth trinitrate in bismuth nitrate solution in step one, and the concentration of nitric acid is 0.2 ~ 8mol/L.Other is identical with embodiment one.
Embodiment three: one of present embodiment and embodiment one or two are 0.008mol/L unlike the concentration of Bismuth trinitrate in bismuth nitrate solution in step one, the concentration of nitric acid is 0.9mol/L.Other is not identical with one of embodiment one or two.
Embodiment four: one of present embodiment and embodiment one to three are 0.5mol/L unlike the concentration of ammonia soln in step 2.Other is identical with one of embodiment one to three.
Embodiment five: one of present embodiment and embodiment one to four are 8 unlike the pH value of the hierarchy of control in dropping process in step 3.Other is identical with one of embodiment one to four.
Embodiment six: one of present embodiment and embodiment one to five are unlike obtaining the ferric chloride Solution that concentration is 0.01mol/L in step 4.Other is identical with one of embodiment one to five.
Embodiment seven: one of present embodiment and embodiment one to six are 5g/L unlike the concentration of polyoxyethylene glycol in mixed system in step 6.Other is identical with one of embodiment one to six.
Embodiment eight: one of present embodiment and embodiment one to seven are 1: 4 unlike the mol ratio of bismuth hydroxide in step 6 and iron(ic) chloride.Other is identical with one of embodiment one to seven.
Embodiment nine: one of present embodiment and embodiment one to eight are unlike in step 6 in holding temperature being insulation 5 ~ 40h under the condition of 160 ~ 190 DEG C.Other is identical with one of embodiment one to eight.
Embodiment ten: one of present embodiment and embodiment one to nine are unlike being be incubated 28h under the condition of 170 DEG C in holding temperature in step 6.Other is identical with one of embodiment one to nine.
Adopt following verification experimental verification effect of the present invention:
Test one:
Fe
2o
3the preparation method of/BiOCl composite nano-powder carries out according to following steps:
One, be dissolved in nitric acid by Bismuth trinitrate, thin up after stirring, obtains bismuth nitrate solution, and in bismuth nitrate solution, the concentration of Bismuth trinitrate is 0.001mol/L, and the concentration of nitric acid is 0.5mol/L;
Two, compound concentration is the ammonia soln of 0.05mol/L;
Three, ammoniacal liquor and bismuth nitrate solution are added drop-wise in the container be filled with water simultaneously and stir simultaneously, in dropping process, the pH value of the hierarchy of control is 8.5, obtains bismuth hydroxide colloid;
Four, iron(ic) chloride is dissolved in water, obtains the ferric chloride Solution that concentration is 0.01mol/L;
Five, be dissolved in water by polyoxyethylene glycol, obtain Aqueous Solutions of Polyethylene Glycol, described polyoxyethylene glycol is Macrogol 2000;
Six, after the Aqueous Solutions of Polyethylene Glycol of the ferric chloride Solution in the bismuth hydroxide colloid obtained in step 3, step 4 and step 5 being mixed, pour in water heating kettle, obtain mixed system, in mixed system, the concentration of polyoxyethylene glycol is 2g/L, the mol ratio of bismuth hydroxide and iron(ic) chloride is 1: 1, then be incubated 6h under the condition of 180 DEG C in holding temperature, use washed with de-ionized water 6 times after naturally cooling, obtain Fe
2o
3/ BiOCl composite nano-powder.
Fig. 1 is the material phase analysis XRD figure spectrum of the composite granule of preparation in this test, and in figure, ★ represents BiOCl,
represent Fe
2o
3, illustrate that composite granule is by Fe
2o
3form with BiOCl.
Test two:
Fe
2o
3the preparation method of/BiOCl composite nano-powder carries out according to following steps:
One, be dissolved in nitric acid by Bismuth trinitrate, thin up after stirring, obtains bismuth nitrate solution, and in bismuth nitrate solution, the concentration of Bismuth trinitrate is 0.0001mol/L, and the concentration of nitric acid is 0.02mol/L;
Two, compound concentration is the ammonia soln of 0.001mol/L;
Three, ammoniacal liquor and bismuth nitrate solution are added drop-wise in the container be filled with water simultaneously and stir simultaneously, in dropping process, the pH value of the hierarchy of control is 7, obtains bismuth hydroxide colloid;
Four, iron(ic) chloride is dissolved in water, obtains the ferric chloride Solution that concentration is 0.005mol/L;
Five, be dissolved in water by polyoxyethylene glycol, obtain Aqueous Solutions of Polyethylene Glycol, described polyoxyethylene glycol is poly(oxyethylene glycol) 400;
Six, after the Aqueous Solutions of Polyethylene Glycol of the ferric chloride Solution in the bismuth hydroxide colloid obtained in step 3, step 4 and step 5 being mixed, pour in water heating kettle, obtain mixed system, in mixed system, the concentration of polyoxyethylene glycol is 0.1g/L, the mol ratio of bismuth hydroxide and iron(ic) chloride is 1: 1, then be incubated 1h under the condition of 150 DEG C in holding temperature, use alcohol washes 4 times after naturally cooling, obtain Fe
2o
3/ BiOCl composite nano-powder.
Test three:
Fe
2o
3the preparation method of/BiOCl composite nano-powder carries out according to following steps:
One, be dissolved in nitric acid by Bismuth trinitrate, thin up after stirring, obtains bismuth nitrate solution, and in bismuth nitrate solution, the concentration of Bismuth trinitrate is 0.02mol/L, and the concentration of nitric acid is 10mol/L;
Two, compound concentration is the ammonia soln of 2mol/L;
Three, ammoniacal liquor and bismuth nitrate solution are added drop-wise in the container be filled with water simultaneously and stir simultaneously, in dropping process, the pH value of the hierarchy of control is 10, obtains bismuth hydroxide colloid;
Four, iron(ic) chloride is dissolved in water, obtains the ferric chloride Solution that concentration is 0.02mol/L;
Five, be dissolved in water by polyoxyethylene glycol, obtain Aqueous Solutions of Polyethylene Glycol, described polyoxyethylene glycol is the mixture of poly(oxyethylene glycol) 400, polyethylene glycol 1500, wherein poly(oxyethylene glycol) 400 and polyethylene glycol 1500 be arbitrarily than;
Six, after the Aqueous Solutions of Polyethylene Glycol of the ferric chloride Solution in the bismuth hydroxide colloid obtained in step 3, step 4 and step 5 being mixed, pour in water heating kettle, obtain mixed system, in mixed system, the concentration of polyoxyethylene glycol is 1.0g/L, the mol ratio of bismuth hydroxide and iron(ic) chloride is 1: 10, then be incubated 48h under the condition of 200 DEG C in holding temperature, with deionized water or alcohol washes 10 times after naturally cooling, obtain Fe
2o
3/ BiOCl composite nano-powder.
Test four:
Fe
2o
3the preparation method of/BiOCl composite nano-powder carries out according to following steps:
One, be dissolved in nitric acid by Bismuth trinitrate, thin up after stirring, obtains bismuth nitrate solution, and in bismuth nitrate solution, the concentration of Bismuth trinitrate is 0.015mol/L, and the concentration of nitric acid is 6mol/L;
Two, compound concentration is the ammonia soln of 1mol/L;
Three, ammoniacal liquor and bismuth nitrate solution are added drop-wise in the container be filled with water simultaneously and stir simultaneously, in dropping process, the pH value of the hierarchy of control is 8, obtains bismuth hydroxide colloid;
Four, iron(ic) chloride is dissolved in water, obtains the ferric chloride Solution that concentration is 0.015mol/L;
Five, polyoxyethylene glycol is dissolved in water, obtain Aqueous Solutions of Polyethylene Glycol, described polyoxyethylene glycol is the mixture in poly(oxyethylene glycol) 400, polyethylene glycol 1500, Macrogol 2000 and PEG 20000, between poly(oxyethylene glycol) 400, polyethylene glycol 1500, Macrogol 2000 and PEG 20000 be wherein arbitrarily than;
Six, after the Aqueous Solutions of Polyethylene Glycol of the ferric chloride Solution in the bismuth hydroxide colloid obtained in step 3, step 4 and step 5 being mixed, pour in water heating kettle, obtain mixed system, in mixed system, the concentration of polyoxyethylene glycol is 7g/L, the mol ratio of bismuth hydroxide and iron(ic) chloride is 1: 7, then be incubated 20h under the condition of 180 DEG C in holding temperature, with deionized water or alcohol washes 8 times after naturally cooling, obtain Fe
2o
3/ BiOCl composite nano-powder.
Claims (10)
1.Fe
2o
3the preparation method of/BiOCl composite nano-powder, is characterized in that Fe
2o
3the preparation method of/BiOCl composite nano-powder carries out according to following steps:
One, be dissolved in nitric acid by Bismuth trinitrate, thin up after stirring, obtains bismuth nitrate solution, and in bismuth nitrate solution, the concentration of Bismuth trinitrate is 0.0001 ~ 0.02mol/L, and the concentration of nitric acid is 0.02 ~ 10mol/L;
Two, compound concentration is the ammonia soln of 0.001 ~ 2mol/L;
Three, ammoniacal liquor and bismuth nitrate solution are added drop-wise in the container be filled with water simultaneously and stir simultaneously, in dropping process, the pH value of the hierarchy of control is 7 ~ 10, obtains bismuth hydroxide colloid;
Four, iron(ic) chloride is dissolved in water, obtains the ferric chloride Solution that concentration is 0.005 ~ 0.02mol/L;
Five, be dissolved in water by polyoxyethylene glycol, obtain Aqueous Solutions of Polyethylene Glycol, described polyoxyethylene glycol is one or several the mixing in poly(oxyethylene glycol) 400, polyethylene glycol 1500, Macrogol 2000 and PEG 20000;
Six, after the Aqueous Solutions of Polyethylene Glycol of the ferric chloride Solution in the bismuth hydroxide colloid obtained in step 3, step 4 and step 5 being mixed, pour in water heating kettle, obtain mixed system, in mixed system, the concentration of polyoxyethylene glycol is 0.1 ~ 10g/L, the mol ratio of bismuth hydroxide and iron(ic) chloride is 1: 1 ~ 10, then be incubated 1 ~ 48h under the condition of 150 ~ 200 DEG C in holding temperature, with deionized water or alcohol washes 4 ~ 10 times after naturally cooling, obtain Fe
2o
3/ BiOCl composite nano-powder.
2. Fe according to claim 1
2o
3the preparation method of/BiOCl composite nano-powder, it is characterized in that the concentration of Bismuth trinitrate in bismuth nitrate solution in step one is 0.001 ~ 0.015mol/L, the concentration of nitric acid is 0.2 ~ 8mol/L.
3. Fe according to claim 1
2o
3the preparation method of/BiOCl composite nano-powder, it is characterized in that the concentration of Bismuth trinitrate in bismuth nitrate solution in step one is 0.008mol/L, the concentration of nitric acid is 0.9mol/L.
4. Fe according to claim 1
2o
3the preparation method of/BiOCl composite nano-powder, is characterized in that the concentration of ammonia soln in step 2 is 0.5mol/L.
5. Fe according to claim 1
2o
3the preparation method of/BiOCl composite nano-powder, is characterized in that the pH value of the hierarchy of control in dropping process in step 3 is 8.
6. Fe according to claim 1
2o
3the preparation method of/BiOCl composite nano-powder, is characterized in that obtaining the ferric chloride Solution that concentration is 0.01mol/L in step 4.
7. Fe according to claim 1
2o
3the preparation method of/BiOCl composite nano-powder, is characterized in that the concentration of polyoxyethylene glycol in mixed system in step 6 is 5g/L.
8. Fe according to claim 1
2o
3the preparation method of/BiOCl composite nano-powder, is characterized in that the mol ratio of bismuth hydroxide and iron(ic) chloride in step 6 is 1: 4.
9. Fe according to claim 1
2o
3the preparation method of/BiOCl composite nano-powder, is characterized in that under holding temperature is the condition of 160 ~ 190 DEG C, being incubated 5 ~ 40h in step 6.
10. Fe according to claim 1
2o
3the preparation method of/BiOCl composite nano-powder, is characterized in that under holding temperature is the condition of 170 DEG C, being incubated 28h in step 6.
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CN103769175B (en) * | 2014-03-04 | 2015-09-23 | 南京信息工程大学 | A kind of preparation method of composite photo-catalyst and application thereof |
CN105195182A (en) * | 2015-10-19 | 2015-12-30 | 扬州大学 | Preparation method for visible light catalytic composite material |
CN106669741A (en) * | 2015-11-11 | 2017-05-17 | 孙文彬 | Visual light driven semiconductor photocatalyst as well as preparation method and application thereof |
CN105344364A (en) * | 2015-11-30 | 2016-02-24 | 环境保护部华南环境科学研究所 | Ferric oxide/bismuth oxybromide composite material and preparation method and application thereof |
CN105457662B (en) * | 2015-12-24 | 2018-06-26 | 江苏大学 | A kind of 3D bouquets structure BiOCl-ZnFe2O4Composite photocatalyst material and preparation method thereof |
CN110773206A (en) * | 2019-11-27 | 2020-02-11 | 中国科学院青岛生物能源与过程研究所 | Fe with high catalytic degradation activity 2O 3BiOCl composite photocatalyst and preparation method and application thereof |
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CN101602007A (en) * | 2009-07-14 | 2009-12-16 | 中国科学院上海硅酸盐研究所 | Visible light-responded magnetic photocatalytic material and preparation thereof |
CN102549836A (en) * | 2009-08-07 | 2012-07-04 | 布莱克光电有限公司 | Heterogeneous hydrogen-catalyst power system |
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2013
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DE4104310A1 (en) * | 1991-02-13 | 1992-08-20 | Merck Patent Gmbh | Flaky pigment having metal substrate with iron oxide coating - prodn. by pptn. from aq. soln., used in paint, plastics, cosmetics or magneto=optical medium |
CN1536031A (en) * | 2003-04-11 | 2004-10-13 | 陈书怡 | Polycrystalline state composite and its preparation method |
CN101602007A (en) * | 2009-07-14 | 2009-12-16 | 中国科学院上海硅酸盐研究所 | Visible light-responded magnetic photocatalytic material and preparation thereof |
CN102549836A (en) * | 2009-08-07 | 2012-07-04 | 布莱克光电有限公司 | Heterogeneous hydrogen-catalyst power system |
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