CN103241775A - Preparation method of Fe2O3/BiOCl nano-composite powder - Google Patents

Preparation method of Fe2O3/BiOCl nano-composite powder Download PDF

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CN103241775A
CN103241775A CN2013101797721A CN201310179772A CN103241775A CN 103241775 A CN103241775 A CN 103241775A CN 2013101797721 A CN2013101797721 A CN 2013101797721A CN 201310179772 A CN201310179772 A CN 201310179772A CN 103241775 A CN103241775 A CN 103241775A
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bismuth
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CN103241775B (en
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刘刚
迟庆国
杨志韬
张昌海
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Harbin University of Science and Technology
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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

Fe 2O 3The preparation method of/BiOCl composite nano-powder
Technical field
The present invention relates to a kind of preparation method of composite granule.
Background technology
Evenly disperse development very fast in recent years, all be widely used at aspects such as catalyzer, function ceramics, sensor, superconductor, coating and medicine and makeup.Compound pearly pigment mainly mixed by two kinds and two or more pigment and obtained present stage, because that powder mixes is evenly unsuitable, it is bigger to obtain the composite granule aberration, thereby influences pearl effect; In addition, the Bi based compound is because having special laminate structure and the suitable energy gap of size, in the process of research novel photocatalysis material and receive much concern.Photocatalyst material can be decomposed into inorganic molecules with organic pollutant, as water and carbonic acid gas, and has advantages such as low cost, efficient, non-secondary pollution.Single application Fe 2O 3Or during the BiOCl catalyzing organic, photochemical catalysis absorbing wavelength frequency band is narrower, thermostability is relatively poor, when perhaps using as paint additive, and problem such as pearl effect is not obvious.
Summary of the invention
The objective of the invention is in order to solve single application Fe 2O 3Or during the 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, Bismuth trinitrate is dissolved in the nitric acid, the back thin up that stirs obtains bismuth nitrate solution, and the concentration of Bismuth trinitrate is 0.0001～0.02mol/L in the bismuth nitrate solution, 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 to stirring simultaneously in the container that is filled with water simultaneously, the pH value of the hierarchy of control is 7～10 in the dropping process, obtains the bismuth hydroxide colloid;
Four, iron(ic) chloride is dissolved in the water, obtains the ferric chloride Solution that concentration is 0.005～0.02mol/L;
Five, polyoxyethylene glycol is dissolved in the water, obtains the polyoxyethylene glycol aqueous solution, described polyoxyethylene glycol is one or several the mixing in poly(oxyethylene glycol) 400, polyethylene glycol 1500, Macrogol 2000 and the Macrogol 2000 0;
Six, with the polyoxyethylene glycol aqueous solution of the bismuth hydroxide colloid that obtains in the step 3, ferric chloride Solution in the step 4 and step 5 evenly after, pour in the water heating kettle, obtain mixed system, the concentration of polyoxyethylene glycol is 0.1～10g/L in the mixed system, the mol ratio of bismuth hydroxide and iron(ic) chloride is 1: 1～10, under holding temperature is 150～200 ℃ condition, be incubated 1～48h then, with deionized water or alcohol wash 4～10 times, namely get Fe behind the naturally cooling 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.
Description of drawings
Fig. 1 is the Fe of test one preparation 2O 3The material phase analysis XRD figure of/BiOCl composite nano-powder, ★ represents BiOCl in the spectrogram,
Figure BDA00003194519500021
Expression Fe 2O 3
Fig. 2 is the Fe of test one preparation 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 the present embodiment 2O 3The preparation method of/BiOCl composite nano-powder carries out according to following steps:
One, Bismuth trinitrate is dissolved in the nitric acid, the back thin up that stirs obtains bismuth nitrate solution, and the concentration of Bismuth trinitrate is 0.0001～0.02mol/L in the bismuth nitrate solution, 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 to stirring simultaneously in the container that is filled with water simultaneously, the pH value of the hierarchy of control is 7～10 in the dropping process, obtains the bismuth hydroxide colloid;
Four, iron(ic) chloride is dissolved in the water, obtains the ferric chloride Solution that concentration is 0.005～0.02mol/L;
Five, polyoxyethylene glycol is dissolved in the water, obtains the polyoxyethylene glycol aqueous solution, described polyoxyethylene glycol is poly-second
Figure BDA00003194519500022
400, the mixing of one or several in polyethylene glycol 1500, Macrogol 2000 and the Macrogol 2000 0;
Six, with the polyoxyethylene glycol aqueous solution of the bismuth hydroxide colloid that obtains in the step 3, ferric chloride Solution in the step 4 and step 5 evenly after, pour in the water heating kettle, obtain mixed system, the concentration of polyoxyethylene glycol is 0.1～10g/L in the mixed system, the mol ratio of bismuth hydroxide and iron(ic) chloride is 1: 1～10, under holding temperature is 150～200 ℃ condition, be incubated 1～48h then, with deionized water or alcohol wash 4～10 times, namely get Fe behind the naturally cooling 2O 3/ BiOCl composite nano-powder.
When the described polyoxyethylene glycol of step 5 is mixture in the present embodiment, between each composition be arbitrarily than.
Embodiment two: present embodiment and embodiment one are different be in the step 1 in the bismuth nitrate solution concentration of Bismuth trinitrate be 0.001～0.015mol/L, the concentration of nitric acid is 0.2～8mol/L.Other is identical with embodiment one.
Embodiment three: present embodiment is different with one of embodiment one or two be in the step 1 in the bismuth nitrate solution concentration of Bismuth trinitrate be 0.008mol/L, the concentration of nitric acid is 0.9mol/L.Other and one of embodiment one or two are inequality.
Embodiment four: present embodiment is different with one of embodiment one to three is that the concentration of ammonia soln in the step 2 is 0.5mol/L.Other is identical with one of embodiment one to three.
Embodiment five: present embodiment is different with one of embodiment one to four be in the step 3 in the dropping process pH value of the hierarchy of control be 8.Other is identical with one of embodiment one to four.
Embodiment six: what present embodiment was different with one of embodiment one to five is to obtain the ferric chloride Solution that concentration is 0.01mol/L in the step 4.Other is identical with one of embodiment one to five.
Embodiment seven: present embodiment is different with one of embodiment one to six be in the step 6 in the mixed system concentration of polyoxyethylene glycol be 5g/L.Other is identical with one of embodiment one to six.
Embodiment eight: present embodiment is different with one of embodiment one to seven is that the mol ratio of bismuth hydroxide and iron(ic) chloride is 1: 4 in the step 6.Other is identical with one of embodiment one to seven.
Embodiment nine: present embodiment is different with one of embodiment one to eight is to be incubated 5～40h in the step 6 under holding temperature is 160～190 ℃ condition.Other is identical with one of embodiment one to eight.
Embodiment ten: present embodiment is different with one of embodiment one to nine is to be incubated 28h in the step 6 under holding temperature is 170 ℃ condition.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, Bismuth trinitrate is dissolved in the nitric acid, the back thin up that stirs obtains bismuth nitrate solution, and the concentration of Bismuth trinitrate is 0.001mol/L in the bismuth nitrate solution, 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 to stirring simultaneously in the container that is filled with water simultaneously, the pH value of the hierarchy of control is 8.5 in the dropping process, obtains the bismuth hydroxide colloid;
Four, iron(ic) chloride is dissolved in the water, obtains the ferric chloride Solution that concentration is 0.01mol/L;
Five, polyoxyethylene glycol is dissolved in the water, obtains the polyoxyethylene glycol aqueous solution, described polyoxyethylene glycol is Macrogol 2000;
Six, with the polyoxyethylene glycol aqueous solution of the bismuth hydroxide colloid that obtains in the step 3, ferric chloride Solution in the step 4 and step 5 evenly after, pour in the water heating kettle, obtain mixed system, the concentration of polyoxyethylene glycol is 2g/L in the mixed system, the mol ratio of bismuth hydroxide and iron(ic) chloride is 1: 1, under holding temperature is 180 ℃ condition, be incubated 6h then, with washed with de-ionized water 6 times, namely get Fe behind the naturally cooling 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 ★ represents BiOCl among the figure,
Figure BDA00003194519500031
Expression 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, Bismuth trinitrate is dissolved in the nitric acid, the back thin up that stirs obtains bismuth nitrate solution, and the concentration of Bismuth trinitrate is 0.0001mol/L in the bismuth nitrate solution, 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 to stirring simultaneously in the container that is filled with water simultaneously, the pH value of the hierarchy of control is 7 in the dropping process, obtains the bismuth hydroxide colloid;
Four, iron(ic) chloride is dissolved in the water, obtains the ferric chloride Solution that concentration is 0.005mol/L;
Five, polyoxyethylene glycol is dissolved in the water, obtains the polyoxyethylene glycol aqueous solution, described polyoxyethylene glycol is poly(oxyethylene glycol) 400;
Six, with the polyoxyethylene glycol aqueous solution of the bismuth hydroxide colloid that obtains in the step 3, ferric chloride Solution in the step 4 and step 5 evenly after, pour in the water heating kettle, obtain mixed system, the concentration of polyoxyethylene glycol is 0.1g/L in the mixed system, the mol ratio of bismuth hydroxide and iron(ic) chloride is 1: 1, under holding temperature is 150 ℃ condition, be incubated 1h then, with alcohol wash 4 times, namely get Fe behind the naturally cooling 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, Bismuth trinitrate is dissolved in the nitric acid, the back thin up that stirs obtains bismuth nitrate solution, and the concentration of Bismuth trinitrate is 0.02mol/L in the bismuth nitrate solution, 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 to stirring simultaneously in the container that is filled with water simultaneously, the pH value of the hierarchy of control is 10 in the dropping process, obtains the bismuth hydroxide colloid;
Four, iron(ic) chloride is dissolved in the water, obtains the ferric chloride Solution that concentration is 0.02mol/L;
Five, polyoxyethylene glycol is dissolved in the water, obtains the polyoxyethylene glycol aqueous solution, 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, with the polyoxyethylene glycol aqueous solution of the bismuth hydroxide colloid that obtains in the step 3, ferric chloride Solution in the step 4 and step 5 evenly after, pour in the water heating kettle, obtain mixed system, the concentration of polyoxyethylene glycol is 1.0g/L in the mixed system, the mol ratio of bismuth hydroxide and iron(ic) chloride is 1: 10, under holding temperature is 200 ℃ condition, be incubated 48h then, with deionized water or alcohol wash 10 times, namely get Fe behind the naturally cooling 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, Bismuth trinitrate is dissolved in the nitric acid, the back thin up that stirs obtains bismuth nitrate solution, and the concentration of Bismuth trinitrate is 0.015mol/L in the bismuth nitrate solution, 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 to stirring simultaneously in the container that is filled with water simultaneously, the pH value of the hierarchy of control is 8 in the dropping process, obtains the bismuth hydroxide colloid;
Four, iron(ic) chloride is dissolved in the water, obtains the ferric chloride Solution that concentration is 0.015mol/L;
Five, polyoxyethylene glycol is dissolved in the water, obtain the polyoxyethylene glycol aqueous solution, described polyoxyethylene glycol is the mixture in poly(oxyethylene glycol) 400, polyethylene glycol 1500, Macrogol 2000 and the Macrogol 2000 0, wherein between poly(oxyethylene glycol) 400, polyethylene glycol 1500, Macrogol 2000 and the Macrogol 2000 0 be arbitrarily than;
Six, with the polyoxyethylene glycol aqueous solution of the bismuth hydroxide colloid that obtains in the step 3, ferric chloride Solution in the step 4 and step 5 evenly after, pour in the water heating kettle, obtain mixed system, the concentration of polyoxyethylene glycol is 7g/L in the mixed system, the mol ratio of bismuth hydroxide and iron(ic) chloride is 1: 7, under holding temperature is 180 ℃ condition, be incubated 20h then, with deionized water or alcohol wash 8 times, namely get Fe behind the naturally cooling 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, Bismuth trinitrate is dissolved in the nitric acid, the back thin up that stirs obtains bismuth nitrate solution, and the concentration of Bismuth trinitrate is 0.0001～0.02mol/L in the bismuth nitrate solution, 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 to stirring simultaneously in the container that is filled with water simultaneously, the pH value of the hierarchy of control is 7～10 in the dropping process, obtains the bismuth hydroxide colloid;
Four, iron(ic) chloride is dissolved in the water, obtains the ferric chloride Solution that concentration is 0.005～0.02mol/L;
Five, polyoxyethylene glycol is dissolved in the water, obtains the polyoxyethylene glycol aqueous solution, described polyoxyethylene glycol is one or several the mixing in poly(oxyethylene glycol) 400, polyethylene glycol 1500, Macrogol 2000 and the Macrogol 2000 0;
Six, with the polyoxyethylene glycol aqueous solution of the bismuth hydroxide colloid that obtains in the step 3, ferric chloride Solution in the step 4 and step 5 evenly after, pour in the water heating kettle, obtain mixed system, the concentration of polyoxyethylene glycol is 0.1～10g/L in the mixed system, the mol ratio of bismuth hydroxide and iron(ic) chloride is 1: 1～10, under holding temperature is 150～200 ℃ condition, be incubated 1～48h then, with deionized water or alcohol wash 4～10 times, namely get Fe behind the naturally cooling 2O 3/ BiOCl composite nano-powder.
2. Fe according to claim 1 2O 3The preparation method of/BiOCl composite nano-powder is characterized in that in the step 1 that the concentration of Bismuth trinitrate is 0.001～0.015mol/L in the bismuth nitrate solution, and 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 is characterized in that in the step 1 that the concentration of Bismuth trinitrate is 0.008mol/L in the bismuth nitrate solution, and the concentration of nitric acid is 0.9mol/L.
4. Fe according to claim 1 2O 3The preparation method of/BiOCl composite nano-powder, the concentration that it is characterized in that ammonia soln in the 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 in the step 3 that the pH value of the hierarchy of control is 8 in the dropping process.
6. Fe according to claim 1 2O 3The preparation method of/BiOCl composite nano-powder is characterized in that obtaining in the step 4 ferric chloride Solution that concentration is 0.01mol/L.
7. Fe according to claim 1 2O 3The preparation method of/BiOCl composite nano-powder is characterized in that in the step 6 that the concentration of polyoxyethylene glycol is 5g/L in the mixed system.
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 is 1: 4 in the step 6.
9. Fe according to claim 1 2O 3The preparation method of/BiOCl composite nano-powder is characterized in that in the step 6 being incubated 5～40h under holding temperature is 160～190 ℃ condition.
10. Fe according to claim 1 2O 3The preparation method of/BiOCl composite nano-powder is characterized in that in the step 6 being incubated 28h under holding temperature is 170 ℃ condition.
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Cited By (6)

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CN103769175A (en) * 2014-03-04 2014-05-07 南京信息工程大学 Preparation method and application of composite photocatalyst
CN105195182A (en) * 2015-10-19 2015-12-30 扬州大学 Preparation method for visible light catalytic composite material
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
CN105457662A (en) * 2015-12-24 2016-04-06 江苏大学 3D ball-flower-structured BiOCl-ZnFe2O4 composite photocatalysis material and preparation method thereof
CN106669741A (en) * 2015-11-11 2017-05-17 孙文彬 Visual light driven semiconductor photocatalyst as well as preparation method and application 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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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103769175A (en) * 2014-03-04 2014-05-07 南京信息工程大学 Preparation method and application of composite photocatalyst
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
CN105457662A (en) * 2015-12-24 2016-04-06 江苏大学 3D ball-flower-structured BiOCl-ZnFe2O4 composite photocatalysis material and preparation method 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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