CN100343165C - Alkaline zinc carbonate nano-wire and its preparation method - Google Patents
Alkaline zinc carbonate nano-wire and its preparation method Download PDFInfo
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- CN100343165C CN100343165C CNB2005100311834A CN200510031183A CN100343165C CN 100343165 C CN100343165 C CN 100343165C CN B2005100311834 A CNB2005100311834 A CN B2005100311834A CN 200510031183 A CN200510031183 A CN 200510031183A CN 100343165 C CN100343165 C CN 100343165C
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Abstract
The present invention relates to an alkali zinc carbonate nanometer wire and a preparation method thereof, which mainly solves the technical problems that alkali zinc carbonate nanometer wire materials and preparation methods do not exist at present, etc. The preparation method has the technical scheme that zinc oxide (or zinc salts) is used as raw materials, ammonia water (or EDTA) is used as coordination agents and soluble carbonate is used as precipitating agents to carry out reactions and generate a zinc coordination compound solution. Then, alkali zinc carbonate is uniformly precipitated to generate nanometer wires by the addition of distilled water or other solvents, or heating, or the addition and the heating of the distilled water or other solvents. The nanometer wires are washed and precipitated by the distilled water (or dilute ammonia water) through filtration and separation, and are dried to obtain alkali zinc carbonate nanometer wires. The alkali zinc carbonate is prepared in aqueous solution systems, the process flow is simple, the reaction conditions are mild, and the preparation cost is very low.
Description
Technical field
The present invention relates to a kind of alkaline zinc carbonate nano-wire and preparation method thereof.Alkaline zinc carbonate nano-wire with this method preparation can be used for preparing inorganic/high polymer composite nano-material.
Background technology
The method for preparing at present the inorganic nano wire material all needs severe condition such as high temperature and high pressure, and yields poorly, and is with high costs, seriously restricted the application of such nano material.Therefore research and develop out production technique inorganic nano wire material and technology of preparing thereof simple, with low cost, have crucial meaning.
Summary of the invention
The purpose of this invention is to provide a kind of alkaline zinc carbonate nano-wire.
Another object of the present invention provides a kind of preparation method who adopts prepared alkaline zinc carbonate nano-wires such as coordination reaction, precipitation from homogeneous solution, filtering separation, washing, drying.
The technical solution adopted for the present invention to solve the technical problems is: with zinc oxide or zinc salt is raw material, with ammoniacal liquor or EDTA is coordination agent, the soluble carbon hydrochlorate is a precipitation agent, through prepared alkaline zinc carbonate nano-wires such as coordination reaction, precipitation from homogeneous solution, filtering separation, washing, dryings.
The preparation method of described alkaline zinc carbonate nano-wire is: with zinc oxide or zinc salt is raw material, with ammoniacal liquor or EDTA is coordination agent, the soluble carbon hydrochlorate is a precipitation agent, earlier that each coordination reaction thing is required or suitably excessive by reaction stoichiometric ratio generates Zn complex solution with coordination agent ammoniacal liquor or EDTA and soluble carbon hydrochlorate through coordination reaction with zinc oxide or zinc salt, in this Zn complex solution, add distilled water then, or alcohols, or acetone, or the solvent of its arbitrary combination, under 10-90 ℃ temperature and agitation condition precipitation from homogeneous solution 0.1-48 hour alkaline zinc carbonate nano-wire, after separating after filtration again, with distilled water or weak ammonia washing precipitation 1-10 time, drying promptly makes the alkaline zinc carbonate nano-wire product under 30-200 ℃ of temperature condition.
Described raw material zinc salt comprises zinc chloride or zinc nitrate or zinc carbonate or zinc sulfate or zinc acetate or its arbitrary combination.
Described coordination agent is that concentration is greater than 0.1mol.dm
-3Ammoniacal liquor or concentration be 0.01-1.0mol.dm
-3EDTA solution, its add-on be the zinc mole number 0.5-20 doubly.
Described soluble carbon hydrochlorate comprises bicarbonate of ammonia, volatile salt, yellow soda ash or salt of wormwood, and its add-on is 0.5-4.0 a times of zinc mole number.
The add-on of described distilled water is 0.5-20 a times of Zn complex saturated solution volume.
Described alcoholic solvent comprises methyl alcohol or ethanol or its arbitrary combination, and add-on is 0.05-10 a times of Zn complex saturated solution volume.
The add-on of described acetone is 0.05-10 a times of Zn complex saturated solution volume.
The solvent of described washing precipitation is that concentration is 0.01-2.0mol.dm
-3Weak ammonia.
The characteristics of the alkaline zinc carbonate nano-wire of the present invention's preparation are:
(1) this law is to prepare alkaline zinc carbonate nano-wire in water solution system, the reaction conditions gentleness, and preparation technology is simple, and cost is very cheap.
(2) this law adopts this law just can prepare the alkaline zinc carbonate nano-wire product without any need for template.
(3) adopt this law not only can the high alkaline zinc carbonate nano-wire product of preparation quality, and realize suitability for industrialized production easily.
Description of drawings
Fig. 1 is the transmission electron microscope photo 1 (amplifying 100,000 times) of product of the present invention.
Fig. 2 is the transmission electron microscope photo 2 (amplifying 100,000 times) of product of the present invention.
Fig. 3 is the transmission electron microscope photo 3 (amplifying 100,000 times) of product of the present invention.
Fig. 4 is the transmission electron microscope photo 4 (amplifying 100,000 times) of product of the present invention.
Embodiment
The present invention is by being raw material with zinc oxide or zinc salt, with ammoniacal liquor or EDTA (sodium ethylene diamine tetracetate) solution is coordination agent, the soluble carbon hydrochlorate is a precipitation agent, generate Zn complex solution through coordination reaction, in this Zn complex solution, add distilled water then, or alcohols, or acetone, or the solvent of its arbitrary combination, precipitation from homogeneous solution generates alkaline zinc carbonate nano-wire under 10-90 ℃ temperature and agitation condition, after separating after filtration again, with distilled water or weak ammonia washing precipitation 2-3 time, drying promptly makes the alkaline zinc carbonate nano-wire product under 30-200 ℃ of temperature condition.
Concrete steps are:
(1) with zinc oxide (or zinc salt) solid and concentration greater than 0.1mol.dm
-3Ammoniacal liquor (or concentration is 0.01-1.0mol.dm
-3EDTA solution) and soluble carbon hydrochlorate solid stirring reaction at normal temperatures, all dissolve until solid and generate Zn complex solution.
(2) in above-mentioned complex solution, add the water that 1-10 doubly measures, allow its precipitation from homogeneous solution.The temperature of precipitation from homogeneous solution is 10-90 ℃, and the time of precipitation from homogeneous solution is 0.1-48 hour;
Or in above-mentioned complex solution, add the methyl alcohol that 0.5-5 doubly measures, allow its precipitation from homogeneous solution.The temperature of precipitation from homogeneous solution is 10-90 ℃, and the time of precipitation from homogeneous solution is 0.1-48 hour;
Or in above-mentioned complex solution, add the ethanol that 0.5-5 doubly measures, allow its precipitation from homogeneous solution.The temperature of precipitation from homogeneous solution is 10-90 ℃, and the time of precipitation from homogeneous solution is 0.1-48 hour;
Or in above-mentioned complex solution, add the acetone that 0.5-5 doubly measures, allow its precipitation from homogeneous solution.The temperature of precipitation from homogeneous solution is 10-90 ℃, and the time of precipitation from homogeneous solution is 0.1-48 hour.
(3) filtering to isolate precipitation, is 0.01-1.0mol.dm with distilled water or concentration
-3Ammonia scrubbing precipitation for several times.
(4) will be deposited in 30-200 ℃ of drying down, obtain the alkaline zinc carbonate nano-wire material.
Further specify embodiment below in conjunction with embodiment.
Embodiment 1, takes by weighing ZnO16 gram (0.197mol), adds concentration 6mol.dm
3Ammoniacal liquor 200ml (1.2mol), NH
1HCO
320 grams (0.253mol), stirring reaction all dissolves to all ZnO under the normal temperature, removes by filter insolubles, adds 800ml distilled water then, heats in water-bath to 55 ℃, stirs insulation down 1 hour, obtains a large amount of white precipitates.With sedimentation and filtration, precipitate three times with distilled water wash, after 80 ℃ of following dryings of temperature, get product.
Embodiment 2, take by weighing ZnO16 gram (0.197mol), add concentration 3mol.dm
-3Ammoniacal liquor 420ml (1.26mol), (NH
1)
2CO
324 grams (0.25mol), stirring reaction all dissolves to all ZnO under the normal temperature, removes by filter insolubles, adds 600ml distilled water then, heats in water-bath to 60 ℃, stirs insulation down 1 hour, obtains a large amount of white precipitates.With sedimentation and filtration, be 0.05mol.dm with concentration
-3Ammonia scrubbing precipitation three times after 85 ℃ of following dryings of temperature, gets product.
Embodiment 3, take by weighing ZnSO
1.7H
2O 60 grams (0.208mol) add concentration 6mol.dm
-3Ammoniacal liquor 200ml (1.2mol), NH
1HCO
320 grams (0.253mol), stirring reaction to all zinc salts all dissolve under the normal temperature, remove by filter insolubles, add 800ml distilled water then, heat in water-bath to 55 ℃, stir insulation down 1 hour, obtain a large amount of white precipitates.With sedimentation and filtration, precipitate three times with distilled water wash, after 60 ℃ of following dryings of temperature, get product.
Embodiment 4, take by weighing ZnCL
2.2H
2O 30 grams (0.175mol) add concentration 6mol.dm
-3Ammoniacal liquor 200ml (1.2mol), NH
1HCO
322 grams (0.278mol), stirring reaction to all zinc salts all dissolve under the normal temperature, remove by filter insolubles, add 800ml distilled water then, heat in water-bath to 60 ℃, stir insulation down 1 hour, obtain a large amount of white precipitates.With sedimentation and filtration, precipitate three times with distilled water wash, after 70 ℃ of following dryings of temperature, get product.
Embodiment 5, take by weighing ZnO16 gram (0.197mol), add concentration 6mol.dm
-3Ammoniacal liquor 200ml (1.2mol), NH
4HCO
320 grams (0.253mol), stirring reaction all dissolves to all ZnO under the normal temperature, removes by filter insolubles, adds 100ml ethanol then, at normal temperature (25 ℃) stirring reaction 0.5 hour down, obtains a large amount of white precipitates.With sedimentation and filtration, be 0.1mol.dm with concentration
-3Ammonia scrubbing precipitation three times after 80 ℃ of following dryings of temperature, gets product.
Embodiment 6, take by weighing ZnO 16 grams (0.197mol), add concentration 6mol.dm
-3Ammoniacal liquor 200ml (1.2mol), NH
1HCO
324 grams (0.303mol), stirring reaction all dissolves to all ZnO under the normal temperature, removes by filter insolubles, adds 50ml acetone then, at normal temperature (25 ℃) stirring reaction 0.5 hour down, obtains a large amount of white precipitates.With sedimentation and filtration, precipitate three times with distilled water wash, after 80 ℃ of following dryings of temperature, get product.
Embodiment 7, take by weighing ZnO 16 grams (0.197mol), and adding concentration is 0.5mol.dm
-3EDTA500ml (0.25mol), NH
1HCO
324 grams (0.303mol), stirring reaction all dissolves to all ZnO under the normal temperature, removes by filter insolubles, adds 800ml distilled water then, heats in water-bath to 65 ℃, stirs insulation down 1 hour, obtains a large amount of white precipitates.With sedimentation and filtration, precipitate three times with distilled water wash, after 80 ℃ of following dryings of temperature, get product.
Embodiment 8, take by weighing Zn (NO
3)
236 grams (0.19mol) add concentration 0.5mol.dm
-3EDTA500ml, NH
1HCO
320 grams (0.23mol), stirring reaction to all zinc salts all dissolve under the normal temperature, remove by filter insolubles, add 800ml distilled water then, heat in water-bath to 65 ℃, stir insulation down 1 hour, obtain a large amount of white precipitates.With sedimentation and filtration, precipitate three times with distilled water wash, after 80 ℃ of following dryings of temperature, get product.
Embodiment 9, take by weighing Zn (NO
3)
236 grams (0.19mol) add concentration 0.5mol.dm
-3EDTA500ml, Zn (Ac)
236.6 gram (0.2mol), stirring reaction to all zinc salts all dissolve under the normal temperature, remove by filter insolubles, add 800ml distilled water then, heat in water-bath to 65 ℃, stir insulation down 1 hour, obtain a large amount of white precipitates.With sedimentation and filtration, precipitate three times with distilled water wash, after 80 ℃ of following dryings of temperature, get product.
Obviously, described soluble carbon hydrochlorate can be selected bicarbonate of ammonia or volatile salt or yellow soda ash or salt of wormwood or its arbitrary combination respectively for use.
Claims (9)
1, a kind of alkaline zinc carbonate nano-wire, it is characterized in that: with zinc oxide or zinc salt is raw material, with ammoniacal liquor or EDTA is coordination agent, and the soluble carbon hydrochlorate is a precipitation agent, prepares alkaline zinc carbonate nano-wire through coordination reaction, precipitation from homogeneous solution, filtering separation, washing, drying process.
2, the preparation method of alkaline zinc carbonate nano-wire according to claim 1, it is characterized in that: with zinc oxide or zinc salt is raw material, with ammoniacal liquor or EDTA is coordination agent, the soluble carbon hydrochlorate is a precipitation agent, earlier that each coordination reaction thing is required or suitably excessive by reaction stoichiometric ratio generates Zn complex solution with coordination agent ammoniacal liquor or EDTA and soluble carbon hydrochlorate through coordination reaction with zinc oxide or zinc salt, in this Zn complex solution, add then and comprise distilled water, or alcohols, or acetone, or the solvent of its arbitrary combination, under 10-90 ℃ temperature and agitation condition precipitation from homogeneous solution 0.1-48 hour alkaline zinc carbonate nano-wire, after separating after filtration again, with distilled water or weak ammonia washing precipitation 1-10 time, drying promptly makes the alkaline zinc carbonate nano-wire product under 30-200 ℃ of temperature condition.
3, the preparation method of alkaline zinc carbonate nano-wire according to claim 2 is characterized in that: described raw material zinc salt comprises zinc chloride or zinc nitrate or zinc carbonate or zinc sulfate or its arbitrary combination.
4, according to the preparation method of the described alkaline zinc carbonate nano-wire of claim 2, it is characterized in that: described coordination agent is that concentration is greater than 0.1mol.dm
-3Ammoniacal liquor or concentration be 0.01-1.0mol.dm
-3EDTA solution, its add-on be the zinc mole number 0.5-20 doubly.
5, according to the preparation method of the described alkaline zinc carbonate nano-wire of claim 2, it is characterized in that: described soluble carbon hydrochlorate comprises bicarbonate of ammonia, volatile salt or yellow soda ash, and its add-on is 0.5-4.0 a times of zinc mole number.
6, according to the preparation method of the described alkaline zinc carbonate nano-wire of claim 2, it is characterized in that: the add-on of described distilled water is 0.5-20 a times of Zn complex saturated solution volume.
7, according to the preparation method of the described alkaline zinc carbonate nano-wire of claim 2, it is characterized in that: described alcoholic solvent comprises methyl alcohol or ethanol or its arbitrary combination, and add-on is 0.05-10 a times of Zn complex saturated solution volume.
8, according to the preparation method of the described alkaline zinc carbonate nano-wire of claim 2, it is characterized in that: the add-on of described acetone is 0.05-10 a times of Zn complex saturated solution volume.
9, according to the preparation method of the described alkaline zinc carbonate nano-wire of claim 2, it is characterized in that: the solvent of described washing precipitation is that concentration is 0.01-2.0mol.dm
-3Weak ammonia.
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| CN101948634A (en) * | 2010-09-06 | 2011-01-19 | 天津工业大学 | Preparation method of cadmium carbonate-Trypan blue composite nanorod bundle by reflux |
| CN104098123B (en) * | 2014-07-24 | 2016-09-07 | 北京三聚创洁科技发展有限公司 | The preparation method of one zinc oxide desulfurizer |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1088183A (en) * | 1993-12-09 | 1994-06-22 | 张安沅 | One-stage process of preparing basic zinc carbonate by metathetical reaction |
| CN1270144A (en) * | 2000-04-30 | 2000-10-18 | 杨国华 | Process for preparing high-purity active zinc oxide by immersing in ammonia water and ammonium carbonate solution and complexing |
| JP2001342021A (en) * | 2000-05-31 | 2001-12-11 | Hakusui Tech Co Ltd | Method of preparing zinc oxide fine particles |
| JP2002201024A (en) * | 2000-12-27 | 2002-07-16 | Hakusui Tech Co Ltd | Method for producing compound microparticle comprising zinc oxide as main component |
| US6555075B2 (en) * | 2001-05-23 | 2003-04-29 | Raymond Lee Nip | Method of preparing zinc carbonate |
| CN1456693A (en) * | 2003-05-19 | 2003-11-19 | 南京铅锌银矿业有限责任公司 | Method for producing low-stacking density nano-zinc oxide by ammonia leaching method |
-
2005
- 2005-01-21 CN CNB2005100311834A patent/CN100343165C/en not_active Expired - Fee Related
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1088183A (en) * | 1993-12-09 | 1994-06-22 | 张安沅 | One-stage process of preparing basic zinc carbonate by metathetical reaction |
| CN1270144A (en) * | 2000-04-30 | 2000-10-18 | 杨国华 | Process for preparing high-purity active zinc oxide by immersing in ammonia water and ammonium carbonate solution and complexing |
| JP2001342021A (en) * | 2000-05-31 | 2001-12-11 | Hakusui Tech Co Ltd | Method of preparing zinc oxide fine particles |
| JP2002201024A (en) * | 2000-12-27 | 2002-07-16 | Hakusui Tech Co Ltd | Method for producing compound microparticle comprising zinc oxide as main component |
| US6555075B2 (en) * | 2001-05-23 | 2003-04-29 | Raymond Lee Nip | Method of preparing zinc carbonate |
| CN1456693A (en) * | 2003-05-19 | 2003-11-19 | 南京铅锌银矿业有限责任公司 | Method for producing low-stacking density nano-zinc oxide by ammonia leaching method |
Non-Patent Citations (2)
| Title |
|---|
| 碱式碳酸锌热分解机理及动力学 马正先等，中国工程科学，第5卷第10期 2003 * |
| 碱式碳酸锌煅烧制备纳米氧化锌 张宪玺等，无机化学学报，第18卷第10期 2002 * |
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