CN102992293A - Rod-shaped zirconium phosphate and preparation method thereof - Google Patents
Rod-shaped zirconium phosphate and preparation method thereof Download PDFInfo
- Publication number
- CN102992293A CN102992293A CN 201110272640 CN201110272640A CN102992293A CN 102992293 A CN102992293 A CN 102992293A CN 201110272640 CN201110272640 CN 201110272640 CN 201110272640 A CN201110272640 A CN 201110272640A CN 102992293 A CN102992293 A CN 102992293A
- Authority
- CN
- China
- Prior art keywords
- zirconium phosphate
- preparation
- shaped
- rod
- bar
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Images
Landscapes
- Catalysts (AREA)
Abstract
The invention relates to a rod-shaped zirconium phosphate and a preparation method thereof. The diameter of the rod-shaped zirconium phosphate is 0.4-1.0mum, and a length-diameter ratio is 5-20. The preparation method comprises the specific steps that: certain amounts of zirconium oxychloride octahydrate, oxalic acid, phosphoric acid and ethylenediamine are sequentially added in deionized water; a reaction is carried out under stirring; and pump-filtration, washing, and drying are carried out, such that the rod-shaped zirconium phosphate is obtained. a molar ratio of zirconium oxychloride octahydrate to oxalic acid to phosphoric acid to ethylenediamine is 1: a: 1: b. a corresponds to a molar ratio of oxalic acid, and is 3-5. b corresponds to a molar ratio of ethylenediamine, and is 3-5. a and b are integers or non-integers. The preparation method has the advantage of simple process, and uniform sizes of prepared rod-shaped zirconium phosphate. The rod-shaped zirconium phosphate can be applied in fields such that catalysis, ion exchange, and the like, and can be used as an antibacterial agent carrier.
Description
Technical field
The present invention relates to a kind of zirconium phosphate and preparation method thereof, particularly relate to a kind of bar-shaped zirconium phosphate and preparation method thereof, prepared bar-shaped zirconium phosphate can be applicable to the fields such as catalysis, ion-exchange, belongs to inorganic materials and synthesis technical field.
Technical background
Zirconium phosphate has stronger catalysis, absorption and ion-exchange performance, is widely used in ion exchanger, particularly as the carrier of carrying silver antimicrobials.Zirconium phosphate mainly contains three kinds of methods, and a kind of is the circumfluence method that was proposed in 1964 by Clearfield, and the method is dissolved in eight water zirconium oxychlorides in the hydrochloric acid, add phosphoric acid and hydrochloric acid mixed solution, reaction refluxed 1～7 day, adopted strong acid condition in the building-up process, long reaction time.Another kind is the direct precipitation method of G.Alberti proposition, perhaps is fluorine coordination method, and the method adds hydrofluoric acid as complexing agent, forms with zirconium oxychloride first and comparatively stablizes co-ordination complex, and then deviate from fluorion generation zirconium phosphate with phosphatase reaction.Use a large amount of hydrofluoric acid for overcoming the standby zirconium phosphate of this traditional fluorine coordination legal system, temperature of reaction is high, long reaction time, the defective of condition harshness has document that a kind of a small amount of hydrofluoric acid and strong phosphoric acid only used is provided, temperature of reaction is lower, the method for preparing zirconium phosphate that reaction times is short, disclosed method is specially in the document: soluble in water at the 1mol zirconates, add 1～2mol hydrofluoric acid and 2～3mol phosphoric acid, stirred 2～4 hours at 60～90 ℃, prepare the sheet zirconium phosphate.The conversion rate of zirconium phosphate has been accelerated in the introducing of hydrofluoric acid, and still, the use of severe corrosive hydrofluoric acid has high erosion resistance to requiring equipment, thereby increases equipment cost, and there are potential safety hazard in producers and environment.Another is the hydrothermal crystallization method that is subject in recent years research worker's extensive concern, after the method is fully mixed zirconates strong phosphoric acid etc., move into reacting by heating in stainless steel or the tetrafluoroethylene reactor, temperature of reaction generally is higher than 180 ℃, reaction process produces high pressure, equipment material and stopping property etc. are required height, and counter investment is large, and the production cycle is also longer.
The present invention overcomes the defective that exists in the existing technology of preparing of the above zirconium phosphate, provide the bar-shaped zirconium phosphate preparation method under a kind of mild conditions: at first use oxalic acid and quadrol as reaction promotor, building-up process is only used a small amount of phosphoric acid (mol ratio of phosphoric acid and zirconium oxychloride is 1: 1), temperature of reaction is 20～40 ℃, near room temperature condition, and the reaction times is short.This method has low for equipment requirements, and is with short production cycle, but the advantages such as Effective Raise output.
Summary of the invention
The present invention is directed to and use a large amount of strong phosphoric acid or deep-etching hydrofluoric acid in traditional zirconium phosphate preparation process, the shortcoming of the severe reaction conditions such as temperature of reaction height and long reaction time, use oxalic acid and quadrol have been proposed as reaction promotor, the phosphoric acid consumption is less, a kind of zirconium phosphate preparation method under the gentle conditions such as temperature of reaction is low, and the time is short, feature of the present invention is that also prepared zirconium phosphate is bar-shaped, can be applicable to the fields such as catalysis, ion-exchange, particularly can be used as carrier.
The invention provides a kind of bar-shaped zirconium phosphate, it is characterized in that, the diameter of bar-shaped zirconium phosphate is 0.4～1.0um, and length-to-diameter ratio is 5～20.
The invention provides a kind of preparation method of bar-shaped zirconium phosphate, it is characterized in that, be sequentially added into eight water zirconium oxychlorides, oxalic acid, phosphoric acid and quadrol in deionized water, stirring reaction is through obtaining bar-shaped zirconium phosphate after suction filtration, washing, the drying.
Wherein eight water zirconium oxychlorides, oxalic acid, phosphoric acid, quadrol molar ratio are 1: a: 1: b, and the corresponding oxalic acid molar ratio of a wherein, value is 3～5; The corresponding quadrol molar ratio of b, value is that 3～5, a, b are integer, or non-integer.
Temperature of reaction is 20～40 ℃, and mixing speed is 150～300rpm, and the reaction times is 3～8 hours; Drying temperature is 60～100 ℃.
This preparation method's technique is simple, and prepared bar-shaped zirconium phosphate size uniform can be applicable to the fields such as catalysis, ion-exchange, particularly can be used as carrier.
Description of drawings
The zirconium phosphate stereoscan photograph that Fig. 1 embodiment 1 is prepared;
The zirconium phosphate stereoscan photograph that Fig. 2 embodiment 2 is prepared;
The zirconium phosphate stereoscan photograph that Fig. 3 Comparative Examples is prepared.
Embodiment
Two specific embodiments of the present invention and Comparative Examples are described below, but content of the present invention is not limited to this.
Embodiment 1
The 16.1g eight water zirconium oxychlorides, 25.2g oxalic acid, 4.9g phosphoric acid and the 13.5g quadrol that in the 350ml deionized water, are sequentially added into, at 30 ℃ of lower stirring reaction 3h, stir speed (S.S.) 250rpm, after crossing suction filtration, washing, 80 ℃ of dryings, obtain bar-shaped zirconium phosphate, such as Fig. 1, the zirconium phosphate diameter is about 500nm, and length-to-diameter ratio is about 15.
Embodiment 2
The 16.1g eight water zirconium oxychlorides, 25.2g oxalic acid, 4.9g phosphoric acid and the 13.5g quadrol that in the 350ml deionized water, are sequentially added into, at 30 ℃ of lower stirring reaction 6h, stir speed (S.S.) 250rpm, after crossing suction filtration, washing, 80 ℃ of dryings, obtain bar-shaped zirconium phosphate, such as Fig. 2, the zirconium phosphate diameter is about 750nm, and length-to-diameter ratio is about 10.
Comparative Examples
The 16.1g eight water zirconium oxychlorides, 12.6g oxalic acid, 4.9g phosphoric acid and the 13.5g quadrol that in the 350ml deionized water, are sequentially added into, at 30 ℃ of lower stirring reaction 3h, stir speed (S.S.) 250rpm, after crossing suction filtration, washing, 80 ℃ of dryings, obtain non-bar-shaped zirconium phosphate, such as Fig. 3, zirconium phosphate is about 200nm, wide 70nm.
Claims (4)
1. a bar-shaped zirconium phosphate is characterized in that, the diameter of bar-shaped zirconium phosphate is 0.4～1.0um, and length-to-diameter ratio is 5～20.
2. the preparation method of a kind of bar-shaped zirconium phosphate according to claim 1, it is characterized in that, be sequentially added into eight water zirconium oxychlorides, oxalic acid, phosphoric acid and quadrol in deionized water, stirring reaction is through obtaining bar-shaped zirconium phosphate after suction filtration, washing, the drying.
3. the preparation method of a kind of bar-shaped zirconium phosphate according to claim 2, it is characterized in that, eight water zirconium oxychlorides, oxalic acid, phosphoric acid, quadrol molar ratio are 1: a: 1: b, the corresponding oxalic acid molar ratio of a wherein, value is the corresponding quadrol molar ratio of 3～5, b, and value is 3～5, a, b are integer, or non-integer.
4. the preparation method of a kind of bar-shaped zirconium phosphate according to claim 2 is characterized in that, temperature of reaction is 20～40 ℃, and mixing speed is 150～300rpm, and the reaction times is 3～8 hours, and drying temperature is 60～100 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201110272640 CN102992293A (en) | 2011-09-15 | 2011-09-15 | Rod-shaped zirconium phosphate and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201110272640 CN102992293A (en) | 2011-09-15 | 2011-09-15 | Rod-shaped zirconium phosphate and preparation method thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN102992293A true CN102992293A (en) | 2013-03-27 |
Family
ID=47921501
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 201110272640 Pending CN102992293A (en) | 2011-09-15 | 2011-09-15 | Rod-shaped zirconium phosphate and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102992293A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103832991A (en) * | 2014-03-03 | 2014-06-04 | 湖南雅城新材料发展有限公司 | Preparation method of iron phosphate nano material |
| CN105858631A (en) * | 2016-04-08 | 2016-08-17 | 山东理工大学 | Simple method for preparing acicular zirconium hydrogen phosphate |
| CN112142027A (en) * | 2020-09-17 | 2020-12-29 | 赣州瑞德化工有限公司 | Preparation method of nano layered zirconium phosphate and silver-loaded zirconium phosphate thereof |
-
2011
- 2011-09-15 CN CN 201110272640 patent/CN102992293A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103832991A (en) * | 2014-03-03 | 2014-06-04 | 湖南雅城新材料发展有限公司 | Preparation method of iron phosphate nano material |
| CN103832991B (en) * | 2014-03-03 | 2015-11-25 | 湖南雅城新材料发展有限公司 | A kind of preparation method of iron phosphate nano material |
| CN105858631A (en) * | 2016-04-08 | 2016-08-17 | 山东理工大学 | Simple method for preparing acicular zirconium hydrogen phosphate |
| CN112142027A (en) * | 2020-09-17 | 2020-12-29 | 赣州瑞德化工有限公司 | Preparation method of nano layered zirconium phosphate and silver-loaded zirconium phosphate thereof |
| CN112142027B (en) * | 2020-09-17 | 2022-03-29 | 赣州瑞德化工有限公司 | Preparation method of nano layered zirconium phosphate and silver-loaded zirconium phosphate thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102992397B (en) | Preparation method for rare earth element-doped titanium dioxide nano material | |
| CN102580721B (en) | Method for preparing TiO2/BiVO4 composite photocatalyst by MH method | |
| CN103991891B (en) | The preparation method of flake nano cerium oxide | |
| CN103172101B (en) | Preparation method of alkali-type cerous carbonate | |
| CN103787418A (en) | Method for preparing WO3.H2O hollow sphere assembled by nanosheets | |
| CN102910654A (en) | Preparation method of fibrous boehmite with large specific surface area and large pore area | |
| CN103101896A (en) | Cubic zirconium phosphate and preparation method thereof | |
| CN102992293A (en) | Rod-shaped zirconium phosphate and preparation method thereof | |
| CN105130805A (en) | Alcohol ether carboxylate preparation method | |
| CN102408102A (en) | Preparation method of nanometer iron phosphate | |
| CN106315690A (en) | Porous cobalt tetroxide nanosheet and preparation method thereof | |
| CN101445228B (en) | Spherical nano-aluminum phosphate powder and preparation method | |
| CN101544402B (en) | Nanometer zirconia sol and preparation method thereof | |
| CN103787408B (en) | A kind of preparation method of trifluoro oxygen titanium acid ammonium | |
| CN102134089A (en) | Fusiform large-scale cerium based composite oxide powder and preparation method thereof | |
| CN101759221A (en) | Method for preparing nano cerium dioxide powder | |
| CN102992376A (en) | Preparation method of sheet-shaped nano-grade cerium oxide | |
| CN101781796A (en) | Simple method for preparing hydroxyapatite nanocrystals | |
| CN103349976B (en) | Preparation method for two-dimensional ultrathin mesh-shaped ZnO nano photocatalyst | |
| CN105152192A (en) | Preparation method of magnesium oxide/rare-earth oxide core-shell-structure flower-like nano composite material | |
| CN103771482B (en) | A kind of preparation method of high-purity nanometer yttrium aluminium garnet powder | |
| CN103204554A (en) | Method for preparing spherical nickel hydroxide | |
| CN102659170A (en) | Room temperature solid-phase synthesis method for platy zinc oxide nanometer powder | |
| CN102120596B (en) | Method for preparing aluminum hydroxide by utilizing precipitation method | |
| CN102923757A (en) | Method for preparing ZnO Nano-rods |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20130327 |