CN104817315A - Sodium zirconium silicate powder and preparation method thereof - Google Patents
Sodium zirconium silicate powder and preparation method thereof Download PDFInfo
- Publication number
- CN104817315A CN104817315A CN201510170672.1A CN201510170672A CN104817315A CN 104817315 A CN104817315 A CN 104817315A CN 201510170672 A CN201510170672 A CN 201510170672A CN 104817315 A CN104817315 A CN 104817315A
- Authority
- CN
- China
- Prior art keywords
- zirconium silicate
- dioxide
- zirconium
- powder
- raw material
- 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
Abstract
The invention discloses a sodium zirconium silicate powder and its preparation method. The molecular formula of the sodium zirconium silicate powder is Na2ZrSi3O9. Raw materials comprise silicon dioxide, zirconium dioxide and sodium silicate, and molar ratio of silicon dioxide to zirconium dioxide to sodium silicate is 2:1:1. Purity of the sodium zirconium silicate powder prepared after ball milling and calcining of the above raw materials is greater than or equal to 99.5%. Mass percentage of Fe2O3 in the sodium zirconium silicate powder is less than or equal to 0.01%, and mass percentage of TiO2 is less than or equal to 0.0005%. The sodium zirconium silicate powder has high purity and low impurity content. The preparation method is simple and can meet high-quality requirement of the sodium zirconium silicate powder in various fields.
Description
Technical field
The present invention relates to a kind of Chemicals, be specifically related to a kind of zirconium silicate powder and preparation method thereof.
Background technology
Zirconium silicate (Na
2zrSi
3o
9) be a kind of important Chemicals, can be used for the ramming mass at the positions such as the melting end of glass furnace, fining end and kiln wall, also can be used for the tanning agent of leather sector and the industrial chemicals as opticglass.
To have with zirconium English powder (zirconium silicate), sodium carbonate and sodium hydroxide for raw material in prior art, prepare sodium silico-zirconate (Na
2zrSiO
3).Because in zirconium English powder, impurity is many, if prepare zirconium silicate (Na in this way
2zrSi
3o
9), zirconium silicate (Na will be had a strong impact on
2zrSi
3o
9) whiteness of product and purity.According to the raw material of this zirconium silicate product as opticglass, TiO wherein
2and Fe
2o
3glass will be caused seriously painted Deng impurity, increase photoabsorption.Therefore, highly purified zirconium silicate (Na is prepared
2zrSi
3o
9) very important.
Summary of the invention
The present invention proposes a kind of zirconium silicate powder and preparation method thereof, it is high that its main purpose is to provide a kind of purity, the zirconium silicate powder that foreign matter content is few, and the preparation method simple to operate of this zirconium silicate powder, to meet the multi-field high-quality requirement to zirconium silicate powder.
On the one hand, the invention provides a kind of zirconium silicate powder, its molecular formula is Na
2zrSi
3o
9, its raw material is silicon-dioxide, zirconium dioxide and water glass, and the mol ratio of described raw material is silicon-dioxide: zirconium dioxide: water glass=2:1:1.
As preferably, described raw material through ball milling, calcine and obtain zirconium silicate powder.
As preferably, the ball grinder of zirconium dioxide material put into by described raw material, and puts into zirconium dioxide abrading-ball and deionized water and carry out ball milling and obtain slurry, namely obtains described zirconium silicate powder after the solid calcining obtained after slurry solid-liquid separation.
As preferably, the volume ratio of described raw material and deionized water is 1:1-1:2.
As preferably, during ball milling, the rotating speed of described ball grinder is 50-80rpm, and the time of ball milling is 24-30h.
As preferably, the temperature of described calcining is 1400-1500 DEG C, and the time of calcining is 5-8h.
As preferably, purity >=99.5% of silicon-dioxide in described raw material, granularity≤100 μm; Purity >=99.99% of zirconium dioxide, granularity≤10 μm; Purity >=99.5% of water glass, granularity≤100 μm.
As preferably, purity>=99.5% of this zirconium silicate powder, Fe in this zirconium silicate powder
2o
3mass percentage≤0.01%, TiO
2mass percentage≤0.0005%.
On the other hand, the invention provides a kind of zirconium silicate raw powder's production technology, comprise the following steps:
(1) be silicon-dioxide by mol ratio: zirconium dioxide: the ball grinder of zirconium dioxide material put into by the raw material of water glass=2:1:1, and put into zirconium dioxide abrading-ball and deionized water and carry out ball milling and obtain slurry;
(2) solid-liquid separation is carried out to described slurry, the solid after being separated is calcined, obtains described zirconium silicate powder.
As preferably, purity >=99.5% of silicon-dioxide in described raw material, granularity≤100 μm; Purity >=99.99% of zirconium dioxide, granularity≤10 μm; Purity >=99.5% of water glass, granularity≤100 μm.
As preferably, the volume ratio of described raw material and deionized water is 1:1-1:2.
As preferably, during ball milling, the rotating speed of described ball grinder is 50-80rpm, and the time of ball milling is 24-30h.
As preferably, the temperature of described calcining is 1400-1500 DEG C, and the time of calcining is 5-8h.
As preferably, the molecular formula of the zirconium silicate powder prepared according to the method is Na
2zrSi
3o
9.
As preferably, according to purity>=99.5% of zirconium silicate powder prepared by the method, Fe in this zirconium silicate powder
2o
3mass percentage≤0.01%, TiO
2mass percentage≤0.0005%.
Compared with prior art, beneficial effect of the present invention is:
(1) zirconium silicate (Na for preparing of the present invention
2zrSi
3o
9) purity>=99.5% of powder, Fe in this zirconium silicate powder
2o
3mass percentage≤0.01%, TiO
2mass percentage≤0.0005%, can meet multi-field to zirconium silicate (Na
2zrSi
3o
9) the high-quality requirement of powder.
(2) zirconium silicate (Na provided by the invention
2zrSi
3o
9) raw powder's production technology is simple to operate, without the need to carrying out chemical removal of iron, process environmental protection.
Accompanying drawing explanation
Fig. 1 is zirconium silicate (Na
2zrSi
3o
9) powder XRD figure spectrum, wherein X-coordinate is diffraction angle 2 θ, and ordinate zou is diffracted intensity.
Embodiment
Below in conjunction with specific embodiment, the present invention is described in further detail, but not as a limitation of the invention.
Embodiment
With the silicon-dioxide of purity >=99.5%, the zirconium dioxide of purity >=99.99%, the water glass of purity >=99.5% is raw material, and the mol ratio of this raw material is silicon-dioxide: zirconium dioxide: water glass=2:1:1, raw material ball mill carries out ball milling, and wherein the material of ball grinder is zirconium dioxide material.Ball grinder put into by raw material, and puts into zirconium dioxide abrading-ball and deionized water, obtains slurry after ball milling, and the volume ratio of its Raw and deionized water is 1:1-1:2, and the rotating speed of ball grinder is 50-80rpm, and the time of ball milling is 24-30h; After adopting whizzer to carry out solid-liquid separation to this slurry, in High Temperature Furnaces Heating Apparatus, carry out calcining thermal treatment to the solid after separation, the temperature of wherein calcining is 1400-1500 DEG C, and the time of calcining is 5-8h, obtains zirconium silicate (Na
2zrSi
3o
9) powder.
Varigrained raw material is adopted to prepare zirconium silicate (Na by above-mentioned preparation method
2zrSi
3o
9) powder, concrete technology parameter and synthetic effect are in table 1.
Table 1. zirconium silicate (Na
2zrSi
3o
9) preparation technology parameter of powder and purity
As can be seen from Table 1, the embodiment of the present invention is with the silicon-dioxide of purity>=99.5%, granularity≤100 μm, the zirconium dioxide of purity>=99.99%, granularity≤10 μm, the water glass of purity>=99.5%, granularity≤100 μm is raw material, the zirconium silicate (Na prepared according to the processing condition that embodiment is given
2zrSi
3o
9) purity of powder is high, is not less than 99.5%, and Fe
2o
3mass percentage≤0.01%, TiO
2mass percentage≤0.0005%; Zirconium silicate (Na prepared by comparative example
2zrSi
3o
9) purity of powder all lower than 99.5%, the service requirements of follow-up high-quality cannot be met.
Accompanying drawing 1 is zirconium silicate (Na prepared by embodiment 2
2zrSi
3o
9) powder XRD figure spectrum, can find out, diffraction peak is Na
2zrSi
3o
9corresponding peak, does not find other crystalline phase diffraction peak, and illustrate and adopt this processing parameter, silicon-dioxide, zirconium dioxide and water glass react completely.
Granularity≤100 μm of silicon-dioxide in the raw material that the embodiment of the present invention uses, granularity≤10 μm of zirconium dioxide, during granularity≤100 μm of water glass, can prepare the zirconium silicate (Na of purity>=99.5%
2zrSi
3o
9) powder.When the granularity of the raw material used is greater than these scopes, obtained zirconium silicate (Na
2zrSi
3o
9) purity of powder is lower than 99.5%.Raw material granularity is large, causes ball milling insufficient, and during calcining, raw material reaction is incomplete, final obtained zirconium silicate (Na
2zrSi
3o
9) powder purity is lower.
The volume ratio of embodiment of the present invention Raw and deionized water controls at 1:1-1:2, is conducive to preparing highly purified zirconium silicate (Na
2zrSi
3o
9) powder, avoid amount of water few and amount of water is many time the ball milling that causes insufficient.
In the embodiment of the present invention, the rotating speed of ball grinder controls as 50-80rpm, and the time controling of ball milling is 24-30h, is conducive to preparing highly purified zirconium silicate (Na
2zrSi
3o
9) powder, avoid the ball milling that the low and Ball-milling Time of the rotating speed of ball grinder causes in short-term insufficient, and the energy consumption increase caused when the rotating speed of ball grinder is high and Ball-milling Time is long and efficiency low.
The temperature of calcining in the embodiment of the present invention controls, for 1400-1500 DEG C, when the time controling of calcining is 5-8h, to be conducive to preparing highly purified zirconium silicate (Na
2zrSi
3o
9) powder, avoid the low raw material reaction caused in short-term with calcination time of calcining temperature not exclusively, and the energy consumption caused when calcining temperature is high and calcination time is long increases.
What finally illustrate is, above embodiment is only in order to illustrate technical scheme of the present invention and unrestricted, although with reference to preferred embodiment to invention has been detailed description, those of ordinary skill in the art is to be understood that, can modify to technical scheme of the present invention or equivalent replacement, and not departing from aim and the scope of technical solution of the present invention, it all should be encompassed in the middle of right of the present invention.
Claims (10)
1. a zirconium silicate powder, its molecular formula is Na
2zrSi
3o
9, it is characterized in that, its raw material is silicon-dioxide, zirconium dioxide and water glass, and the mol ratio of described raw material is silicon-dioxide: zirconium dioxide: water glass=2:1:1.
2. zirconium silicate powder according to claim 1, is characterized in that, described raw material through ball milling, calcine and obtain zirconium silicate powder.
3. zirconium silicate powder according to claim 2, it is characterized in that, the ball grinder of zirconium dioxide material put into by described raw material, and puts into zirconium dioxide abrading-ball and deionized water and carry out ball milling and obtain slurry, namely obtains described zirconium silicate powder after the solid calcining obtained after slurry solid-liquid separation.
4. zirconium silicate powder according to claim 3, is characterized in that, the volume ratio of described raw material and deionized water is 1:1-1:2; During ball milling, the rotating speed of described ball grinder is 50-80rpm, and the time of ball milling is 24-30h.
5. zirconium silicate powder according to claim 1, is characterized in that, purity >=99.5% of silicon-dioxide in described raw material, granularity≤100 μm; Purity >=99.99% of zirconium dioxide, granularity≤10 μm; Purity >=99.5% of water glass, granularity≤100 μm.
6. a zirconium silicate raw powder's production technology, comprises the following steps:
(1) be silicon-dioxide by mol ratio: zirconium dioxide: the ball grinder of zirconium dioxide material put into by the raw material of water glass=2:1:1, and put into zirconium dioxide abrading-ball and deionized water and carry out ball milling and obtain slurry;
(2) solid-liquid separation is carried out to described slurry, the solid after being separated is calcined, obtains described zirconium silicate powder.
7. zirconium silicate raw powder's production technology according to claim 6, is characterized in that, purity >=99.5% of silicon-dioxide in described raw material, granularity≤100 μm; Purity >=99.99% of zirconium dioxide, granularity≤10 μm; Purity >=99.5% of water glass, granularity≤100 μm.
8. zirconium silicate raw powder's production technology according to claim 6, is characterized in that, the volume ratio of described raw material and deionized water is 1:1-1:2.
9. zirconium silicate raw powder's production technology according to claim 6, is characterized in that, during ball milling, the rotating speed of described ball grinder is 50-80rpm, and the time of ball milling is 24-30h.
10. zirconium silicate raw powder's production technology according to claim 6, is characterized in that, the temperature of described calcining is 1400-1500 DEG C, and the time of calcining is 5-8h.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510170672.1A CN104817315A (en) | 2015-04-10 | 2015-04-10 | Sodium zirconium silicate powder and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510170672.1A CN104817315A (en) | 2015-04-10 | 2015-04-10 | Sodium zirconium silicate powder and preparation method thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN104817315A true CN104817315A (en) | 2015-08-05 |
Family
ID=53727826
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510170672.1A Pending CN104817315A (en) | 2015-04-10 | 2015-04-10 | Sodium zirconium silicate powder and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104817315A (en) |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6117595A (en) * | 1997-02-25 | 2000-09-12 | Agency Of Industrial Science & Technology And Ministry Of International Trade & Industry | High sodium ion conducting inorganic composite solid electrolyte and method for production thereof |
| CN104379252A (en) * | 2012-03-12 | 2015-02-25 | 大塚化学株式会社 | Exhaust gas purification catalyst, exhaust gas purification device and filter, and production method for said catalyst |
-
2015
- 2015-04-10 CN CN201510170672.1A patent/CN104817315A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6117595A (en) * | 1997-02-25 | 2000-09-12 | Agency Of Industrial Science & Technology And Ministry Of International Trade & Industry | High sodium ion conducting inorganic composite solid electrolyte and method for production thereof |
| CN104379252A (en) * | 2012-03-12 | 2015-02-25 | 大塚化学株式会社 | Exhaust gas purification catalyst, exhaust gas purification device and filter, and production method for said catalyst |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN108675327B (en) | Preparation method of low-sodium submicron calcined alumina | |
| CN104386719B (en) | A kind of preparation method of Alpha-alumina | |
| CN102020302A (en) | Method for reducing content of sodium in aluminum hydroxide | |
| CN104528834B (en) | Artificial rutile mether liquor recycling novel method | |
| CN109824072B (en) | Method for preparing alumina by using industrial waste residues | |
| CN102001693B (en) | Process for preparing light magnesium oxide and calcium carbonate powder by utilizing dolomite acid method | |
| CN105294138A (en) | Doublet aluminum oxide micropowder and preparation method thereof | |
| CN106220190A (en) | A kind of method utilizing aluminous fly-ash to prepare mullite | |
| CN102502722A (en) | Preparation method of high-purity magnesium oxide | |
| CN1281499C (en) | Process for producing high purity magnesia | |
| CN105776254A (en) | Technology for preparing lithium carbonate by means of recycling of slag obtained in purifying process of lepidolite | |
| EA035062B1 (en) | Extraction of products from titanium-bearing minerals | |
| CN103204641A (en) | Purification method for low-grade magnesite via hydration | |
| CN104894636A (en) | Preparation method of potassium octatitanate whisker | |
| US9676635B2 (en) | Method for producing aqueous zirconium chloride solution | |
| CN104016334A (en) | Purification method for graphite | |
| CN109437264A (en) | A method of aluminium oxide is prepared from mentioning in lithium waste residue | |
| CN102001705A (en) | Process for synthesizing calcium zirconate by liquid-phase and solid-phase mixed calcination method | |
| CN101417806A (en) | Silicon micropowder and preparation method thereof | |
| CN104817315A (en) | Sodium zirconium silicate powder and preparation method thereof | |
| CN102303887A (en) | Production method for special strontium chloride for liquid crystal | |
| CN1686812A (en) | Method for producing alumina | |
| CN101863508A (en) | High-purity mixed-crystal titanium pigment and production method thereof | |
| CN105039702A (en) | Leaching method for valuable elements in quadratic aluminum dust | |
| CN109053181A (en) | A kind of calcium hexaluminate lightweight Materials with High Strength and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| EXSB | Decision made by sipo to initiate substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20150805 |
|
| RJ01 | Rejection of invention patent application after publication |