CN107032398A - A kind of preparation technology of metal zirconia sol - Google Patents
A kind of preparation technology of metal zirconia sol Download PDFInfo
- Publication number
- CN107032398A CN107032398A CN201710421282.6A CN201710421282A CN107032398A CN 107032398 A CN107032398 A CN 107032398A CN 201710421282 A CN201710421282 A CN 201710421282A CN 107032398 A CN107032398 A CN 107032398A
- Authority
- CN
- China
- Prior art keywords
- metal
- zirconia sol
- quaternary ammonium
- preparation technology
- zirconium
- 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.)
- Withdrawn
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G25/00—Compounds of zirconium
- C01G25/02—Oxides
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention belongs to metal working technical area there is provided a kind of preparation technology of metal zirconia sol, including：Zirconium compounds is carried out to 10 20min of heating at 63 100 DEG C in the aqueous medium containing quaternary ammonium carbonate, zirconium metal salt solution is obtained；By obtained zirconium metal salt solution at 30 40 DEG C, it is electrolysed, hydrolyzes zirconium metal salt solution；Hydrolyzate carries out hydro-thermal process at 130 220 DEG C, you can.The present invention carries out hydro-thermal process by hydrolyzing, being electrolysed and heat aging by metallic compounds such as zirconates in the basic conditions, so as to manufacture the method for the metal zirconia sol of the stabilization of particle diameter distribution unanimously.
Description
Technical field
The invention belongs to metal working technical area, in particular it relates to a kind of preparation technology of metal zirconia sol.
Background technology
Conventional method, as the method for obtaining metal oxide sol, such as zirconia sol, there is heating hydrolysis zirconates water
The method of solution, into zirconium saline solution add aqueous hydrogen peroxide solution and the method that is heated and in basic region
Heat method of zirconium hydroxide etc..
But many methods are the manufacture methods that the metallic compound of zirconates etc. is hydrolyzed and heated under acid range.But
Be, the metal oxide sol such as zirconia sol manufactured using this method be when only pH is in acidic region it is stable, when
PH is when neutrality is into basic region, and its viscosity rises or occurred gelation, it is impossible to be used in be used as the purposes of colloidal sol.In addition,
In the acid that the metal oxide sol of the zirconia sol etc. is used for as smears etc. in the occasion of metal based material, colloidal sol
Cause etching problem, it is difficult to use, therefore, it is intended that a kind of zirconia sol stable in neutral or basic region of exploitation etc.
Metal oxide sol.
In addition, using ammonium carbonate, alkali metal hydroxide, the side in the basic conditions hydrolyzing the metallic compounds such as zirconates
In method, although generation particle, but process over time, substantial amounts of precipitum is produced, becomes slurry, it is impossible to is obtained completely
Stable colloidal sol.
The content of the invention
For defect of the prior art, it is an object of the invention to provide a kind of preparation technology of metal zirconia sol,
By hydrolyzing, being electrolysed and heat aging by metallic compounds such as zirconates in the basic conditions, and then hydro-thermal process is carried out, so that
The method for manufacturing the metal zirconia sol of the stabilization of particle diameter distribution unanimously.
A kind of preparation technology of the metal zirconia sol provided according to the present invention, the preparation of the metal zirconia sol
Technique comprises the following steps：
（1）Zirconium compounds is subjected to heating 10-20min at 63-100 DEG C in the aqueous medium containing quaternary ammonium carbonate, obtained
Obtain zirconium metal salt solution；
（2）Will（1）In obtained zirconium metal salt solution at 30-40 DEG C, be electrolysed, hydrolyze zirconium metal salt solution；
（3）Hydrolyzate carries out hydro-thermal process at 130-220 DEG C, you can.
Preferably, the quaternary ammonium carbonate is（NR4）2CO3Or NR4HCO3, it is described it is various in R be alkyl.
Preferably, the quaternary ammonium ion in described quaternary ammonium carbonate is made up of carbon number for 4-13 alkyl.
Preferably, the quaternary ammonium ion in the quaternary ammonium carbonate is made up of carbon number for 2-3 alkyl.
Preferably, washing procedure is carried out after described hydro-thermal process.
Preferably, enrichment process is also carried out after described washing procedure.
Preferably, the pH after the enrichment process is 9-10.
Preferably, the voltage applied during the electrolysis is between 2-20V, and current strength is in 0.21-0.4A/cm2Between.
Compared with prior art, the present invention has following beneficial effect：
The preparation technology of metal zirconia sol of the present invention comprises the following steps：（1）Containing the aqueous of quaternary ammonium carbonate
Zirconium compounds is subjected to heating 10-20min at 63-100 DEG C in medium, zirconium metal salt solution is obtained；（2）Will（1）In be made
Zirconium metal salt solution at 30-40 DEG C, be electrolysed, make zirconium metal salt solution hydrolyze；（3）Hydrolyzate is at 130-220 DEG C
Carry out hydro-thermal process, you can.By in the heats metalized compound of alkaline aqueous medium containing quaternary ammonium carbonate, companion on one side
Have the generation of the gases such as amine and carbon dioxide while being hydrolyzed, metal ion or cationic metal compound by with
Stabilized from the interaction of the quaternary ammonium ion of quaternary ammonium carbonate.By the way that the hydrolyzate of this state is carried out at hydro-thermal
Reason, can manufacture stable alkaline metal oxide sol.Simultaneously by the zirconium metal salt solution of acquisition at 30-40 DEG C, carry out
Electrolysis so that metal zirconium oxide Stability of Sols.
The alkaline metal oxide sol that the present invention is obtained, can be used in various uses.Zirconia sol can be used for
Such as the ceramics and sensor raw material of electronic material, smears, the Composite material of ceramics, fire resistance products formed, casting mold
In adhesive, grinding agent etc..
Embodiment
With reference to specific embodiment, the present invention is expanded on further.It should be understood that these embodiments are merely to illustrate the present invention
Rather than limitation the scope of the present invention.
It is an object of the invention to provide a kind of preparation technology of metal zirconia sol, by the basic conditions by zirconates
Deng metallic compound hydrolysis, it is electrolysed and heat aging, and then carries out hydro-thermal process, so as to manufactures the stabilization of particle diameter distribution unanimously
Metal zirconia sol method.
A kind of preparation technology of the metal zirconia sol provided according to the present invention, the preparation of the metal zirconia sol
Technique comprises the following steps：
（1）Zirconium compounds is subjected to heating 10-20min at 63-100 DEG C in the aqueous medium containing quaternary ammonium carbonate, obtained
Obtain zirconium metal salt solution；
（2）Will（1）In obtained zirconium metal salt solution at 30-40 DEG C, be electrolysed, hydrolyze zirconium metal salt solution；
（3）Hydrolyzate carries out hydro-thermal process at 130-220 DEG C, you can.
Preferably, the quaternary ammonium carbonate is（NR4）2CO3Or NR4HCO3, it is described it is various in R be alkyl.
Preferably, the quaternary ammonium ion in described quaternary ammonium carbonate is made up of carbon number for 4-13 alkyl.
Preferably, the quaternary ammonium ion in the quaternary ammonium carbonate is made up of carbon number for 2-3 alkyl.
Preferably, washing procedure is carried out after described hydro-thermal process.
Preferably, enrichment process is also carried out after described washing procedure.
Preferably, the pH after the enrichment process is 9-10.
Preferably, the voltage applied during the electrolysis is between 2-20V, and current strength is in 0.21-0.4A/cm2Between.
Compared with prior art, the present invention has following beneficial effect：
The preparation technology of metal zirconia sol of the present invention comprises the following steps：（1）Containing the aqueous of quaternary ammonium carbonate
Zirconium compounds is subjected to heating 10-20min at 63-100 DEG C in medium, zirconium metal salt solution is obtained；（2）Will（1）In be made
Zirconium metal salt solution at 30-40 DEG C, be electrolysed, make zirconium metal salt solution hydrolyze；（3）Hydrolyzate is at 130-220 DEG C
Carry out hydro-thermal process, you can.By in the heats metalized compound of alkaline aqueous medium containing quaternary ammonium carbonate, companion on one side
Have the generation of the gases such as amine and carbon dioxide while being hydrolyzed, metal ion or cationic metal compound by with
Stabilized from the interaction of the quaternary ammonium ion of quaternary ammonium carbonate.By the way that the hydrolyzate of this state is carried out at hydro-thermal
Reason, can manufacture stable alkaline metal oxide sol.Simultaneously by the zirconium metal salt solution of acquisition at 30-40 DEG C, carry out
Electrolysis so that metal zirconium oxide Stability of Sols.
The alkaline metal oxide sol that the present invention is obtained, can be used in various uses.Zirconia sol can be used for
Such as the ceramics and sensor raw material of electronic material, smears, the Composite material of ceramics, fire resistance products formed, casting mold
In adhesive, grinding agent etc..
Embodiment 1
A kind of preparation technology for metal zirconia sol that the present embodiment is provided, the preparation technology bag of the metal zirconia sol
Include following steps：
（1）Zirconium compounds is subjected to heating 10min at 100 DEG C in the aqueous medium containing quaternary ammonium carbonate, zirconium gold is obtained
Belong to salting liquid；
（2）Will（1）In obtained zirconium metal salt solution at 40 DEG C, be electrolysed, hydrolyze zirconium metal salt solution；
（3）Hydrolyzate carries out hydro-thermal process at 130 DEG C, you can.
The quaternary ammonium carbonate is（NR4）2CO3Or NR4HCO3, it is described it is various in R be alkyl.
Quaternary ammonium ion in described quaternary ammonium carbonate is made up of carbon number for 13 alkyl.
Quaternary ammonium ion in the quaternary ammonium carbonate is made up of carbon number for 2 alkyl.
Washing procedure is carried out after described hydro-thermal process.
Enrichment process is also carried out after described washing procedure.
PH after the enrichment process is 9-10.
The voltage applied during the electrolysis is 21, and current strength is 0.31A/cm2。
Embodiment 2
A kind of preparation technology for metal zirconia sol that the present embodiment is provided, the preparation technology bag of the metal zirconia sol
Include following steps：
（1）Zirconium compounds is subjected to heating 10-20min at 63 DEG C in the aqueous medium containing quaternary ammonium carbonate, zirconium is obtained
Metal salt solution；
（2）Will（1）In obtained zirconium metal salt solution at 40 DEG C, be electrolysed, hydrolyze zirconium metal salt solution；
（3）Hydrolyzate carries out hydro-thermal process at 130 DEG C, you can.
The quaternary ammonium carbonate is（NR4）2CO3Or NR4HCO3, it is described it is various in R be alkyl.
Quaternary ammonium ion in described quaternary ammonium carbonate is made up of carbon number for 13 alkyl.
Quaternary ammonium ion in the quaternary ammonium carbonate is made up of carbon number for 2 alkyl.
Washing procedure is carried out after described hydro-thermal process.
Enrichment process is also carried out after described washing procedure.
PH after the enrichment process is 10.
The voltage applied during the electrolysis is 21, and current strength is 0.22A/cm2。
Embodiment 3
A kind of preparation technology for metal zirconia sol that the present embodiment is provided, the preparation technology bag of the metal zirconia sol
Include following steps：
（1）Zirconium compounds is subjected to heating 10-20min at 90 DEG C in the aqueous medium containing quaternary ammonium carbonate, zirconium is obtained
Metal salt solution；
（2）Will（1）In obtained zirconium metal salt solution at 35 DEG C, be electrolysed, hydrolyze zirconium metal salt solution；
（3）Hydrolyzate carries out hydro-thermal process at 170 DEG C, you can.
The quaternary ammonium carbonate is（NR4）2CO3Or NR4HCO3, it is described it is various in R be alkyl.
Quaternary ammonium ion in described quaternary ammonium carbonate is made up of carbon number for 9 alkyl.
Quaternary ammonium ion in the quaternary ammonium carbonate is made up of carbon number for 2 alkyl.
Washing procedure is carried out after described hydro-thermal process.
Enrichment process is also carried out after described washing procedure.
PH after the enrichment process is 9-10.
The voltage applied during the electrolysis is 15, and current strength is 0.25A/cm2。
Embodiment 4
A kind of preparation technology for metal zirconia sol that the present embodiment is provided, the preparation technology bag of the metal zirconia sol
Include following steps：
（1）Zirconium compounds is subjected to heating 10-20min at 90 DEG C in the aqueous medium containing quaternary ammonium carbonate, zirconium is obtained
Metal salt solution；
（2）Will（1）In obtained zirconium metal salt solution at 38 DEG C, be electrolysed, hydrolyze zirconium metal salt solution；
（3）Hydrolyzate carries out hydro-thermal process at 170 DEG C, you can.
The quaternary ammonium carbonate is（NR4）2CO3Or NR4HCO3, it is described it is various in R be alkyl.
Quaternary ammonium ion in described quaternary ammonium carbonate is made up of carbon number for 9 alkyl.
Quaternary ammonium ion in the quaternary ammonium carbonate is made up of carbon number for 3 alkyl.
Washing procedure is carried out after described hydro-thermal process.
Enrichment process is also carried out after described washing procedure.
PH after the enrichment process is 9-10.
The voltage applied during the electrolysis is 11, and current strength is 0.33A/cm2。
The specific embodiment of the present invention is described above.It is to be appreciated that the invention is not limited in above-mentioned
Particular implementation, those skilled in the art can make various deformations or amendments within the scope of the claims, this not shadow
Ring the substantive content of the present invention.
Claims (8)
1. a kind of preparation technology of metal zirconia sol, it is characterised in that：The preparation technology bag of the metal zirconia sol
Include following steps：
Zirconium compounds is subjected to heating 10-20min at 63-100 DEG C in the aqueous medium containing quaternary ammonium carbonate, zirconium is obtained
Metal salt solution；
Will（1）In obtained zirconium metal salt solution at 30-40 DEG C, be electrolysed, hydrolyze zirconium metal salt solution；
（3）Hydrolyzate carries out hydro-thermal process at 130-220 DEG C, you can.
2. the preparation technology of metal zirconia sol according to claim 1, it is characterised in that：The quaternary ammonium carbonate is
（NR4）2CO3Or NR4HCO3, it is described it is various in R be alkyl.
3. the preparation technology of metal zirconia sol according to claim 1, it is characterised in that：Described quaternary ammonium carbonate
In quaternary ammonium ion be made up of carbon number for 4-13 alkyl.
4. the preparation technology of metal zirconia sol according to claim 1, it is characterised in that：In the quaternary ammonium carbonate
Quaternary ammonium ion be made up of carbon number for 2-3 alkyl.
5. the preparation technology of metal zirconia sol according to claim 1, it is characterised in that：In described hydro-thermal process
Washing procedure is carried out afterwards.
6. the preparation technology of metal zirconia sol according to claim 5, it is characterised in that：Described washing procedure it
Enrichment process is also carried out afterwards.
7. the preparation technology of metal zirconia sol according to claim 6, it is characterised in that：After the enrichment process
PH be 9-10.
8. the preparation technology of metal zirconia sol according to claim 1, it is characterised in that：Apply during the electrolysis
Voltage between 2-20V, current strength is in 0.21-0.4A/cm2Between.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710421282.6A CN107032398A (en) | 2017-06-07 | 2017-06-07 | A kind of preparation technology of metal zirconia sol |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710421282.6A CN107032398A (en) | 2017-06-07 | 2017-06-07 | A kind of preparation technology of metal zirconia sol |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN107032398A true CN107032398A (en) | 2017-08-11 |
Family
ID=59541785
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710421282.6A Withdrawn CN107032398A (en) | 2017-06-07 | 2017-06-07 | A kind of preparation technology of metal zirconia sol |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN107032398A (en) |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1072740A (en) * | 1991-11-30 | 1993-06-02 | 默克专利股份有限公司 | Use preparation of metal oxide sols by electrolysis |
| CN101031512A (en) * | 2004-08-17 | 2007-09-05 | 日产化学工业株式会社 | Method for producing metal oxide sol |
| CN101208268A (en) * | 2005-06-29 | 2008-06-25 | 日产化学工业株式会社 | Process for production of alkaline zirconia sol |
| CN102037160A (en) * | 2008-03-20 | 2011-04-27 | 魁北克钛铁公司 | Electrochemical process for the recovery of metallic iron and chlorine values from iron-rich metal chloride wastes |
-
2017
- 2017-06-07 CN CN201710421282.6A patent/CN107032398A/en not_active Withdrawn
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1072740A (en) * | 1991-11-30 | 1993-06-02 | 默克专利股份有限公司 | Use preparation of metal oxide sols by electrolysis |
| CN101031512A (en) * | 2004-08-17 | 2007-09-05 | 日产化学工业株式会社 | Method for producing metal oxide sol |
| CN101208268A (en) * | 2005-06-29 | 2008-06-25 | 日产化学工业株式会社 | Process for production of alkaline zirconia sol |
| CN102037160A (en) * | 2008-03-20 | 2011-04-27 | 魁北克钛铁公司 | Electrochemical process for the recovery of metallic iron and chlorine values from iron-rich metal chloride wastes |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| JP2018538224A (en) | Airgel sheet manufacturing method and apparatus | |
| CN106698446A (en) | Low-cost method for preparing aerogel by means of atmospheric pressure drying | |
| CN109415214A (en) | The preparation method of aerosil felt and the aerosil felt thus prepared | |
| CN104760964A (en) | Silicon dioxide aerogel preparation method | |
| CN102701221B (en) | Method for preparing nano white carbon black from coal gangue | |
| CN104016717A (en) | Preparation method of zirconium-silicate-coated cerium sulfide scarlet pigment and product prepared by same | |
| CN108790012A (en) | Aluminum based resin composite material and preparation method | |
| CN108380144A (en) | A kind of Al2O3-SiO2The preparation method of composite aerogel | |
| CN104402197A (en) | Low water content quartz glass material preparation method | |
| CN104909375A (en) | Method for rapidly preparing hydrophobicsilica aerogel by carbon dioxidesubcritical drying method | |
| CN110565366A (en) | Preparation method of silicon aerogel composite material | |
| CN108975366A (en) | A kind of macropore boehmite and preparation method thereof | |
| CN107032398A (en) | A kind of preparation technology of metal zirconia sol | |
| CN104525064B (en) | A kind of alkaline silica sol and preparation method thereof | |
| JP2005179111A (en) | Method for manufacturing zirconia sol | |
| CN103183377B (en) | Method for hydrolyzing low-concentration self-generating crystal seed in process of preparing titanium dioxide by sulfuric acid method | |
| CN111320180A (en) | Preparation method of silicon dioxide aerogel | |
| CN109850868A (en) | A kind of preparation method and application of silica modified porous Lauxite base carbon ball | |
| CN106148962A (en) | The treatment fluid of a kind of stainless steel surface nano hole and application process thereof | |
| CN107128933A (en) | A kind of supercritical drying preparation method of aerosil heat-barrier material | |
| CN106084311B (en) | A kind of method for preparing oxide-Chitosan Composites and oxide-Chitosan Composites | |
| CN108752046A (en) | A kind of dipping method preparing isostatic pressing formed graphite product | |
| CN105366944B (en) | A kind of preparation method of reflective glass beads | |
| CN103254783B (en) | A kind of aqueous surface-treating agent and preparation method thereof | |
| CN103922709B (en) | Al2O3/TiC core/shell structure powder preparation method |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| WW01 | Invention patent application withdrawn after publication |
Application publication date: 20170811 |
|
| WW01 | Invention patent application withdrawn after publication |