CN108439461A - A kind of industrialized preparing process of high-purity nm calcium titanate - Google Patents
A kind of industrialized preparing process of high-purity nm calcium titanate Download PDFInfo
- Publication number
- CN108439461A CN108439461A CN201810169077.XA CN201810169077A CN108439461A CN 108439461 A CN108439461 A CN 108439461A CN 201810169077 A CN201810169077 A CN 201810169077A CN 108439461 A CN108439461 A CN 108439461A
- Authority
- CN
- China
- Prior art keywords
- purity
- temperature
- solution
- calcium titanate
- calcium
- 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
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G23/00—Compounds of titanium
- C01G23/003—Titanates
- C01G23/006—Alkaline earth titanates
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
Abstract
The present invention is intended to provide a kind of technological process is simple, manufacturing cost is low, product purity is high, the industrialized preparing process of high-purity nm calcium titanate that is produced on a large scale.The industrialized preparing process of high-purity nm calcium titanate of the present invention includes：The calcium hydroxide solution of a concentration of 210~220g/l is added into the titanyl sulfate solution of a concentration of 195~205g/l of TiO2, and it is 95~100 DEG C that agitated heating, which maintains system temperature, keeps the temperature 15 minutes；Above-mentioned mixed liquor is put into hydro-thermal slot afterwards, is warming up to 103~108 DEG C, stir and keeps the temperature 4 hours；By plate compression three times and through desalted water washing until Fe, K, Na content are reduced to 50ppm or less；The filter cake of gained is calcined 6 hours at 580~620 DEG C again, product high-purity nm calcium titanate is made by crushing.
Description
Technical field
The invention belongs to technical field of fine, more particularly to the industrialized production side of high-purity nm calcium titanate
Law technology field.
Background technology
Calcium titanate（Calcium Tianate）For yellow crystals, it is insoluble in water.Density is 3.98g/mL（25℃）, melt
Point is 1980 DEG C.Calcium titanate belongs to cubic system, and titanium ion and six oxonium ions form octahedral coordination, ligancy 6；Calcium from
Son is located in the hole being made of octahedron, ligancy 12.It is mainly used for making middle high-pressure ceramic capacitor, PTC temperature-sensitive electricity
The precise electronics components such as resistance.Pure calcium titanate is difficult to sinter ceramics into, and 1%~2% zirconium dioxide can be added；Electronic ceramics is industrial
In manufacture monocrystalline, the basic electro-conducting element of high frequency instrument, it is used as raw material powder, such as produces dielectric material.
Currently used preparation method has：Using titanium oxide and calcium oxide as raw material, by the calcium oxide of the amount of equal substances, oxidation
Titanium and other additives are sufficiently mixed, polished extrusion forming, are calcined then at 1350 DEG C, are crushed, ground i.e. after calcining
It obtains product to mix titanium oxide and calcium oxide in water, is being sufficiently stirred lower addition oxalic acid solution, then detach, wash, is dry,
And in 925 DEG C of calcinings；Titanium tetrachloride is reacted with oxalic acid solution, oxalic acid titanium solution is first made, then it is mixed with calcium chloride solution,
Calcium oxalate titanium, filtering, drying and the calcining generation calcium titanate at 1050 DEG C is made；With calcium hydroxide and nitric acid calcium compound in
575 DEG C and titanium dioxide reaction.The above preparation method is of high cost or grain size is big or purity is not high, and technical scale metaplasia produces electron level
All there is disadvantage in calcium titanate.
Invention content
That the object of the present invention is to provide a kind of technological processes is simple, manufacturing cost is low, product purity is high, can advise
The industrialized preparing process of the high-purity nm calcium titanate of modelling production
To solve the above problems, a kind of industrialized preparing process of high-purity nm calcium titanate of the present invention, including following six step：
Step 1: preparing TiO2 a concentration of 195~205g/l, iron titanium ratio ＜ 0.18, F values are 1.95~2.05, temperature is 95~
98 DEG C of titanyl sulfate solution；
Step 2: it is 210~220g/l, the calcium hydroxide solution that temperature is 95~98 DEG C to prepare solution concentration；
Step 3: being added calcium hydroxide solution made from step 2 to step（1）The titanyl sulfate of gained
In solution, and it is 95~100 DEG C that agitated heating, which maintains system temperature, keeps the temperature 15 minutes；
Step 4: the mixed liquor of three gained of above-mentioned steps is put into hydro-thermal slot, 103~108 DEG C are warming up to,
It stirs and keeps the temperature 4 hours；
Step 5: by mixed solution described in step 4 by plate compression three times and through desalted water washing until Fe, K, Na content
It is reduced to 50ppm or less；
Step 6: the filter cake obtained by step 5 is calcined 6 hours at 580~620 DEG C, product high-purity nm is made by crushing
Calcium titanate.
As a further improvement on the present invention, the titanyl sulfate solution described in step 1 is sulfate process titanium dioxide production technology
The titanyl sulfate solution produced.
As a preference of the present invention, calcium hydroxide solution made from step 2 is added to obtained by step 1 in step 3
In titanyl sulfate solution, and it is 96 DEG C that agitated heating, which maintains system temperature,；The mixed liquor obtained by step 3 is put in step 4
Enter hydro-thermal slot, is warming up to 105 DEG C.
In summary the beneficial effects of the invention are as follows：The industrial metaplasia of high-purity nm calcium titanate of the present invention
Production method, technological process is simple, manufacturing cost is low, product purity is high, is produced on a large scale.
Specific implementation mode
The present invention will be further described for following example：
Embodiment one：
Step 1：Using sulfate process titanium dioxide production technology, extracting sulfuric acid oxygen titanium solution TiO2 a concentration of 200g/l, iron titanium ratio ＜
0.18, F value is 2.0, and the temperature of titanyl sulfate solution is 97 DEG C；
Step 2：Preparation solution concentration is 220g/l, the calcium hydroxide solution that temperature is 96 DEG C；
Step 3：Calcium hydroxide solution made from step 2 is added to the titanyl sulfate obtained by step 1
In solution, and it is 96 DEG C that agitated heating, which maintains system temperature, keeps the temperature 15 minutes；
Step 4：The mixed liquor of three gained of above-mentioned steps is put into hydro-thermal slot, 105 DEG C is warming up to, stirs and keep the temperature 4 hours；
Step 5：By mixed solution described in step 4 by plate compression three times and through desalted water washing until Fe, K, Na content
It is reduced to 50ppm or less；
Step 6：Filter cake obtained by step 5 is calcined 6 hours at 610 DEG C, product high-purity nm metatitanic acid is made by crushing
Calcium.
Embodiment two：
Step 1：Using sulfate process titanium dioxide production technology, extracting sulfuric acid oxygen titanium solution TiO2 a concentration of 195g/l, iron titanium ratio ＜
0.18, F value is 1.95, and the temperature of titanyl sulfate solution is 96 DEG C；
Step 2：Preparation solution concentration is 210g/l, the calcium hydroxide solution that temperature is 96 DEG C；
Step 3：Calcium hydroxide solution made from step 2 is added to the titanyl sulfate obtained by step 1
In solution, and it is 96 DEG C that agitated heating, which maintains system temperature, keeps the temperature 15 minutes；
Step 4：The mixed liquor of three gained of above-mentioned steps is put into hydro-thermal slot, 105 DEG C is warming up to, stirs and keep the temperature 4 hours；
Step 5：By mixed solution described in step 4 by plate compression three times and through desalted water washing until Fe, K, Na content
It is reduced to 50ppm or less；
Step 6：Filter cake obtained by step 5 is calcined 6 hours at 600 DEG C, product high-purity nm metatitanic acid is made by crushing
Calcium.
Embodiment three：
Step 1：Using sulfate process titanium dioxide production technology, extracting sulfuric acid oxygen titanium solution TiO2 a concentration of 205g/l, iron titanium ratio ＜
0.18, F value is 1.98, and the temperature of titanyl sulfate solution is 96 DEG C；
Step 2：Preparation solution concentration is 220g/l, the calcium hydroxide solution that temperature is 96 DEG C；
Step 3：Calcium hydroxide solution made from step 2 is added to the titanyl sulfate obtained by step 1
In solution, and it is 96 DEG C that agitated heating, which maintains system temperature, keeps the temperature 15 minutes；
Step 4：The mixed liquor of three gained of above-mentioned steps is put into hydro-thermal slot, 105 DEG C is warming up to, stirs and keep the temperature 4 hours；
Step 5：By mixed solution described in step 4 by plate compression three times and through desalted water washing until Fe, K, Na content
It is reduced to 50ppm or less；
Step 6：Filter cake obtained by step 5 is calcined 6 hours at 620 DEG C, product high-purity nm metatitanic acid is made by crushing
Calcium.
Claims (4)
1. a kind of industrialized preparing process of high-purity nm calcium titanate, which is characterized in that include the following steps：
Step 1：TiO2 a concentration of 195~205g/l, iron titanium ratio ＜ 0.18 are prepared, F values are 1.95~2.05, temperature is 95~
98 DEG C of titanyl sulfate solution；
Step 2：Preparation solution concentration is 210~220g/l, the calcium hydroxide solution that temperature is 95~98 DEG C；
Step 3：Calcium hydroxide solution made from step 2 is added to step（1）The titanyl sulfate of gained
In solution, and it is 95~100 DEG C that agitated heating, which maintains system temperature, keeps the temperature 15 minutes；
Step 4：The mixed liquor of three gained of above-mentioned steps is put into hydro-thermal slot, is warming up to 103~108 DEG C,
It stirs and keeps the temperature 4 hours；
Step 5：By mixed solution described in step 4 by plate compression three times and through desalted water washing until Fe, K, Na content
It is reduced to 50ppm or less；
Step 6：Filter cake obtained by step 5 is calcined 6 hours at 580~620 DEG C, product high-purity nm is made by crushing
Calcium titanate.
2. the industrialized preparing process of high-purity nm calcium titanate according to claim 1, which is characterized in that institute in step 1
It is the titanyl sulfate solution that sulfate process titanium dioxide production technology is produced to state titanyl sulfate solution.
3. the industrialized preparing process of high-purity nm calcium titanate according to claim 1, which is characterized in that the step 3
It is middle that calcium hydroxide solution made from step 2 is added into the titanyl sulfate solution obtained by step 1, and agitated heating maintains
System temperature is 96 DEG C.
4. the industrialized preparing process of high-purity nm calcium titanate according to claim 1 or 3, which is characterized in that the step
The mixed liquor obtained by step 3 is put into hydro-thermal slot in rapid four, is warming up to 105 DEG C.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810169077.XA CN108439461A (en) | 2018-02-28 | 2018-02-28 | A kind of industrialized preparing process of high-purity nm calcium titanate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810169077.XA CN108439461A (en) | 2018-02-28 | 2018-02-28 | A kind of industrialized preparing process of high-purity nm calcium titanate |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN108439461A true CN108439461A (en) | 2018-08-24 |
Family
ID=63193170
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201810169077.XA Pending CN108439461A (en) | 2018-02-28 | 2018-02-28 | A kind of industrialized preparing process of high-purity nm calcium titanate |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN108439461A (en) |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4520004A (en) * | 1982-09-08 | 1985-05-28 | Sony Corporation | Method of manufacturing metal titanate fine powder |
| CN102139914A (en) * | 2011-04-20 | 2011-08-03 | 浙江大学 | Method for preparing calcium titanate nanoparticles |
| CN106915766A (en) * | 2015-12-25 | 2017-07-04 | 兰州大学 | A kind of preparation method of butterfly-like shape calcium titanate particle |
| CN107469760A (en) * | 2017-09-28 | 2017-12-15 | 江苏大学 | A kind of nanometer CaTiO3Powder adsorbent and its preparation method and application |
| CN107487782A (en) * | 2017-09-29 | 2017-12-19 | 兰州理工大学 | A kind of CaTiO3The preparation method of nanometer pane |
-
2018
- 2018-02-28 CN CN201810169077.XA patent/CN108439461A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4520004A (en) * | 1982-09-08 | 1985-05-28 | Sony Corporation | Method of manufacturing metal titanate fine powder |
| CN102139914A (en) * | 2011-04-20 | 2011-08-03 | 浙江大学 | Method for preparing calcium titanate nanoparticles |
| CN106915766A (en) * | 2015-12-25 | 2017-07-04 | 兰州大学 | A kind of preparation method of butterfly-like shape calcium titanate particle |
| CN107469760A (en) * | 2017-09-28 | 2017-12-15 | 江苏大学 | A kind of nanometer CaTiO3Powder adsorbent and its preparation method and application |
| CN107487782A (en) * | 2017-09-29 | 2017-12-19 | 兰州理工大学 | A kind of CaTiO3The preparation method of nanometer pane |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Yang et al. | Preparation of rutile titania nanocrystals by liquid method at room temperature | |
| KR20080078864A (en) | Methods for production of metal oxide nano particles, and nano particles and preparations produced thereby | |
| CN101888973A (en) | Nanoparticulate composition and method for the production thereof | |
| JPS60155532A (en) | Production of barium strontium titanate fine particle | |
| CN105271378A (en) | Preparation method of tetragonal barium titanate with high tetragonal rate | |
| KR20080080350A (en) | Methods for production of metal oxide nano particles with controlled properties, and nano particles and preparations produced thereby | |
| CN101348938A (en) | Preparation of nano barium titanate powder | |
| CN105439196A (en) | Low-temperature preparation method of high-tetragonal-phase-content nano barium titanate powder | |
| JP2726439B2 (en) | Method for producing ceramic powder having perovskite structure | |
| CN113744991B (en) | Co2Z type ferrite material and preparation method and application thereof | |
| KR101621831B1 (en) | Ultrafine particles of titanium dioxide and process for producing the same | |
| JPS61146710A (en) | Production of fine barium titanate particle of high purity | |
| CN108439461A (en) | A kind of industrialized preparing process of high-purity nm calcium titanate | |
| CN101573297A (en) | Processes for the flux calcination production of titanium dioxide | |
| CN106564936A (en) | Preparation method of titanium dioxide conductive powder | |
| JPS6272525A (en) | Production of barium titanate or strontium titanate | |
| WO2013018742A1 (en) | Barium titanate, strontium titanate, and manufacturing method for alkaline earth metal carbonate | |
| JPS61141619A (en) | Production of zirconia fine powder | |
| JPS623004A (en) | Production of easily sintering perovskite raw material powder by wet method | |
| JPH0388720A (en) | Production of titanyl barium oxalate particles | |
| KR100503858B1 (en) | Preparation of Nano-sized Crystalline Titanic Acid Strontium Powder from Aqueous Titanium Tetrachloride and Strontium Carbonate Solutions Prepared by Use of Inorganic Acids | |
| CN102730767B (en) | Rapid preparation method of nano alpha-iron oxide powder | |
| KR101792278B1 (en) | A method of preparing barium titanate powder and barium titanate powder prepared by same | |
| KR20000001995A (en) | Process for preparing ceramic powder of barium titanate | |
| KR20060102928A (en) | Manufacturing method of barium titanate powder |
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 | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20180824 |
|
| RJ01 | Rejection of invention patent application after publication |