CN103803647B - A kind of preparation method of high purity electronic-grade rutile titanium dioxide - Google Patents
A kind of preparation method of high purity electronic-grade rutile titanium dioxide Download PDFInfo
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- CN103803647B CN103803647B CN201410101426.6A CN201410101426A CN103803647B CN 103803647 B CN103803647 B CN 103803647B CN 201410101426 A CN201410101426 A CN 201410101426A CN 103803647 B CN103803647 B CN 103803647B
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- titanium dioxide
- high purity
- rutile titanium
- preparation
- grade rutile
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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims abstract description 34
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- XJDNKRIXUMDJCW-UHFFFAOYSA-J titanium tetrachloride Chemical compound Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 0.000 claims abstract description 11
- 229920002125 Sokalan® Polymers 0.000 claims abstract description 7
- 239000007788 liquid Substances 0.000 claims abstract description 7
- 239000004584 polyacrylic acid Substances 0.000 claims abstract description 7
- 238000000926 separation method Methods 0.000 claims abstract description 7
- 238000010438 heat treatment Methods 0.000 claims abstract description 4
- 239000002253 acid Substances 0.000 claims description 12
- 239000002002 slurry Substances 0.000 claims description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims description 9
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- 239000002245 particle Substances 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 3
- 239000000498 cooling water Substances 0.000 claims description 3
- 238000012423 maintenance Methods 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 229920000058 polyacrylate Polymers 0.000 claims description 3
- 239000000463 material Substances 0.000 abstract description 4
- 235000000340 Solanum pseudocapsicum Nutrition 0.000 abstract 1
- 235000001978 Withania somnifera Nutrition 0.000 abstract 1
- 240000004482 Withania somnifera Species 0.000 abstract 1
- 238000010298 pulverizing process Methods 0.000 abstract 1
- 238000005245 sintering Methods 0.000 abstract 1
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 5
- 239000004408 titanium dioxide Substances 0.000 description 5
- 229910052742 iron Inorganic materials 0.000 description 4
- 239000000843 powder Substances 0.000 description 4
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 3
- 239000010931 gold Substances 0.000 description 3
- 229910052737 gold Inorganic materials 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- -1 iron ion Chemical class 0.000 description 3
- 238000000034 method Methods 0.000 description 3
- 239000002086 nanomaterial Substances 0.000 description 3
- 239000012071 phase Substances 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 229910021645 metal ion Inorganic materials 0.000 description 2
- 239000011858 nanopowder Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 2
- 229910010413 TiO 2 Inorganic materials 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 230000002547 anomalous effect Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 238000000975 co-precipitation Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 239000004973 liquid crystal related substance Substances 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000002159 nanocrystal Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 description 1
- 239000002957 persistent organic pollutant Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 238000012876 topography Methods 0.000 description 1
Landscapes
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention discloses a kind of preparation method of high purity electronic-grade rutile titanium dioxide, comprise six steps such as preparation polyacrylic acid saddle solution, preparation titanium tetrachloride solution, Hybrid Heating, partially by the emperor himself wintercherry material, solid-liquid separation, high temperature sintering, pulverizing, high purity electronic-grade rutile titanium dioxide.The purity of prepared rutile titanium dioxide reaches more than 99.9%.
Description
Technical field
The invention belongs to technical field of inorganic material, be specifically related to a kind of preparation method of high purity electronic-grade rutile titanium dioxide.
Background technology
Titanium dioxide is one of important metal oxide, can be widely used in the industry such as plastics, papermaking, printing-ink, chemical fibre, rubber and makeup.Along with the rise of nano material and the development of technology of preparing, the anomalous performance that nano titanium oxide the is different from conventional powder material Application Areas of titanium dioxide is had larger expansion, as can be used as support of the catalyst degradable organic pollutant under ultraviolet irradiation, conversion solar can be electric energy, gas sensor, pressure-active element, the enhancement additive of polymkeric substance, complex function ceramic material structure, nonlinear optical material etc.At present, people, in order to obtain it, have done some and have attempted and effort, as " a kind of preparation method of rutile phase titanium dioxide nano-powder " that disclose in Chinese invention patent application prospectus CN1631759A disclosed in 29 days June in 2005.Titanium tetrachloride preparation of raw material is become the water-sol by this preparation method, and the water-sol is thin up after overaging, then heats and make sol-hydrolysis and produce precipitation, is filtered by gained throw out, dry after rinsing with water, and obtained rutile phase titanium dioxide nano-powder.But this preparation method has unsatisfactory part, first, the particle shape of obtained nano TiO 2 powder is irregular; Secondly, operation is more, causes production process numerous and diverse, and the cost of preparation is increased; Again, Ti in whole reaction process
4+concentration very low, make the productive rate of powder also very low, and only realize in laboratory, still have certain distance apart from suitability for industrialized production.
Because a lot of high-tech area requires very tight especially to iron contamination to nano rutile-type titanium dioxide foreign matter content, prepare at liquid crystal material especially, sophisticated sensor and space flight, the fields such as aviation coating, thus propose very high request to preparing high pure gold redrock nano material, because nano material specific surface area is very large, the electrostatic adsorption of nanoparticle surface metal ion is very strong, usual employing high temperature gas phase method and liquid phase method all do not solve very well, though many bibliographical information liquid phase synthesis gold redrock nano titanium oxide are had existing, see that patent discloses 00119033.4, 1530327A is first colloidal sol processed or collosol and gel substantially, or introduce crystal seed and low temperature obtain solution, the crystallization temperature low reaction time is long, by adding the modes such as alkali adjustment thus causing metallic impurity co-precipitation, cannot metallic impurity in removal system, especially iron ion impurity composition, prior art can not overcome metal ion very well at the electrostatic adhesion of nanocrystal surface and the iron ion that can not fully wash away in solution, be difficult to prepare iron ion content thus and be less than 10ppm, and can be controlled to 3-5ppm, even be less than 3ppm, high pure gold redrock nano-titanium dioxide quality matetrial.
Summary of the invention
The technical problem to be solved in the present invention is the shortcoming and defect overcoming above-mentioned prior art, provides a kind of preparation method of nano size Titania.
To achieve these goals, the technical scheme that the present invention takes is:
A preparation method for high purity electronic-grade rutile titanium dioxide, it is characterized in that, step is as follows:
Step one choose purity be more than 99.9% titanium tetrachloride add a certain amount of deionized water, be mixed with the titanium tetrachloride solution that mass ratio is 1:1;
Step 2 choose purity be more than 99.9% ammonium polyacrylate add a certain amount of deionized water, be mixed with 2 ‰ ~ 2% polyacrylic acid ammonium solution;
Above-mentioned titanium tetrachloride solution and polyacrylic acid ammonium solution by after 2: 1 mixing and stirring, are heated to 90 DEG C by step 3, and average rate stirs maintenance 40 minutes, generate metatitanic acid slurry, then with below cooling water temperature to 40 DEG C;
Metatitanic acid slurry flame filter press after above-mentioned cooling is carried out solid-liquid separation by step 4, makes the water ratio of metatitanic acid slurry reach less than 50%;
Metatitanic acid slurry after solid-liquid separation with after saggar dress, is placed High Temperature Furnaces Heating Apparatus and sinter 3 hours at 800 DEG C of temperature, obtain granular high purity electronic-grade rutile titanium dioxide by step 5;
The granular high purity electronic-grade rutile titanium dioxide micronizer mill sintered is pulverized by 160 object fineness by step 6, obtains: purity>=99.9%; 100 DEG C of 2hr moisture content≤0.100%; 700 DEG C of 1hr, burning decrement≤0.100%; Physical index: D
max≤ 1 μm; BET>=5m
2; Particle morphology: spherical or be similar to spherical high purity electronic-grade rutile titanium dioxide, then packs.
Accompanying drawing explanation
Fig. 1 is the SEM figure of embodiment products obtained therefrom;
Fig. 2 is process flow sheet of the present invention.
Embodiment
A preparation method for high purity electronic-grade rutile titanium dioxide, it is characterized in that, step is as follows:
Step one choose purity be more than 99.9% titanium tetrachloride add a certain amount of deionized water, be mixed with the titanium tetrachloride solution that mass ratio is 1:1;
Step 2 choose purity be more than 99.9% ammonium polyacrylate add a certain amount of deionized water, be mixed with 2 ‰ ~ 2% polyacrylic acid ammonium solution;
Above-mentioned titanium tetrachloride solution and polyacrylic acid ammonium solution by after 2: 1 mixing and stirring, are heated to 90 DEG C by step 3, and average rate stirs maintenance 40 minutes, generate metatitanic acid slurry, then with below cooling water temperature to 40 DEG C;
Metatitanic acid slurry flame filter press after above-mentioned cooling is carried out solid-liquid separation by step 4, makes the water ratio of metatitanic acid slurry reach less than 50%;
Metatitanic acid slurry after solid-liquid separation with after saggar dress, is placed High Temperature Furnaces Heating Apparatus and sinter 3 hours at 800 DEG C of temperature, obtain granular high purity electronic-grade rutile titanium dioxide by step 5;
The granular high purity electronic-grade rutile titanium dioxide micronizer mill sintered is pulverized by 160 object fineness by step 6, obtains: purity>=99.9%; 100 DEG C of 2hr moisture content≤0.100%; 700 DEG C of 1hr, burning decrement≤0.100%; Physical index: D
max≤ 1 μm; BET>=5m
2; Particle morphology: spherical or be similar to spherical high purity electronic-grade rutile titanium dioxide, then packs.
| Crystal formation | Purity | Outward appearance | Particle diameter | Surface topography |
| Rutile-type | 99.9% | White powder | 0.15μm | Spherical |
Last it is noted that obviously, above-described embodiment is only for the application's example is clearly described, and the restriction not to embodiment.For those of ordinary skill in the field, can also make other changes in different forms on the basis of the above description.Here exhaustive without the need to also giving all embodiments.And thus the apparent change of amplifying out or variation be still among the protection domain of the application's type.
Claims (1)
1. a preparation method for high purity electronic-grade rutile titanium dioxide, is characterized in that, step is as follows:
Step one choose purity be more than 99.9% titanium tetrachloride add a certain amount of deionized water, be mixed with the titanium tetrachloride solution that mass ratio is 1:1;
Step 2 choose purity be more than 99.9% ammonium polyacrylate add a certain amount of deionized water, be mixed with 2 ‰ ~ 2% polyacrylic acid ammonium solution;
Above-mentioned titanium tetrachloride solution and polyacrylic acid ammonium solution by after 2: 1 mixing and stirring, are heated to 90 DEG C by step 3, and average rate stirs maintenance 40 minutes, generate metatitanic acid slurry, then with below cooling water temperature to 40 DEG C;
Metatitanic acid slurry flame filter press after above-mentioned cooling is carried out solid-liquid separation by step 4, makes the water ratio of metatitanic acid slurry reach less than 50%;
Metatitanic acid slurry after solid-liquid separation with after saggar dress, is placed High Temperature Furnaces Heating Apparatus and sinter 3 hours at 800 DEG C of temperature, obtain granular high purity electronic-grade rutile titanium dioxide by step 5;
The granular high purity electronic-grade rutile titanium dioxide micronizer mill sintered is pulverized by 160 object fineness by step 6, obtains: purity>=99.9%; 100 DEG C of 2hr moisture content≤0.100%; 700 DEG C of 1hr, burning decrement≤0.100%; Physical index: D
max≤ 1 μm; BET>=5m
2; Particle morphology: spherical or be similar to spherical high purity electronic-grade rutile titanium dioxide, then packs.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410101426.6A CN103803647B (en) | 2014-03-19 | 2014-03-19 | A kind of preparation method of high purity electronic-grade rutile titanium dioxide |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410101426.6A CN103803647B (en) | 2014-03-19 | 2014-03-19 | A kind of preparation method of high purity electronic-grade rutile titanium dioxide |
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| Publication Number | Publication Date |
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| CN103803647A CN103803647A (en) | 2014-05-21 |
| CN103803647B true CN103803647B (en) | 2015-11-18 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108706630B (en) * | 2018-07-09 | 2020-11-06 | 江苏中研创星材料科技有限公司 | Preparation method of titanium dioxide special for lithium titanate |
| CN109911934A (en) * | 2019-04-08 | 2019-06-21 | 湖北展朋新材料股份有限公司 | A kind of rutile titanium dioxide of large specific surface area and preparation method thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1092384A (en) * | 1993-02-10 | 1994-09-21 | 泰奥塞特殊品有限公司 | The preparation method of titanium dioxide |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1092384A (en) * | 1993-02-10 | 1994-09-21 | 泰奥塞特殊品有限公司 | The preparation method of titanium dioxide |
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Address after: 433000 Hubei province Xiantao Peng Chang Industrial Park Zhanpeng Road No. 68 Patentee after: HUBEI ZHANPENG NEW MATERIAL Co.,Ltd. Address before: 433000 Hubei province Xiantao Peng Chang Industrial Park Zhanpeng Road No. 68 Patentee before: XIANTAO ZHANPENG NEW MATERIAL Co.,Ltd. |
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Address after: 433000 No. 68, Zhanpeng Road, PENGCHANG Industrial Park, Xiantao City, Hubei Province Patentee after: XIANTAO ZHANPENG NEW MATERIAL Co.,Ltd. Country or region after: China Address before: 433000 No. 68, Zhanpeng Road, PENGCHANG Industrial Park, Xiantao City, Hubei Province Patentee before: HUBEI ZHANPENG NEW MATERIAL CO.,LTD. Country or region before: China |
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Denomination of invention: A preparation method for high-purity electronic grade rutile type titanium dioxide Granted publication date: 20151118 Pledgee: Bank of China Limited Xiantao branch Pledgor: XIANTAO ZHANPENG NEW MATERIAL Co.,Ltd. Registration number: Y2024980011389 |