CN106745220A - A kind of preparation technology of high-purity titanium dioxide - Google Patents
A kind of preparation technology of high-purity titanium dioxide Download PDFInfo
- Publication number
- CN106745220A CN106745220A CN201710007034.7A CN201710007034A CN106745220A CN 106745220 A CN106745220 A CN 106745220A CN 201710007034 A CN201710007034 A CN 201710007034A CN 106745220 A CN106745220 A CN 106745220A
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- Prior art keywords
- titanium dioxide
- purity
- preparation technology
- refining agent
- speed centrifugation
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G23/00—Compounds of titanium
- C01G23/04—Oxides; Hydroxides
- C01G23/047—Titanium dioxide
- C01G23/0475—Purification
-
- 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 invention discloses a kind of preparation technology of high-purity titanium dioxide, it is characterized in that, during titanium dioxide raw material put into refining agent I, refining agent I is 2: 1~5: 1 with the mass ratio of titanium dioxide raw material, ultrasonic irradiation shakes 3h~6h, temperature control is in 30 DEG C~40 DEG C, filtration under diminished pressure after high speed centrifugation；During cake solids are put into refining agent II, refining agent II is 2: 1~5: 1 with the mass ratio of cake solids, ultrasonic irradiation concussion 5h~10h, and temperature control is in 30 DEG C~50 DEG C, filtration under diminished pressure after high speed centrifugation；The solid that will be obtained is washed 2~3 times in putting into deionized water, high speed centrifugation, and depressurize suction filtration, and filter cake is pressed dry, and more than 10h is vacuum dried at 100 DEG C~120 DEG C, obtains the titanium dioxide product of purity more than 99.99%.The present invention utilizes 99% titanium dioxide, refines purification, directly prepares 99.99% high-purity titanium dioxide.Operation is easy, and equipment investment is low.
Description
Technical field
The present invention relates to a kind of preparation technology of high-purity titanium dioxide, belong to technical field of preparation for inorganic material.
Background technology
Titanium dioxide is a kind of important Inorganic Chemicals, and tool has been widely used.Can be used as catalyst carrier, light to urge
Change media and anti-ultraviolet radiation protection medium.Simultaneously in coating, plastics, screen glass bulb, medical treatment, cosmetics, purification of air, Shui Chu
The aspects such as reason also have different purposes.Recent new material development is accelerated, and titanium dioxide is more and more wider as functional material application.With
Titanium dioxide is in new energy, gas sensor, particularly nonlinear optics, sophisticated sensor, effective catalyst, space flight and aviation coating
Etc. the further investigation and application of high-tech area, to titanium dioxide impurity content and purity use requirement more and more higher.
At present report high-purity titanium dioxide preparation method, mainly have sulfuric acid process, titanium tetrachloride hydrolysis method, chloridising and
Titanium alkoxides Hydrolyze method, such as CN101074112B, CN101445270A, CN103803647B, CN104477987B,
CN102030367A etc..These open methods are both needed to by chemical process, or even multistep reaction prepares high-purity titanium dioxide, generally
There is tedious process, equipment requirement high, complex process, production cost deficiency and defect high.Process route is anti-because being related to simultaneously
Process is answered, larger environmental pressure is brought to scale industrial production, do not meet the friendly chemistry theme of the green vigorously advocated at present.
To avoid the deficiency in prior art path, in the urgent need to developing a kind of effective ways for preparing high-purity titanium dioxide.Research is high
The preparation technology of pure titinium dioxide, for meeting the use demand of current new material, high-tech area to high-purity titanium dioxide, tool
It is significant.
The content of the invention
Problem to be solved by this invention is to provide the high-purity two that a kind of technique is easy, product purity is high, environment-friendly
The preparation method of titanium oxide, meets specific demand of the domestic and international high-tech area to high-purity titanium dioxide.
In order to solve the above problems, the invention provides a kind of preparation technology of high-purity titanium dioxide, it is characterised in that
Specific steps include：
The first step：During titanium dioxide raw material put into refining agent I, refining agent I is 2 with the mass ratio of titanium dioxide raw material
: 1~5: 1, ultrasonic irradiation concussion 3h~6h, temperature control is in 30 DEG C~40 DEG C, filtration under diminished pressure after high speed centrifugation；
Second step：During cake solids obtained by the first step are put into refining agent II, the matter of refining agent II and cake solids
Amount than be 2: 1~5: 1, ultrasonic irradiation concussion 5h~10h, temperature control at 30 DEG C~50 DEG C, filtration under diminished pressure after high speed centrifugation；
3rd step：Washed 2~3 times during the solid that second step is obtained is put into deionized water, high speed centrifugation, decompression is taken out
Filter, filter cake is pressed dry, and more than 10h is vacuum dried at 100 DEG C~120 DEG C, obtains the titanium dioxide product of purity more than 99.99%.
Preferably, the titanium dioxide raw material specification in the first step is AR grades, purity 99%.
Preferably, the refining agent I in the first step is electronic grade hydrochloric acid deionized water wiring solution-forming, and mass concentration is
5%~10%.
Preferably, the refining agent II in the second step is electronic grade nitric acid deionized water wiring solution-forming, mass concentration
It is 10%~15%.
Preferably, deionized water and the mass ratio of titanium dioxide raw material are 3: 1~5: 1 in the 3rd step.
Preferably, the ultrasonic irradiation ultrasonic frequency that uses of concussion in the first step and second step for 35kHz~
53kHz。
Compared with prior art, the beneficial effects of the invention are as follows：
1st, the present invention combines ultrasonic irradiation cavitation and imitates with the titanium dioxide of content 99% as raw material using refining agent washing
Should, raw material impurity is efficiently removed, the high-purity titanium dioxide of purity 99.99% is directly obtained.
2nd, process proposed by the present invention, is not related to product to chemically react in itself, and operational sequence is easy, equipment investment is low
Remarkable advantage, for prepare high-purity titanium dioxide product provide a new way.
Specific embodiment
To become apparent the present invention, hereby with preferred embodiment, it is described in detail below.
Embodiment 1
A kind of preparation technology of high-purity titanium dioxide, concretely comprises the following steps：
The first step：The titanium dioxide of 600g contents 99% is put into the refining agent I (electronics that 1200g mass concentrations are 10%
Grade hydrochloric acid deionized water wiring solution-forming) in, ultrasonic irradiation concussion 3h, ultrasonic frequency is 35kHz, and temperature control is at 30 DEG C
~40 DEG C, filtration under diminished pressure after high speed centrifugation obtains cake solids；
Second step：Cake solids obtained by the first step are put into refining agent II (the electron level nitre that 3000g concentration is 15%
Deionized water wiring solution-forming use in acid) in, ultrasonic irradiation shakes 10h, and ultrasonic frequency is 53kHz, temperature control 30 DEG C~
50 DEG C, filtration under diminished pressure after high speed centrifugation obtains cake solids；
3rd step：Washed 2~3 times during the solid that second step is obtained is put into 3000g deionized waters, high speed centrifugation subtracts
Pressure suction filtration, filter cake is pressed dry, and 10h is vacuum dried at 100 DEG C, obtains 547g titanium dioxide products, purity 99.994%.
Embodiment 2
A kind of preparation method of high-purity titanium dioxide, concretely comprises the following steps：
The first step：The titanium dioxide of 1400g contents 99% is put into the refining agent I (electronics that 7000g mass concentrations are 5%
Grade hydrochloric acid deionized water wiring solution-forming) in, ultrasonic irradiation concussion 6h, ultrasonic frequency is 53kHz, and temperature control is at 30 DEG C
~40 DEG C, filtration under diminished pressure after high speed centrifugation obtains cake solids；
Second step：Cake solids obtained by the first step are put into refining agent II (the electron level nitre that 2800g concentration is 10%
Deionized water wiring solution-forming is used in acid) in, ultrasonic irradiation concussion 5h, ultrasonic frequency is 35kHz, and temperature control is 30 DEG C~50
DEG C, filtration under diminished pressure after high speed centrifugation obtains cake solids；
3rd step：Washed 2~3 times during the solid that second step is obtained is put into 4200g deionized waters, high speed centrifugation subtracts
Pressure suction filtration, filter cake is pressed dry, and 15h is vacuum dried at 120 DEG C, obtains 1284g titanium dioxide products, purity 99.991%.
Claims (6)
1. a kind of preparation technology of high-purity titanium dioxide, it is characterised in that specific steps include：
The first step：During titanium dioxide raw material put into refining agent I, the mass ratio of refining agent I and titanium dioxide raw material for 2: 1~
5: 1, ultrasonic irradiation concussion 3h~6h, temperature control is in 30 DEG C~40 DEG C, filtration under diminished pressure after high speed centrifugation；
Second step：During cake solids obtained by the first step are put into refining agent II, the mass ratio of refining agent II and cake solids
It is 2: 1~5: 1, ultrasonic irradiation concussion 5h~10h, temperature control is in 30 DEG C~50 DEG C, filtration under diminished pressure after high speed centrifugation；
3rd step：Washed 2~3 times during the solid that second step is obtained is put into deionized water, high speed centrifugation, depressurize suction filtration, filter
Cake is pressed dry, and more than 10h is vacuum dried at 100 DEG C~120 DEG C, obtains the titanium dioxide product of purity more than 99.99%.
2. the preparation technology of high-purity titanium dioxide as claimed in claim 1, it is characterised in that the dioxy in the first step
It is AR grades, purity 99% to change titanium material specification.
3. the preparation technology of high-purity titanium dioxide as claimed in claim 1, it is characterised in that refined in the first step
Agent I is electronic grade hydrochloric acid deionized water wiring solution-forming, and mass concentration is 5%~10%.
4. the preparation technology of high-purity titanium dioxide as claimed in claim 1, it is characterised in that refined in the second step
Agent II is electronic grade nitric acid deionized water wiring solution-forming, and mass concentration is 10%~15%.
5. the preparation technology of high-purity titanium dioxide as claimed in claim 1, it is characterised in that deionization in the 3rd step
Water is 3: 1~5: 1 with the mass ratio of titanium dioxide raw material.
6. the preparation technology of high-purity titanium dioxide as claimed in claim 1, it is characterised in that the first step and second step
In the ultrasonic irradiation ultrasonic frequency that uses of concussion be 35kHz~53kHz.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201710007034.7A CN106745220A (en) | 2017-01-05 | 2017-01-05 | A kind of preparation technology of high-purity titanium dioxide |
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| CN201710007034.7A CN106745220A (en) | 2017-01-05 | 2017-01-05 | A kind of preparation technology of high-purity titanium dioxide |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107324404A (en) * | 2017-08-15 | 2017-11-07 | 上海阿拉丁生化科技股份有限公司 | A kind of preparation method of the cobalt oxide of high-purity four |
| CN107381648A (en) * | 2017-08-15 | 2017-11-24 | 上海阿拉丁生化科技股份有限公司 | Preparation method of high-purity manganese dioxide |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101417814A (en) * | 2008-11-21 | 2009-04-29 | 桂林工学院 | Method for preparing one-dimensional red schorl type nanocrystalline titanic oxide |
| CN104386755A (en) * | 2014-11-06 | 2015-03-04 | 上海晶纯生化科技股份有限公司 | Preparation method of high-purity tungstic acid |
-
2017
- 2017-01-05 CN CN201710007034.7A patent/CN106745220A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101417814A (en) * | 2008-11-21 | 2009-04-29 | 桂林工学院 | Method for preparing one-dimensional red schorl type nanocrystalline titanic oxide |
| CN104386755A (en) * | 2014-11-06 | 2015-03-04 | 上海晶纯生化科技股份有限公司 | Preparation method of high-purity tungstic acid |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107324404A (en) * | 2017-08-15 | 2017-11-07 | 上海阿拉丁生化科技股份有限公司 | A kind of preparation method of the cobalt oxide of high-purity four |
| CN107381648A (en) * | 2017-08-15 | 2017-11-24 | 上海阿拉丁生化科技股份有限公司 | Preparation method of high-purity manganese dioxide |
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Application publication date: 20170531 |