CN108190946A - A kind of method for preparing high-purity sulfuric acid oxygen titanium crystal - Google Patents
A kind of method for preparing high-purity sulfuric acid oxygen titanium crystal Download PDFInfo
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- CN108190946A CN108190946A CN201810191650.7A CN201810191650A CN108190946A CN 108190946 A CN108190946 A CN 108190946A CN 201810191650 A CN201810191650 A CN 201810191650A CN 108190946 A CN108190946 A CN 108190946A
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- sulfuric acid
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- titanyl sulfate
- acidolysis
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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
- C01G23/008—Titanium- and titanyl sulfate
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/10—Particle morphology extending in one dimension, e.g. needle-like
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- 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
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Abstract
The present invention relates to a kind of methods for preparing high-purity sulfuric acid oxygen titanium crystal, include the following steps：1）Ilmenite concentrate is subjected to acidolysis and sedimentation by the acidolysis flow of method for producing gtitanium dioxide with sulphuric acid, after isolating unreacted acidolysis slag, obtains acid hydrolysis solution；2）By step 1）Obtained acid hydrolysis solution is maintained at 100 180oC adds in sulfuric acid and titanyl sulfate crystal seed and is crystallized, isolated acicular crystal while hot after crystallization completely；3）By step 2）Obtained acicular crystal obtains titanyl sulfate crystal after being washed with dilute sulfuric acid.The present invention causes titanyl sulfate crystal structure to be precipitated, then by fully washing, so as to obtain the titanyl sulfate crystal of high-purity by the use of the acid hydrolysis solution of ilmenite concentrate as raw material using the mode of high temperature crystallization.
Description
Technical field
The present invention relates to a kind of methods for preparing high-purity sulfuric acid oxygen titanium crystal, belong to titanyl sulfate preparing technical field.
Background technology
Titanyl sulfate can be widely applied to fabric mordant, reducing agent dyestuff decolourant and be replaced in electroplating industry
Chromic acid carries out chromium-free deactivation processing, while is also used as photochemical catalyst.The preparation of Nano titanium dioxide, also largely
Dependence titanyl sulfate is titanium source, and titanyl sulfate solution can be used to prepare superfine titanic oxide, high-purity sulfuric acid under certain condition
Oxygen titanium can effectively mitigate the reunion of Nano titanium dioxide particle, improve dispersibility, improve its catalytic effect.
The preparation of titanyl sulfate is main at present or is made by sulfuric acid dissolution metatitanic acid, such as the phase in October, 2011《Jiangsu
Ceramics》One it is entitled《Solid TiOSO4Study on the synthesis》As soon as in text, the sulfuric acid concentration that is related generally in preparation process,
It is carried out in terms of the influence of the technological parameters such as reaction temperature and above-mentioned technological parameter to metatitanic acid and sulfuric acid synthesis titanyl sulfate
Detailed research and discussion, it is believed that the best synthetic technological condition of metatitanic acid and sulfuric acid is：Sulfuric acid concentration is not less than 95%, reaction
The temperature of system is controlled in 200 ~ 250 °C of temperature ranges, and the mass ratio of titanyl sulfate and sulfuric acid has reached 1:4.
High-concentration sulfuric acid and reaction high temperature to the selection of Preparation equipment material, protective equipment and state modulator etc. all
There is very high technical requirement, and there is high energy consumption, high；Furthermore high acidolysis temperature pair
Titanyl sulfate solution has a significant impact, and easily grows by-product, make thereafter titanyl sulfate crystalline quality obtained in color and luster and pure
Occur comparable difference in terms of degree, the solubility of titanyl sulfate product in water is caused to reduce, and then influence answering for titanyl sulfate
Use effect.
Invention content
The present invention provides a kind of methods for preparing high-purity sulfuric acid oxygen titanium crystal, specifically include following steps：
A kind of method for preparing high-purity sulfuric acid oxygen titanium crystal, includes the following steps：
1）Ilmenite concentrate is subjected to acidolysis and sedimentation by the acidolysis flow of method for producing gtitanium dioxide with sulphuric acid, isolates unreacted acidolysis slag
Afterwards, acid hydrolysis solution is obtained；
2）By step 1）Obtained acid hydrolysis solution is maintained at 100-180oC, adds in sulfuric acid and titanyl sulfate crystal seed is crystallized, and crystallizes
Isolated acicular crystal while hot after completely；
3）By step 2）Obtained acicular crystal obtains titanyl sulfate crystal after being washed with dilute sulfuric acid.
Further, step 3）A concentration of 5-20% of middle dilute sulfuric acid.
Further, step 2）The additive amount of middle sulfuric acid is calculated as 4- with the mass ratio of titanium dioxide in sulfate radical and solution
10:1。
Further, step 2）The additive amount of middle titanyl sulfate crystal seed is calculated as 1- with the mass ratio with titanium dioxide in solution
15wt%；
The present invention causes titanyl sulfate crystal structure to analyse by the use of the acid hydrolysis solution of ilmenite concentrate as raw material using the mode of high temperature crystallization
Go out, then by fully washing, so as to obtain the titanyl sulfate crystal of high-purity.
At present in the acidolysis flow of method for producing gtitanium dioxide with sulphuric acid, generally using solid phase acidolysis, after ilmenite concentrate is milled with
Sulfuric acid premixes, and the sulfuric acid for adding 92 ~ 95% carries out acidolysis, and acidolysis temperature is controlled at 180 ~ 200 DEG C, obtains yellow solid formation, Gu
Phase object adds acid water and is leached to obtain leaching liquid after overcuring and cooling.This method is efficient with acidolysis, energy consumption
Low, the advantages of cost of equipment maintenance is low.Titanyl sulfate crystal is prepared using this method, it can be in the condition of relative low temperature and Low acid
Under reacted, solve traditional handicraft leaching liquid made from titanyl sulfate crystalline quality occur in terms of color and luster and purity quite
Difference the problem of.
And this method is that high-purity sulfuric acid oxygen titanium crystal is directly prepared from raw material ilmenite concentrate, can reduce sulfuric acid oxygen
The production cost of titanium.
Specific embodiment
With reference to embodiment, the present invention is further described.
Embodiment 1：
Ilmenite concentrate carries out acidolysis and sedimentation by normal acidolysis flow, and after detaching unreacted acidolysis slag, titanium liquid temperature is maintained at
100oC adds in sulfuric acid 10：1 (mass ratio of sulfate radical and titanium dioxide), while titanyl sulfate crystal seed is also added in, crystal seed adds
Dosage be 15wt% (mass ratio with titanium dioxide in solution), accelerate crystallization, it is to be crystallized completely after, be separated by filtration while hot needle-shaped
Titanyl sulfate crystal, and fully washed with a concentration of 20% dilute sulfuric acid, the yield of final titanyl sulfate is 85%.
Embodiment 2：
Ilmenite concentrate carries out acidolysis and sedimentation by normal acidolysis flow, and after detaching unreacted acidolysis slag, titanium liquid temperature is maintained at
150oC adds in sulfuric acid 6：1 (mass ratio of sulfate radical and titanium dioxide), while titanyl sulfate crystal seed is also added in, crystal seed addition
Measure as 10wt% (mass ratio with titanium dioxide in solution), accelerate crystallization, it is to be crystallized completely after, be separated by filtration while hot acicular
Titanyl sulfate crystal, and fully washed with a concentration of 10% dilute sulfuric acid, the yield of final titanyl sulfate is 90%.
Embodiment 3
Ilmenite concentrate carries out acidolysis and sedimentation by normal acidolysis flow, and after detaching unreacted acidolysis slag, titanium liquid temperature is maintained at
180oC adds in sulfuric acid 4：1 (mass ratio of sulfate radical and titanium dioxide), while titanyl sulfate crystal seed is also added in, crystal seed addition
Measure as 1wt% (mass ratio with titanium dioxide in solution), accelerate crystallization, it is to be crystallized completely after, be separated by filtration acicular sulphur while hot
Sour oxygen titanium crystal, and fully washed with a concentration of 5% dilute sulfuric acid, the yield of final titanyl sulfate is 85%.
Claims (4)
- A kind of 1. method for preparing high-purity sulfuric acid oxygen titanium crystal, which is characterized in that include the following steps：1）Ilmenite concentrate is subjected to acidolysis and sedimentation by the acidolysis flow of method for producing gtitanium dioxide with sulphuric acid, isolates unreacted acidolysis slag Afterwards, acid hydrolysis solution is obtained；2）By step 1）Obtained acid hydrolysis solution is maintained at 100-180oC, adds in sulfuric acid and titanyl sulfate crystal seed is crystallized, and crystallizes Isolated acicular crystal while hot after completely；3）By step 2）Obtained acicular crystal obtains titanyl sulfate crystal after being washed with dilute sulfuric acid.
- 2. the method according to claim 1 for preparing high-purity sulfuric acid oxygen titanium crystal, it is characterised in that：Step 3）In dilute sulphur A concentration of 5-20% of acid.
- 3. the method according to claim 1 for preparing high-purity sulfuric acid oxygen titanium crystal, it is characterised in that：Step 2）Middle sulfuric acid Additive amount 4-10 is calculated as with the mass ratio of titanium dioxide in sulfate radical and solution:1.
- 4. the method according to claim 1 for preparing high-purity sulfuric acid oxygen titanium crystal, it is characterised in that：Step 2）Middle sulfuric acid The additive amount of oxygen titanium crystal seed is calculated as 1-15wt% with the mass ratio with titanium dioxide in solution.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113998731A (en) * | 2021-11-26 | 2022-02-01 | 中南大学 | Production method of titanyl sulfate and nano titanium dioxide |
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|---|---|---|---|---|
| CN102515266A (en) * | 2011-12-29 | 2012-06-27 | 攀枝花东方钛业有限公司 | Method for preparing titanium oxysulfate solution by flotation of titanium concentrate |
| CN102531047A (en) * | 2011-12-29 | 2012-07-04 | 攀枝花东方钛业有限公司 | Method for preparing titanyl sulfate solution with flotation ilmenite |
| CN102602990A (en) * | 2012-03-31 | 2012-07-25 | 四川龙蟒钛业股份有限公司 | Recycling method for producing acidolysis slag in titanium dioxide with sulfuric acid method |
| CN104692455A (en) * | 2015-03-10 | 2015-06-10 | 丹东市化学试剂厂 | Preparation method of titanyl sulfate |
| CN105585045A (en) * | 2014-10-21 | 2016-05-18 | 沈炳炜 | Method for preparing titanyl sulfate |
| CN106673056A (en) * | 2015-11-06 | 2017-05-17 | 南通德益化工有限公司 | Method for preparing titanyl sulfate |
| CN106957067A (en) * | 2017-04-24 | 2017-07-18 | 四川龙蟒钛业股份有限公司 | Reduce the sulfuric acid method titanium pigment acid hydrolysis method of reduced iron powder consumption |
| CN107381629A (en) * | 2017-09-11 | 2017-11-24 | 南通意特化工有限公司 | A kind of preparation method of titanyl sulfate |
-
2018
- 2018-03-08 CN CN201810191650.7A patent/CN108190946A/en active Pending
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102515266A (en) * | 2011-12-29 | 2012-06-27 | 攀枝花东方钛业有限公司 | Method for preparing titanium oxysulfate solution by flotation of titanium concentrate |
| CN102531047A (en) * | 2011-12-29 | 2012-07-04 | 攀枝花东方钛业有限公司 | Method for preparing titanyl sulfate solution with flotation ilmenite |
| CN102602990A (en) * | 2012-03-31 | 2012-07-25 | 四川龙蟒钛业股份有限公司 | Recycling method for producing acidolysis slag in titanium dioxide with sulfuric acid method |
| CN105585045A (en) * | 2014-10-21 | 2016-05-18 | 沈炳炜 | Method for preparing titanyl sulfate |
| CN104692455A (en) * | 2015-03-10 | 2015-06-10 | 丹东市化学试剂厂 | Preparation method of titanyl sulfate |
| CN106673056A (en) * | 2015-11-06 | 2017-05-17 | 南通德益化工有限公司 | Method for preparing titanyl sulfate |
| CN106957067A (en) * | 2017-04-24 | 2017-07-18 | 四川龙蟒钛业股份有限公司 | Reduce the sulfuric acid method titanium pigment acid hydrolysis method of reduced iron powder consumption |
| CN107381629A (en) * | 2017-09-11 | 2017-11-24 | 南通意特化工有限公司 | A kind of preparation method of titanyl sulfate |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113998731A (en) * | 2021-11-26 | 2022-02-01 | 中南大学 | Production method of titanyl sulfate and nano titanium dioxide |
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