CN106673056A - Method for preparing titanyl sulfate - Google Patents
Method for preparing titanyl sulfate Download PDFInfo
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- CN106673056A CN106673056A CN201510744751.9A CN201510744751A CN106673056A CN 106673056 A CN106673056 A CN 106673056A CN 201510744751 A CN201510744751 A CN 201510744751A CN 106673056 A CN106673056 A CN 106673056A
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- titanyl sulfate
- sulfuric acid
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Abstract
The invention discloses a method for preparing titanyl sulfate. The method comprises the following steps: sequentially adding a metatitanic acid solid and sulfuric acid to a reaction kettle, stirring the metatitanic acid solid and sulfuric acid to form a slurry without obvious hard blocks according to a mass ratio of metatitanic acid to dehydrated sulfuric acid of 1:5; adding an acidifying assistant accounting for 11% of the mass of the metatitanic acid to the slurry, wherein the acidifying assistant is a sulfuric acid, oxidant and water mixture; decreasing the temperature of the obtained solution to 100 DEG C, adding titanyl sulfate crystal seeds accounting for 0.23% of the mass of the metatitanic acid, and keeping the temperature to precipitate crystals, wherein the crystal seeds are pure titanyl sulfate crystals with uniform texture and with the granularity not exceeding 0.1 mm; and cooling the obtained crystallization solution to room temperature, carrying out vacuum suction filtration or centrifuge filtration, and separating out a mother liquor to obtain titanyl sulfate crystals. The method adopting a reasonable adjusting technology realizes the preparation of titanyl sulfate under low-temperature and low-concentration conditions, and titanyl sulfate prepared in the invention has greatly improved water solubility, and facilitates the preparation of titanyl sulfate downstream products.
Description
Technical field
The invention belongs to chemical technology field, and in particular to a kind of preparation method of titanyl sulfate.
Background technology
Titanyl sulfate is a kind of white or flavescent crystalline powder, molecular formula：TiOSO4, two crystallizations water are often contained in molecule, there is hygroscopy, cold water can be dissolved in.
The application of titanyl sulfate is quite varied.It can be also used as photochemical catalyst as the mordant of fabric, reducing agent and dyestuff decolourant.The preparation of Nano titanium dioxide, it is titanium source also to rely heavily on titanyl sulfate, and titanyl sulfate solution can be used under certain condition prepare superfine titanic oxide.For example, with urea as precipitating reagent, hydrolysis makes superfine titanic oxide be carried on fabric face, and fabric just possesses the functions such as obvious automatically cleaning, uvioresistant.Superfine titanic oxide is carried on activated carbon or molecular sieve, then have stronger catalysis.Adjust by titanium system table of titanyl sulfate, substantial amounts of titanium salt can be provided in metal surface and crystallize nucleus, and constitute one layer of uniform film, be good metal conditioner.Technical research in recent years shows that titanyl sulfate is also used as water treatment agent, is increasingly paid close attention to by people.Titanyl sulfate can effectively remove the Organic Pollution in water body as traditional flocculant, and its coagulation effect is better than traditional aluminium salt and Ferric Salt Flocculants, and flco particle diameter is thick, fast growth, and is easily isolated.Titanyl sulfate can be additionally used in chemical industry production high-purity inorganic titanium salt, such as generate boric acid titanium with acid reaction with titanyl sulfate solution, with titanyl sulfate solution and ammoniacal liquor synthesis titanium acid ammonium, etc..
The sulfate of titanium has titanium sulfate and titanyl sulfate, i.e. Ti (SO4)2And TiOSO2.Calculate by molecular formula, the Ti content of titanium sulfate is only 20%, and the Ti content of titanyl sulfate is up to 30%.So for the aqueous solution of titanium, titanyl sulfate can provide the titanium source of more sufficient quantity, and downstream product is provided a great convenience, and save the cost expenses for removing a large amount of sulfate radicals in solution.Nano titanium dioxide is prepared using titanyl sulfate, high-purity sulfuric acid oxygen titanium can effectively mitigate the reunion of Nano titanium dioxide particle, improve dispersiveness, improve its catalytic effect.
The content of the invention
Present invention aims to the deficiencies in the prior art, now provide a kind of preparation method of the titanyl sulfate under low concentration, cryogenic conditions.
For achieving the above object, the technical scheme is that：A kind of preparation method of titanyl sulfate, its innovative point is：Including following preparation process：
（1）The sulfuric acid that metatitanic acid solid and concentration are 40% is put into successively in reactor, is stirred to without obvious lump, being uniform slurries, wherein, the mass ratio that metatitanic acid is gone after water with the sulfuric acid is 1：5；
（2）The acidification adjuvant of metatitanic acid quality 6～16% is added in slurries one step up；Described acidification adjuvant is the mixture of sulfuric acid, oxidant and water, and oxidant therein is the aqueous hydrogen peroxide solution that concentration is 45%, and water is deionized water, and sulfuric acid, oxidant and water press 5:1:15 quality proportionings mix；
（3）Solution temperature is declined and is adjusted to 50～150 DEG C, then put into titanyl sulfate crystal seed, insulation separates out crystal；The addition of described crystal seed is the 0.2～0.25% of metatitanic acid quality, and the crystal seed is homogeneous, pure titanyl sulfate crystal, the not super 0.1mm of its crystal size size；
（4）Crystal solution is cooled to after room temperature, vacuum filtration or centrifugal filtration, isolates mother liquor, obtains titanyl sulfate crystal.
Beneficial effects of the present invention are as follows：The present invention realizes the preparation of titanyl sulfate under low temperature, low consistency conditions by Reasonable adjustment technique, and the titanyl sulfate water solubility for preparing is greatly improved, and is conducive to the preparation of the dirty product of titanyl sulfate.
Specific embodiment
Hereinafter embodiments of the present invention are illustrated by particular specific embodiment, the content that those skilled in the art can be by disclosed by this specification understands easily other advantages and effect of the present invention.
Embodiment 1
A kind of preparation method of titanyl sulfate, including following preparation process：
（1）The sulfuric acid that metatitanic acid solid and concentration are 40% is put into successively in reactor, is stirred to without obvious lump, being uniform slurries, wherein, the mass ratio that metatitanic acid is gone after water with sulfuric acid is 1：5；
（2）The acidification adjuvant of metatitanic acid quality 6% is added in slurries one step up；Acidification adjuvant is the mixture of sulfuric acid, oxidant and water, and oxidant therein is the aqueous hydrogen peroxide solution that concentration is 45%, and water is deionized water, and sulfuric acid, oxidant and water press 5:1:15 quality proportionings mix；
（3）Solution temperature is declined and is adjusted to 50 DEG C, then put into titanyl sulfate crystal seed, insulation separates out crystal；The addition of crystal seed is the 0.2% of metatitanic acid quality, and the crystal seed is homogeneous, pure titanyl sulfate crystal, the not super 0.1mm of its crystal size size；
（4）Crystal solution is cooled to after room temperature, vacuum filtration or centrifugal filtration, isolates mother liquor, obtains titanyl sulfate crystal.
Embodiment 2
A kind of preparation method of titanyl sulfate, including following preparation process：
（1）The sulfuric acid that metatitanic acid solid and concentration are 40% is put into successively in reactor, is stirred to without obvious lump, being uniform slurries, wherein, the mass ratio that metatitanic acid is gone after water with sulfuric acid is 1：5；
（2）The acidification adjuvant of metatitanic acid quality 16% is added in slurries one step up；Acidification adjuvant is the mixture of sulfuric acid, oxidant and water, and oxidant therein is the aqueous hydrogen peroxide solution that concentration is 45%, and water is deionized water, and sulfuric acid, oxidant and water press 5:1:15 quality proportionings mix；
（3）Solution temperature is declined and is adjusted to 150 DEG C, then put into titanyl sulfate crystal seed, insulation separates out crystal；The addition of crystal seed is the 0.25% of metatitanic acid quality, and the crystal seed is homogeneous, pure titanyl sulfate crystal, the not super 0.1mm of its crystal size size；
（4）Crystal solution is cooled to after room temperature, vacuum filtration or centrifugal filtration, isolates mother liquor, obtains titanyl sulfate crystal.
Embodiment 3
A kind of preparation method of titanyl sulfate, including following preparation process：
（1）The sulfuric acid that metatitanic acid solid and concentration are 40% is put into successively in reactor, is stirred to without obvious lump, being uniform slurries, wherein, the mass ratio that metatitanic acid is gone after water with sulfuric acid is 1：5；
（2）The acidification adjuvant of metatitanic acid quality 11% is added in slurries one step up；Acidification adjuvant is the mixture of sulfuric acid, oxidant and water, and oxidant therein is the aqueous hydrogen peroxide solution that concentration is 45%, and water is deionized water, and sulfuric acid, oxidant and water press 5:1:15 quality proportionings mix；
（3）Solution temperature is declined and is adjusted to 100 DEG C, then put into titanyl sulfate crystal seed, insulation separates out crystal；The addition of crystal seed is the 0.23% of metatitanic acid quality, and the crystal seed is homogeneous, pure titanyl sulfate crystal, the not super 0.1mm of its crystal size size；
（4）Crystal solution is cooled to after room temperature, vacuum filtration or centrifugal filtration, isolates mother liquor, obtains titanyl sulfate crystal.
The present invention realizes the preparation of titanyl sulfate under low temperature, low consistency conditions by Reasonable adjustment technique, and the titanyl sulfate water solubility for preparing is greatly improved, and is conducive to the preparation of the dirty product of titanyl sulfate.
Above-described embodiment is presently preferred embodiments of the present invention; it is not the restriction to technical solution of the present invention; as long as without the technical scheme that creative work can be realized on the basis of above-described embodiment, in the rights protection scope for being regarded as falling into patent of the present invention.
Claims (1)
1. a kind of preparation method of titanyl sulfate, it is characterised in that：Including following preparation process：
（1）The sulfuric acid that metatitanic acid solid and concentration are 40～70% is put into successively in reactor, is stirred to without obvious lump, being uniform slurries, wherein, the mass ratio that metatitanic acid is gone after water with the sulfuric acid is 1：5～7；
（2）The acidification adjuvant of metatitanic acid quality 6～16% is added in slurries one step up；Described acidification adjuvant is the mixture of sulfuric acid, oxidant and water, and oxidant therein is the aqueous hydrogen peroxide solution that concentration is 45%, and water is deionized water, and sulfuric acid, oxidant and water press 5:1:15 quality proportionings mix；
（3）Solution temperature is declined and is adjusted to 50～150 DEG C, then put into titanyl sulfate crystal seed, insulation separates out crystal；The addition of described crystal seed is the 0.2～0.25% of metatitanic acid quality, and the crystal seed is homogeneous, pure titanyl sulfate crystal, the not super 0.1mm of its crystal size size；
（4）Crystal solution is cooled to after room temperature, vacuum filtration or centrifugal filtration, isolates mother liquor, obtains titanyl sulfate crystal.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201510744751.9A CN106673056A (en) | 2015-11-06 | 2015-11-06 | Method for preparing titanyl sulfate |
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| CN201510744751.9A CN106673056A (en) | 2015-11-06 | 2015-11-06 | Method for preparing titanyl sulfate |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN108190946A (en) * | 2018-03-08 | 2018-06-22 | 四川龙蟒钛业股份有限公司 | A kind of method for preparing high-purity sulfuric acid oxygen titanium crystal |
-
2015
- 2015-11-06 CN CN201510744751.9A patent/CN106673056A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN108190946A (en) * | 2018-03-08 | 2018-06-22 | 四川龙蟒钛业股份有限公司 | A kind of method for preparing high-purity sulfuric acid oxygen titanium crystal |
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| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20170517 |
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| WD01 | Invention patent application deemed withdrawn after publication |