CN106365200A - High-purity ultra-fine titanium dioxide prepared from industrial metatitanic acid and preparation method of titanium dioxide - Google Patents
High-purity ultra-fine titanium dioxide prepared from industrial metatitanic acid and preparation method of titanium dioxide Download PDFInfo
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- CN106365200A CN106365200A CN201610829671.8A CN201610829671A CN106365200A CN 106365200 A CN106365200 A CN 106365200A CN 201610829671 A CN201610829671 A CN 201610829671A CN 106365200 A CN106365200 A CN 106365200A
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- metatitanic acid
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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
- C01G23/08—Drying; Calcining ; After treatment of titanium oxide
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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
- C01P2004/60—Particles characterised by their size
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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- C01P2006/80—Compositional purity
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Abstract
The invention relates to a preparation method of titanium dioxide, in particular to a method for preparing high-purity ultra-fine titanium dioxide by industrial metatitanic acid. The method includes the steps: a, beating dispersion: washing and bleaching hydrolyzed metatitanic acid, adding water for dilution, performing beating and ultrasonic dispersion to obtain slurry, adding dispersing agents into the slurry and performing dispersion to obtain metatitanic acid slurry; b, curing: curing the metatitanic acid slurry, cooling the metatitanic acid slurry to 60-70 DEG C, and filtering and washing the metatitanic acid slurry until ferrous ions are removed to obtain a purified metatitanic acid filter cake; c, calcining: adding water to the metatitanic acid filter cake, performing ultrasonic dispersion and calcining, cooling the filter cake to room temperature, and crushing and grinding the filter cake to obtain the titanium dioxide. By the aid of an impurity ion occurrence form in hydrolyzed metatitanic acid particles and composition and structural characteristics of the metatitanic acid, the high-purity ultra-fine titanium dioxide is directly prepared by dispersion, washing, curing, calcining and the like, new varieties of the titanium dioxide can be increased, product application can be functionalized, and the method has a wide application prospect.
Description
Technical field
The present invention relates to a kind of preparation method of titanium dioxide is and in particular to a kind of industrial metatitanic acid prepares high pure and ultra-fine two
The method of titanium oxide.
Background technology
Titanium dioxide has stable physics and chemical property, is generally produced with the crystal formation of anatase titanium dioxide or rutile-type
Come, because of its excellent optical property, chemical inertness and high index of refraction, first-selected usually as Chinese white, be widely used in coating,
The various fields such as plastics, papermaking, ink, rubber, fiber, pottery, food additive.Titanium dioxide has semiconductive simultaneously
Can, dielectric constant and resistivity higher, and mechanics and electric property excellent, highly purified titanium dioxide such as catalyst carry
Body, UV absorbent, special glass, electronic ceramics, critesistor, semicoductor capacitor, strontium titanates varistor, functionalization two
The aspect extensive application such as titanium oxide and titanium, in recent years demand increase year by year.
The method preparing high-purity superfine titanic oxide at present mainly includes Titanium alkoxides Hydrolyze method, titanium tetrachloride direct hydrolysis
Method, chloridising and sulfuric acid process.Titanium alkoxides Hydrolyze method " three wastes " less, good product quality, good process repeatability, but technological process length,
Production safety hidden danger is many, auxiliary material price is higher, is only suitable for preparing in laboratory.Titanium tetrachloride direct hydrolysis method technological process
Short, good product quality, but feed quality requirements are high, production cost is higher.Chlorination process flow process is short, high degree of automation, " three
Useless " less, good product quality, but have such problems as that technical difficulty is big, feed quality requirements are high, equipment material requirement harsh, industry
Change difficulty big.And sulfuric acid process is prepared high-purity titanium dioxide and is had that process is simple is ripe, raw material is easy to get, cost is relatively low, equipment is simple
The advantages of, but be easily introduced impurity and make product purity low.
And Publication No. " cn101880479a ", a kind of invention entitled " production powdery paints special rutile type titanium white
The method of powder ", discloses following steps: it is 300～400g/l's that the metatitanic acid of gained after rinsing is made titanium dioxide concentration
Serosity, adds calcining auxiliary agent；Gained metatitanic acid is calcined after filtering, grinds and obtain first product；Gained first product is made titanium dioxide
Titanium concentration is the titanium dioxide slurries of 650～850g/l, adds wetting agent to carry out disperseing, sand milling；By gained titanium dioxide slurries
It is warmed up to 40～90 DEG C, sequentially adds dispersant, zirconates or titanium salt, silicon salt, aluminium salt, adjust ph value and be maintained at 5～9, ripening, tune
Section ph value is to 7～8；Then filter, wash, be dried, vapour powder after processing through organic surface treatment, obtain final product.This patent is preparation
Pigment titanium white, makes the reduction of its purity because it needs to add other salts (calcining auxiliary agent), there is also high cost, complex process etc.
Shortcoming.
Content of the invention
The technical problem to be solved is to provide a kind of low cost, process is simple, using industrial metatitanic acid preparation
The method of high-purity superfine titanic oxide.
The method that industrial metatitanic acid of the present invention prepares high-purity superfine titanic oxide, comprises the following steps:
A, making beating dispersion: metatitanic acid washing, bleaching, dilute making beating ultrasonic disperse will be hydrolyzed, obtain serosity, to slurry
Add the dispersant of 2wt ‰～5wt ‰ to be disperseed in liquid, obtain metatitanic acid slurry；The concentration of described serosity is with titanium dioxide
Quality is calculated as 150～400g/l；
B, ripening: the metatitanic acid slurry that a step is obtained is heated to micro-boiling and carries out ripening, keeps slight boiling condition 2～5h, it
After be cooled to 60～70 DEG C, filter, washing, until no ferrous ion exist, obtain the metatitanic acid filter cake of purification；
C, calcining: the metatitanic acid filter cake that b step is obtained adds water, ultrasonic disperse, calcining, it is cooled to room temperature, pulverize, grind
Mill, obtains final product.
In the method that above-mentioned industrial metatitanic acid prepares high-purity superfine titanic oxide, wherein a step, the time of ultrasonic disperse is 5
～15min.
Further, as preferred technical scheme, above-mentioned industrial metatitanic acid prepares the side of high-purity superfine titanic oxide
The time of method, wherein ultrasonic disperse is 10min.
The method that above-mentioned industrial metatitanic acid prepares high-purity superfine titanic oxide, wherein said dispersant is Polyethylene Glycol, gathers
One or more of ammonium methacrylate, polycarboxylate.
Further, as preferred technical scheme, above-mentioned industrial metatitanic acid prepares the side of high-purity superfine titanic oxide
Method, wherein dispersant are Polyethylene Glycol.
Calcine in the method that above-mentioned industrial metatitanic acid prepares high-purity superfine titanic oxide, wherein step c and be: with 10～15
DEG C/temperature rises to 700～800 DEG C from room temperature, and is incubated 100～150min at 700～800 DEG C by the heating rate of min.
Further, as preferred technical scheme, above-mentioned industrial metatitanic acid prepares the side of high-purity superfine titanic oxide
Calcine in method, wherein step c and be: typically with heating rate at the uniform velocity from room temperature to calcining heat, preferably with 12.08
DEG C/temperature rises to 750 DEG C from room temperature (25 DEG C), and is incubated 120min at 750 DEG C by the heating rate of min.
The present invention also provides a kind of high-purity superfine titanic oxide of industrial metatitanic acid preparation.
Above-mentioned high-purity superfine titanic oxide, content >=99.50% of wherein said high-purity superfine titanic oxide, particle diameter is
160～190nm, particle dispersion is 0.1～0.2.
The invention has the benefit that the inventive method is carried out in existing tradition sulfate process titanium dioxide production technology
Improve, using the Nomenclature Composition and Structure of Complexes characteristic of foreign ion occurrence form and metatitanic acid itself in hydrolysis metatitanic acid particle, by dividing
Dissipate, washing, ripening and calcining and other processes, direct preparation of high-purity superfine titanic oxide, titanium dioxide new varieties and realization can be increased
The functionalization of products application, has broad application prospects.
Specific embodiment
The method that industrial metatitanic acid of the present invention prepares high-purity superfine titanic oxide, comprises the following steps:
A, making beating dispersion: metatitanic acid washing, bleaching will be hydrolyzed, plus deionized water dilution making beating ultrasonic disperse, starched
Liquid, adds the dispersant of 2wt ‰～5wt ‰ to carry out in serosity fully dispersed uniform, obtains metatitanic acid slurry；Described serosity
Concentration is calculated as 150～400g/l with titanium dioxide quality；Above-mentioned hydrolysis metatitanic acid can be using in traditional sulfate process titanium dioxide technique
The hydrolysis metatitanic acid of hydrolysis gained；
B, ripening: the metatitanic acid slurry that a step is obtained is heated to micro-boiling and carries out ripening, keeps slight boiling condition 2～5h, it
After be cooled to 60～70 DEG C, filter, be washed with deionized, with ammonium thiocyanate detection, until no ferrous ion exist, obtain pure
The metatitanic acid filter cake changed；
C, calcining: the metatitanic acid filter cake that b step is obtained adds deionized water, ultrasonic disperse, can select to be forged with Muffle furnace
Burn, calcining is cooled to room temperature, attrition grinding after terminating, and obtains final product.
Hydrolysis metatitanic acid after scrubbed, bleaching eliminates a large amount of impurity substantially, adds dispersant fully dispersed and ripening
Afterwards, reduce colloidal nature and the specific surface area of metatitanic acid, further reduce the absorption of impurity, also reduce metatitanic acid simultaneously
The grain size of particle；By controlling follow-up dispersion and calcination condition, the control of achievable superfine titanic oxide particle growth and
The concordance of particle growth, prepares high-purity superfine titanic oxide.
In the method that above-mentioned industrial metatitanic acid prepares high-purity superfine titanic oxide, wherein a step, the time of ultrasonic disperse is 5
～15min.
Further, as the technical scheme more having choosing, above-mentioned industrial metatitanic acid prepares the side of high-purity superfine titanic oxide
The time of method, wherein ultrasonic disperse is 10min.
The method that above-mentioned industrial metatitanic acid prepares high-purity superfine titanic oxide, wherein said dispersant is Polyethylene Glycol, gathers
One or more of ammonium methacrylate, polycarboxylate.
Further, as preferred technical scheme, above-mentioned industrial metatitanic acid prepares the side of high-purity superfine titanic oxide
Method, wherein dispersant are Polyethylene Glycol.
Calcine in the method that above-mentioned industrial metatitanic acid prepares high-purity superfine titanic oxide, wherein step c and be: with 10～15
DEG C/temperature rises to 700～800 DEG C from room temperature, and is incubated 100～150min at 700～800 DEG C by the heating rate of min.
Further, as preferred technical scheme, above-mentioned industrial metatitanic acid prepares the side of high-purity superfine titanic oxide
Calcine in method, wherein step c and be: typically with heating rate at the uniform velocity from room temperature to calcining heat, preferably with 12.08
DEG C/temperature rises to 750 DEG C from room temperature (25 DEG C), and is incubated 120min at 750 DEG C by the heating rate of min.
It is contemplated that using the Hydrolysis Industry metatitanic acid in existing tradition sulfate process titanium dioxide production technology as raw material, utilizing
The Nomenclature Composition and Structure of Complexes characteristic of foreign ion occurrence form and metatitanic acid itself in metatitanic acid, by modes such as dispersion, washing, ripenings
Remove the impurity in metatitanic acid, and control the Calcine Strength of the metatitanic acid titanium dioxide to prepare high pure and ultra-fine, and then increase and produce
Product kind improving product added value.
The present invention also provides a kind of high-purity superfine titanic oxide of industrial metatitanic acid preparation.
Above-mentioned high-purity superfine titanic oxide, content >=99.50% of wherein said high-purity superfine titanic oxide, particle diameter is
160～190nm, particle dispersion is 0.1～0.2.
With reference to embodiment, the specific embodiment of the present invention is further described, therefore the present invention is not limited
System is among described scope of embodiments.
Embodiment 1
Hydrolyze prepared metatitanic acid as raw material with traditional sulfate process titanium dioxide production technology, after scrubbed, bleaching, plus
Enter deionized water dilution making beating, metatitanic acid slurry concentration 210g/l is (with tio for regulation and control2Quality meter), and use 500w ultrasonic grinding
Machine dispersed paste 10 minutes, adds dispersant Polyethylene Glycol 2.5 ‰, fully dispersed good metatitanic acid slurry afterwards.Will be scattered
Metatitanic acid slurry proceeds in the reactor with agitating heating and condensing reflux, is progressively warming up to boiling, keeps slight boiling condition 3 little
When, stopped reaction is simultaneously progressively cooled to 60～70 DEG C, is washed with deionized while hot, and detects the presence of iron ion with ammonium thiocyanate
Existing, washing to can not detecting iron ion, filter cake is the metatitanic acid of purification.Afterwards the metatitanic acid filter cake of purification is added deionization
Moisture dissipate and ultrasonic disperse uniformly, put and be placed in calcining in Muffle furnace to crucible, from the uniform velocity intensification 60min to 750 DEG C of room temperature,
It is incubated 120min at 750 DEG C, terminate calcining.It is cooled to room temperature after taking out calcined product, on three-head grinding machine, grind 60min,
Obtain final product high-purity superfine titanic oxide.The content of gained high purity product titanium dioxide is 99.78%, the particle diameter distribution of titanium dioxide
For: mean diameter 162nm, the dispersion 0.115 of granule, narrow diameter distribution.
Embodiment 2
Hydrolyze prepared metatitanic acid as raw material with traditional sulfate process titanium dioxide production technology, after scrubbed, bleaching, plus
Enter deionized water dilution making beating, metatitanic acid slurry concentration 340g/l is (with tio for regulation and control2Quality meter), and use 500w ultrasonic grinding
Machine dispersed paste 10 minutes, adds dispersant Polyethylene Glycol 3.3 ‰, fully dispersed good metatitanic acid slurry afterwards.Will be scattered
Metatitanic acid slurry proceeds in the reactor with agitating heating and condensing reflux, is progressively warming up to boiling, keeps slight boiling condition 3.5 little
When, stopped reaction is simultaneously progressively cooled to 70 DEG C, is washed with deionized while hot, and detects the presence of iron ion with ammonium thiocyanate and deposits
Washing to can not detecting iron ion, filter cake is the metatitanic acid of purification.Afterwards the metatitanic acid filter cake of purification is added deionized water
Dispersion ultrasonic disperse is uniformly, puts and is placed in calcining in Muffle furnace to crucible, from the uniform velocity intensification 60min to 750 DEG C of room temperature,
It is incubated 120min at 750 DEG C, terminate calcining.It is cooled to room temperature after taking out calcined product, on three-head grinding machine, grind 60min,
Obtain final product high-purity superfine titanic oxide.The content of gained high purity product titanium dioxide is 99.64%, the particle diameter distribution of titanium dioxide
For: mean diameter 181nm, the dispersion 0.193 of granule, narrow diameter distribution.
Embodiment 3
Hydrolyze prepared metatitanic acid as raw material with traditional sulfate process titanium dioxide production technology, after scrubbed, bleaching, plus
Enter deionized water dilution making beating, metatitanic acid slurry concentration 260g/l is (with tio for regulation and control2Quality meter), and use 500w ultrasonic grinding
Machine dispersed paste 10 minutes, adds dispersant Polyethylene Glycol 3.8 ‰, fully dispersed good metatitanic acid slurry afterwards.Will be scattered
Metatitanic acid slurry proceeds in the reactor with agitating heating and condensing reflux, is progressively warming up to boiling, keeps slight boiling condition 4 little
When, stopped reaction is simultaneously progressively cooled to 67 DEG C, is washed with deionized while hot, and detects the presence of iron ion with ammonium thiocyanate and deposits
Washing to can not detecting iron ion, filter cake is the metatitanic acid of purification.Afterwards the metatitanic acid filter cake of purification is added deionized water
Dispersion ultrasonic disperse is uniformly, puts and is placed in calcining in Muffle furnace to crucible, from the uniform velocity intensification 60min to 750 DEG C of room temperature,
It is incubated 120min at 750 DEG C, terminate calcining.It is cooled to room temperature after taking out calcined product, on three-head grinding machine, grind 60min,
Obtain final product high-purity superfine titanic oxide.The content of gained high purity product titanium dioxide is 99.59%, the particle diameter distribution of titanium dioxide
For: mean diameter 174nm, the dispersion 0.157 of granule, narrow diameter distribution.
Claims (9)
1. industrial metatitanic acid prepares the method for high-purity superfine titanic oxide it is characterised in that comprising the following steps:
A, making beating dispersion: metatitanic acid washing, bleaching, dilute making beating ultrasonic disperse will be hydrolyzed, obtain serosity, in serosity
The dispersant adding 2wt ‰～5wt ‰ is disperseed, and obtains metatitanic acid slurry；The concentration of described serosity is with titanium dioxide quality
It is calculated as 150～400g/l；
B, ripening: the metatitanic acid slurry that a step is obtained is heated to micro-boiling and carries out ripening, keep slight boiling condition 2～5h, cold afterwards
But to 60～70 DEG C, filter, washing, until no ferrous ion exists, obtain the metatitanic acid filter cake of purification；
C, calcining: the metatitanic acid filter cake that b step is obtained adds water, ultrasonic disperse, calcining, it is cooled to room temperature, pulverize, grind, that is,
?.
2. according to claim 1 industrial metatitanic acid prepare high-purity superfine titanic oxide method it is characterised in that: a step
The time of middle ultrasonic disperse is 5～15min.
3. according to claim 2 industrial metatitanic acid prepare high-purity superfine titanic oxide method it is characterised in that: ultrasonic point
The scattered time is 10min.
4. according to claim 1 industrial metatitanic acid prepare high-purity superfine titanic oxide method it is characterised in that: dispersant
For at least one in Polyethylene Glycol, ammonium polymethacrylate, polycarboxylate.
5. according to claim 4 industrial metatitanic acid prepare high-purity superfine titanic oxide method it is characterised in that: dispersant
For Polyethylene Glycol.
6. according to claim 1 industrial metatitanic acid prepare high-purity superfine titanic oxide method it is characterised in that: step c
Middle calcining is: with the heating rate of 10～15 DEG C/min, temperature is risen to 700～800 DEG C from room temperature, and at 700～800 DEG C
Insulation 100～150min.
7. according to claim 6 industrial metatitanic acid prepare high-purity superfine titanic oxide method it is characterised in that: step c
Middle calcining is: with the heating rate of 12.08 DEG C/min, from room temperature, temperature is risen to 750 DEG C, and is incubated 120min at 750 DEG C.
8. the high-purity superfine titanic oxide of any one of claim 1～7 methods described preparation.
9. according to claim 8 high-purity superfine titanic oxide it is characterised in that: the content of described high-purity superfine titanic oxide
>=99.50%, particle diameter is 160～190nm, and particle dispersion is 0.1～0.2.
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Cited By (4)
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| CN111013567A (en) * | 2019-12-13 | 2020-04-17 | 绍兴文理学院 | Preparation process and application of composite titanium liquid for catalytic purification of waste gas |
| CN114014355A (en) * | 2021-09-16 | 2022-02-08 | 攀枝花学院 | Method for purifying and deironing industrial metatitanic acid |
| CN109850941B (en) * | 2019-04-16 | 2022-04-15 | 攀枝花学院 | Method for preparing high-purity titanium dioxide by hydrolyzing industrial titanium sulfate solution |
| CN114671460A (en) * | 2022-04-27 | 2022-06-28 | 攀枝花学院 | Method for removing impurities from industrial metatitanic acid in sulfuric acid method titanium dioxide short-flow process |
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Effective date of registration: 20201126 Address after: Room 202, building 5, Bailian innovation and Technology Industrial Park, 16 Xiaguang Avenue, Xingtang sub district office, Linquan County, Fuyang City, Anhui Province Patentee after: Fuyang Keyou Testing Technology Co.,Ltd. Address before: 617000 Airport Road, Panzhihua, Sichuan, No. 10 Patentee before: PANZHIHUA University |
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