CN105948116A - Preparation method for titanium dioxide with high specific surface area - Google Patents
Preparation method for titanium dioxide with high specific surface area Download PDFInfo
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- CN105948116A CN105948116A CN201610504398.1A CN201610504398A CN105948116A CN 105948116 A CN105948116 A CN 105948116A CN 201610504398 A CN201610504398 A CN 201610504398A CN 105948116 A CN105948116 A CN 105948116A
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- preparation
- surface area
- specific surface
- titanium dioxide
- filter cake
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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
- C01G23/053—Producing by wet processes, e.g. hydrolysing titanium salts
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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
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
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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
- C01P2006/12—Surface area
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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
Abstract
The invention relates to a preparation method for titanium dioxide with a high specific surface area. The preparation method comprises the following steps: neutralizing an intermediate product, namely, metatitanic acid, which is obtained by performing acidolysis and hydrolysis on titanic iron ore to the pH of 8 to 10 by using ammonium hydroxide; raising the temperature to 90 DEG C after the neutralizing is completed; keeping the temperature for a certain time; cooling, and performing secondary washing; pulping washed filtering cakes; press-drying the pulp by using a press filter; conveying a dried material to a flash dryer for drying; crushing the dried material by using a micron crushing machine to finally obtain the titanium dioxide with the specific surface area up to 350 to 400 m<2>/g.
Description
Technical field
The invention belongs to field of titanium dioxide production, be specifically related to the preparation method of a kind of high-specific surface area titanium dioxide.
Background technology
Titanium dioxide i.e. titanium dioxide, is a kind of important Inorganic Chemicals.Because it is nontoxic, physicochemical properties are stable, have
The pigment performance of excellent optics, electrology characteristic and brilliance, is widely used in coating, ink, plastics, rubber, papermaking, change
In the fields such as fibre, art painting, daily cosmetics, enamel, pottery, electronics.
The industrial process of titanium dioxide mainly has chloridising and sulfuric acid process two kinds at present.The wherein production process of sulfuric acid method titanium pigment
Though extremely complex, its most basic chemical reaction can following several formulas simply represent:
Acidolysis: FeTiO3(FeO·TiO2)+2H2SO4→TiOSO4+FeSO4+2H2O
Hydrolysis: TiOSO4+2H2O→H2TiO3↓+H2SO4
Calcining: TiO2·xH2O·ySO3→TiO2+xH2O↑+ySO3↑
I.e. by ilmenite through sulfuric acid solution, hydrolyze, calcine three big master operations and prepare.Wherein the product of titanium hydrolysis actually is
Arrange aqueous and adsorbed a certain amount of SO3Colloidal tio 2 condensation product, its molecular formula can write TiO2·xH2O·ySO3, claim
For hydrated titanium dioxide, i.e. metatitanic acid (H2TiO3)。
Owing to titanium dioxide has the features such as light absorption is good, surface activity is big, thermal conductance good, magnetic is strong, it is also extensively used for
Photocatalysis field.Titanium dioxide also acts as the carrier of catalyst, it is possible to the active component of dispersed catalyst effectively, improves catalysis
The catalytic performance of agent.The photo-catalysis capability of titanium dioxide depends primarily on its surface area, has smaller particle size and high specific surface area
Titanium dioxide has higher photo-catalysis capability.And titanium dioxide specific surface area prepared by conventional sulfuric acid method is many 60～100m2/ g, and deposit
The defect such as high at production cost, catalytic effect is poor, service life is short.
The patent documentation of publication number CN1348430A discloses a kind of method preparing titania powder: make raw material with metatitanic acid,
First use in alkaline solution and metatitanic acid is to pH 7～9, be subsequently added a kind of metal-oxide, then with hot-air, this metatitanic acid sprayed
Mist is dried, and obtains spherical granule, sinters this granule and i.e. obtains titania powder.Described alkaline solution is NH4OH and NaOH
The mixture of aqueous solution.It is active with the catalysis improving titanium dioxide that this invention adds extra metal-oxide in preparation process,
And the titanium dioxide specific surface area obtained is only 90～110m2/g。
The titanium dioxide being obtained high-specific surface area by the specific surface area improving raw material metatitanic acid is also a kind of feasible technical scheme.
But, the titanium dioxide specific surface area obtained through conventional neutralization, calcining often reduces than the specific surface area of raw material metatitanic acid
100～150m2/g。
Summary of the invention
For above-mentioned technical problem of the prior art, the present invention provides a kind of product specific surface area can be with starting material specific surface
The preparation method of the long-pending the most higher high-specific surface area titanium dioxide that maintains an equal level.This preparation method needs not move through calcining further, prepares work
Skill is simpler.
The present invention is achieved through the following technical solutions:
The preparation method of a kind of high-specific surface area titanium dioxide, comprises the following steps:
1. by ilmenite through acidolysis, hydrolysis after product metatitanic acid scrubbed after, be the ammonia of 20 ± 2% with mass percent concentration
Water neutralizes, and reaches pH value 8～10, preferable ph 9～10 after neutralization, and N-process keeps 1 hour, and limit is stirred, and limit neutralizes.
After neutralization completes, material is warming up to 90 DEG C, heating rate 1 DEG C/min, is incubated 1 hour.It is subsequently cooled to 75 DEG C, carries out again
Washing, wash time keeps 1 hour, and washing terminal ensures that filter cake sulfur content is less than 0.3%.
2. by washing qualified after filter cake, with 300,000 Ω cm deionized waters making beating, control concentration of slurry 300 ± 20g/L, so
Pressing dry by pressure filter, controlling cake moisture is 45～55%.
3. after taking off cake, filter cake is delivered to expansion drying main frame, in expansion drying main frame, inputs hot-air simultaneously, keep filter cake
90～105 DEG C are reached with temperature after hot air.High speed agitator is set bottom expansion drying machine host, filter cake is beaten rapidly
Dissipate, under hot-air stream and air-introduced machine act on jointly, material in 3～5 seconds by rising very rapidly up to exsiccator top bottom exsiccator
During be oven-dried.Top arranges cyclone classifier, and defective material is returned expansion drying motor spindle and again dries；Qualified
Material drying by air-introduced machine suction pulse dust collector and be attached to filter bag of dust collector surface, by electromagnetism Rapping apparatus and compression
The impact of air stream, makes material fall into bottom pulse dust collector, collects storage bin by auger conveyor and star discharge valve,
High-specific surface area titanium dioxide product is i.e. obtained after micron disintegrator is pulverized.
After metatitanic acid used in above-mentioned preparation method is scrubbed, its specific surface area preferably reaches 350m2/ more than g, regulation before neutralizing
Its concentration is to 200 ± 20g/L；
Using ammonia to neutralize is the sulfate ion in order to remove in meta-titanium acid solution, and ammonia is while playing neutralization,
The volume of metatitanic acid material can also be increased, be allowed to more bulk, more dispersed, add the contact area with ammonia, play surface and live
The effect of property agent；
N-process keeps 1 hour, and is under stirring condition, metatitanic acid can be made to be fully contacted with ammonia, mix homogeneously；
After neutralization, material being warming up to 90 DEG C, and be incubated 1 hour, when neutralization reaction can be made to carry out, the material viscosity of thickening reduces,
Make ammonia molecular motion accelerate, promote that neutralizing reaction is carried out, make neutralization reaction more uniform, and make the final titanium white powder prepared
Footpath is more uniform, activity is more stable；
Using flash dryer, it is 90～105 DEG C that baking temperature is maintained at the temperature of hot-air and filter cake mixture, after drying
Without calcining further, i.e. can get high-specific surface area titanium dioxide.This process modification reduces integral production cost, shortens
Production time, it is suitable for industrialization large-scale production.
Technique effect:
The most above-mentioned preparation method by the concentration of metatitanic acid, neutralize the time, neutralize pH value, neutralize after the control of temperature, with
And the technique of employing expansion drying, the specific surface area of final products titanium dioxide and the specific surface area phase of starting material metatitanic acid can be made
Maintain an equal level, the highest.The specific surface area of starting material metatitanic acid of the present invention is at 350m2/ more than g, the titanium white prepared
Powder specific surface area can reach 350～370m2/ g, it might even be possible to reach 350～400m2/g.The titanium prepared compared to existing method
White lead specific surface area can reduce by 100～150m than starting material2This defect of/g, the present invention achieves significant technological progress and dashes forward
The beneficial effect gone out.
2. the titanium dioxide product index using said method to prepare is as follows:
Titanium dioxide purity 88 ± 0.7%；
Specific surface area 350～370m2/g；
Crystal particle diameter 14～16nm；
Fugitive constituent (105 DEG C, 2h)≤2%；
Calcination loss (600 DEG C of calcination 1h of sample after 105 DEG C of 2h drying)≤10%；
Water slurry pH value 6.5～7.5；
Water absorption (30～35) g/50g；
45 μm residue on sieve≤0.04%；
Fe2O3≤ 0.010%；
SO4 2-Content≤1.5%；
Aggregated particle size D50It is 0.8～1.2 μm；
Aggregated particle size D90≤10μm；
(K2O+Na2O)≤0.01%.
3. use such high-specific surface area prepared by said method, high-purity, low particle diameter, even-grained titanium dioxide to play
Excellent photo-catalysis capability, can replace imported product, and lower than import like product production cost, steady quality.
Detailed description of the invention
The present invention will be described in detail by the specific embodiment of following exemplary, but spirit and claims of the present invention book
Protection domain is not limited by these specific embodiments.
Embodiment 1
The preparation method of a kind of high-specific surface area titanium dioxide, comprises the following steps:
1. by scrubbed qualified for ilmenite product metatitanic acid after acidolysis, hydrolysis, and specific surface area reaches 350m2/ more than g,
Concentration is adjusted to 200g/L, neutralizes with ammonia that mass percent concentration is 20%, and to pH value 9.5, N-process keeps 1 little
Time, limit stirring, limit neutralizes.After neutralization completes, material is warming up to 90 DEG C, heating rate 1 DEG C/min, is incubated 1 hour.Then
Being cooled to 75 DEG C, again wash, wash time keeps 1 hour, and washing terminal ensures that filter cake sulfur content is less than 0.3%.
2. by washing qualified after filter cake, with 300,000 Ω cm deionized waters pull an oar, control concentration of slurry is 300g/L, then
Press dry through pressure filter, control cake moisture and reach 50%.
3. after taking off cake, filter cake is delivered to expansion drying main frame, in expansion drying main frame, inputs hot-air simultaneously, keep filter cake
95 DEG C are reached with temperature after hot air.High speed agitator is set bottom expansion drying machine host, filter cake is broken up rapidly,
Under hot-air stream and air-introduced machine act on jointly, material in 3～5 seconds by the mistake rising very rapidly up to exsiccator top bottom exsiccator
Journey is oven-dried.Top arranges cyclone classifier, and defective material is returned expansion drying motor spindle and again dries；Qualified baking
Dry material is by air-introduced machine suction pulse dust collector and be attached to filter bag of dust collector surface, by electromagnetism Rapping apparatus and compressed air
The impact of stream, makes material fall into bottom pulse dust collector, collects storage bin by auger conveyor and star discharge valve, passes through
Micron disintegrator i.e. obtains high-specific surface area titanium dioxide product after pulverizing.
Embodiment 2
The preparation method of a kind of high-specific surface area titanium dioxide, comprises the following steps:
1. by scrubbed qualified for ilmenite product metatitanic acid after acidolysis, hydrolysis, and specific surface area reaches 350m2/ more than g,
Concentration is adjusted to 180g/L, neutralizes with the ammonia that mass percent concentration is 20%, and to pH 9.8, N-process keeps 1 hour,
Limit is stirred, and limit neutralizes.After neutralization completes, material is warming up to 90 DEG C, heating rate 1 DEG C/min, is incubated 1 hour.Then cool down
To 75 DEG C, again washing, wash time keeps 1 hour, and washing terminal ensures that filter cake sulfur content is less than 0.3%.
2. by washing qualified after filter cake, with 300,000 Ω cm deionized waters pull an oar, control concentration of slurry is 310g/L, then
Pressing dry through pressure filter, controlling cake moisture is 55%.
3. after taking off cake, filter cake is delivered to expansion drying main frame, in expansion drying main frame, inputs hot-air simultaneously, keep filter cake
100 DEG C are reached with temperature after hot air.High speed agitator is set bottom expansion drying machine host, filter cake is broken up rapidly,
Under hot-air stream and air-introduced machine act on jointly, material in 3～5 seconds by rising very rapidly up to exsiccator top bottom exsiccator
During be oven-dried.Top arranges cyclone classifier, and defective material is returned expansion drying motor spindle and again dries；Qualified
Material drying is by air-introduced machine suction pulse dust collector and be attached to filter bag of dust collector surface, by electromagnetism Rapping apparatus and compression sky
The impact of air-flow, makes material fall into bottom pulse dust collector, collects storage bin, warp by auger conveyor and star discharge valve
Cross after micron disintegrator is pulverized and i.e. obtain high-specific surface area titanium dioxide product.
Embodiment 3
The preparation method of a kind of high-specific surface area titanium dioxide, comprises the following steps:
1. by scrubbed qualified for ilmenite product metatitanic acid after acidolysis, hydrolysis, and specific surface area reaches 350m2/ more than g,
Concentration is adjusted to 200g/L, neutralizes with the ammonia that mass percent concentration is 20%, and to pH 9.2, N-process keeps 1 hour,
Limit is stirred, and limit neutralizes.After neutralization completes, material is warming up to 90 DEG C, heating rate 1 DEG C/min, is incubated 1 hour.Then cool down
To 75 DEG C, again washing, wash time keeps 1 hour, and washing terminal ensures that filter cake sulfur content is less than 0.3%.
2. by washing qualified after filter cake, with 300,000 Ω cm deionized waters pull an oar, control concentration of slurry is 290g/L, then
Pressing dry through pressure filter, controlling cake moisture is 45%.
3. after taking off cake, filter cake is delivered to expansion drying main frame, in expansion drying main frame, inputs hot-air simultaneously, keep filter cake
98 DEG C are reached with temperature after hot air.High speed agitator is set bottom expansion drying machine host, filter cake is broken up rapidly,
Under hot-air stream and air-introduced machine act on jointly, material in 3～5 seconds by the mistake rising very rapidly up to exsiccator top bottom exsiccator
Journey is oven-dried.Top arranges cyclone classifier, and defective material is returned expansion drying motor spindle and again dries；Qualified baking
Dry material is by air-introduced machine suction pulse dust collector and be attached to filter bag of dust collector surface, by electromagnetism Rapping apparatus and compressed air
The impact of stream, makes material fall into bottom pulse dust collector, collects storage bin by auger conveyor and star discharge valve, passes through
Micron disintegrator i.e. obtains high-specific surface area titanium dioxide product after pulverizing.
Embodiment 4
The preparation method of a kind of high-specific surface area titanium dioxide, comprises the following steps:
1. by scrubbed qualified for ilmenite product metatitanic acid after acidolysis, hydrolysis, and specific surface area reaches 350m2/ more than g,
Concentration is adjusted to 200g/L, neutralizes with the ammonia that mass percent concentration is 20%, and to pH 8.5, N-process keeps 1 hour,
Limit is stirred, and limit neutralizes.After neutralization completes, material is warming up to 90 DEG C, heating rate 1 DEG C/min, is incubated 1 hour.Then cool down
To 75 DEG C, again washing, wash time keeps 1 hour, and washing terminal ensures that filter cake sulfur content is less than 0.3%.
2. by washing qualified after filter cake, with 300,000 Ω cm deionized waters pull an oar, control concentration of slurry is 290g/L, then
Pressing dry through pressure filter, controlling cake moisture is 45%.
3. after taking off cake, filter cake is delivered to expansion drying main frame, in expansion drying main frame, inputs hot-air simultaneously, keep filter cake
96 DEG C are reached with temperature after hot air.High speed agitator is set bottom expansion drying machine host, filter cake is broken up rapidly,
Under hot-air stream and air-introduced machine act on jointly, material in 3～5 seconds by the mistake rising very rapidly up to exsiccator top bottom exsiccator
Journey is oven-dried.Top arranges cyclone classifier, and defective material is returned expansion drying motor spindle and again dries；Qualified baking
Dry material is by air-introduced machine suction pulse dust collector and be attached to filter bag of dust collector surface, by electromagnetism Rapping apparatus and compressed air
The impact of stream, makes material fall into bottom pulse dust collector, collects storage bin by auger conveyor and star discharge valve, passes through
Micron disintegrator i.e. obtains high-specific surface area titanium dioxide product after pulverizing.
Claims (7)
1. the preparation method of a high-specific surface area titanium dioxide, it is characterised in that comprise the following steps:
A. by the metatitanic acid after washing, it is neutralized to pH value 8～10 with ammonia, has neutralized rear material and be warming up to 90 DEG C, insulation
Certain time, cooling, again wash；
B. by the filter cake making beating after washing, press dry through pressure filter；
C. after taking off cake, filter cake being delivered to flash dryer and is dried, then pulverize through micron disintegrator, the final height for preparing compares
Surface area titanium dioxide.
2. preparation method as claimed in claim 1, it is characterised in that in step A, metatitanic acid used is that ilmenite is through acidolysis, water
After product after solution, and washing, specific surface area is preferably up to 350m2/ more than g, concentration is adjusted to 200 ± 20g/L.
3. preparation method as claimed in claim 1 or 2, it is characterised in that in step A, ammonia mass percent concentration used is
20 ± 2%, N-process need to keep 1 hour, must be stirred while neutralization.
4. preparation method as claimed in claim 3, it is characterised in that be neutralized to pH value 9～10 with ammonia in step A.
5. preparation method as claimed in claim 3, it is characterised in that neutralized rear material in step A and be warming up to 90 DEG C, risen
Temperature speed is 1 DEG C/min, is incubated 1 hour.Being subsequently cooled to 75 DEG C, again wash, wash time keeps 1 hour,
Washing terminal ensures that filter cake sulfur content is less than 0.3%.
6. preparation method as claimed in claim 1, it is characterised in that by the filter cake after washing in step B, preferably with 300,000 Ω cm
Deionized water is pulled an oar, and control concentration of slurry is 300 ± 20g/L, then press dry through pressure filter, and controlling cake moisture is 45～55%.
7. preparation method as claimed in claim 1, it is characterised in that in step C, filter cake is delivered to expansion drying main frame, with
Time in expansion drying main frame, input hot-air, after keeping filter cake and hot air, temperature reaches 90～105 DEG C.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106830064A (en) * | 2017-01-10 | 2017-06-13 | 四川龙蟒钛业股份有限公司 | Metatitanic acid wet desulphurization method |
| CN106986380A (en) * | 2017-04-24 | 2017-07-28 | 四川龙蟒钛业股份有限公司 | The method that metatitanic acid calcines production titanium dioxide base-material without sulphur |
| CN108731429A (en) * | 2018-06-15 | 2018-11-02 | 山东鲁北企业集团总公司 | A kind of ferric phosphate continuous dehydration and crystal form controllable system and its control method |
| CN109911932A (en) * | 2017-12-13 | 2019-06-21 | 广西金茂钛业有限公司 | Plastic masterbatch special titanium pigment |
| CN109908918A (en) * | 2017-12-13 | 2019-06-21 | 广西金茂钛业有限公司 | Photocatalyst material |
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| CN106986380A (en) * | 2017-04-24 | 2017-07-28 | 四川龙蟒钛业股份有限公司 | The method that metatitanic acid calcines production titanium dioxide base-material without sulphur |
| CN109911932A (en) * | 2017-12-13 | 2019-06-21 | 广西金茂钛业有限公司 | Plastic masterbatch special titanium pigment |
| CN109908918A (en) * | 2017-12-13 | 2019-06-21 | 广西金茂钛业有限公司 | Photocatalyst material |
| CN108731429A (en) * | 2018-06-15 | 2018-11-02 | 山东鲁北企业集团总公司 | A kind of ferric phosphate continuous dehydration and crystal form controllable system and its control method |
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Address after: 543399 Tengxian Chemical Industry Zone, Wuzhou City, Guangxi Zhuang Autonomous Region Patentee after: Guangxi Jinmao Titanium Industry Co.,Ltd. Address before: 543300 Tengxian Chemical Industry Park, Guangxi (Pingzheng Village, Tengzhou Town, the original plant area of Tengxian Resin Factory) Patentee before: GUANGXI JINMAO TITANIUM Co.,Ltd. |
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| PE01 | Entry into force of the registration of the contract for pledge of patent right | ||
| PE01 | Entry into force of the registration of the contract for pledge of patent right |
Denomination of invention: A preparation method of high specific surface area titanium dioxide powder Effective date of registration: 20230822 Granted publication date: 20181009 Pledgee: Tengxian Rural Credit Cooperative Association Pledgor: Guangxi Jinmao Titanium Industry Co.,Ltd. Registration number: Y2023980053145 |