CN101029187A - High-water-dispersibility titanium dioxide and preparation method thereof - Google Patents
High-water-dispersibility titanium dioxide and preparation method thereof Download PDFInfo
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- CN101029187A CN101029187A CN 200610082392 CN200610082392A CN101029187A CN 101029187 A CN101029187 A CN 101029187A CN 200610082392 CN200610082392 CN 200610082392 CN 200610082392 A CN200610082392 A CN 200610082392A CN 101029187 A CN101029187 A CN 101029187A
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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims abstract description 147
- 239000004408 titanium dioxide Substances 0.000 title claims abstract description 57
- 238000002360 preparation method Methods 0.000 title description 11
- 238000000034 method Methods 0.000 claims abstract description 45
- 238000001354 calcination Methods 0.000 claims abstract description 19
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000002270 dispersing agent Substances 0.000 claims abstract description 13
- 230000001804 emulsifying effect Effects 0.000 claims abstract description 13
- 238000004519 manufacturing process Methods 0.000 claims abstract description 8
- 239000002994 raw material Substances 0.000 claims abstract description 6
- 235000010215 titanium dioxide Nutrition 0.000 claims description 61
- 239000002253 acid Substances 0.000 claims description 47
- 229910010413 TiO 2 Inorganic materials 0.000 claims description 25
- ADCOVFLJGNWWNZ-UHFFFAOYSA-N antimony trioxide Chemical compound O=[Sb]O[Sb]=O ADCOVFLJGNWWNZ-UHFFFAOYSA-N 0.000 claims description 16
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 14
- GNTDGMZSJNCJKK-UHFFFAOYSA-N divanadium pentaoxide Chemical compound O=[V](=O)O[V](=O)=O GNTDGMZSJNCJKK-UHFFFAOYSA-N 0.000 claims description 14
- 239000003795 chemical substances by application Substances 0.000 claims description 11
- 150000003839 salts Chemical class 0.000 claims description 11
- 239000002002 slurry Substances 0.000 claims description 11
- 238000003756 stirring Methods 0.000 claims description 11
- CHWRSCGUEQEHOH-UHFFFAOYSA-N potassium oxide Chemical compound [O-2].[K+].[K+] CHWRSCGUEQEHOH-UHFFFAOYSA-N 0.000 claims description 10
- 229910001950 potassium oxide Inorganic materials 0.000 claims description 10
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 9
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 7
- 238000009826 distribution Methods 0.000 claims description 7
- 239000012065 filter cake Substances 0.000 claims description 7
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical class [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 claims description 7
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 6
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 6
- 239000004202 carbamide Substances 0.000 claims description 6
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims description 6
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 claims description 5
- 230000003472 neutralizing effect Effects 0.000 claims description 5
- 150000003863 ammonium salts Chemical class 0.000 claims description 4
- 150000003016 phosphoric acids Chemical class 0.000 claims description 4
- 239000001103 potassium chloride Substances 0.000 claims description 4
- 235000011164 potassium chloride Nutrition 0.000 claims description 4
- 238000010009 beating Methods 0.000 claims description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical group [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 2
- 239000008187 granular material Substances 0.000 claims 1
- 239000000049 pigment Substances 0.000 abstract description 10
- 239000011248 coating agent Substances 0.000 abstract description 8
- 238000000576 coating method Methods 0.000 abstract description 8
- 238000005265 energy consumption Methods 0.000 abstract description 3
- 238000003860 storage Methods 0.000 abstract description 3
- 239000003973 paint Substances 0.000 abstract description 2
- 239000000047 product Substances 0.000 description 10
- 239000002245 particle Substances 0.000 description 9
- 239000000843 powder Substances 0.000 description 9
- 208000006558 Dental Calculus Diseases 0.000 description 6
- 238000000227 grinding Methods 0.000 description 6
- 238000001514 detection method Methods 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 3
- MNNHAPBLZZVQHP-UHFFFAOYSA-N diammonium hydrogen phosphate Chemical compound [NH4+].[NH4+].OP([O-])([O-])=O MNNHAPBLZZVQHP-UHFFFAOYSA-N 0.000 description 3
- -1 papermaking Substances 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 239000001038 titanium pigment Substances 0.000 description 3
- 238000005406 washing Methods 0.000 description 3
- 239000004254 Ammonium phosphate Substances 0.000 description 2
- 229910000831 Steel Inorganic materials 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 229910000148 ammonium phosphate Inorganic materials 0.000 description 2
- 235000019289 ammonium phosphates Nutrition 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 238000001493 electron microscopy Methods 0.000 description 2
- 238000004945 emulsification Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 238000012423 maintenance Methods 0.000 description 2
- 238000010298 pulverizing process Methods 0.000 description 2
- 239000010959 steel Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000004094 surface-active agent Substances 0.000 description 2
- LWIHDJKSTIGBAC-UHFFFAOYSA-K tripotassium phosphate Chemical compound [K+].[K+].[K+].[O-]P([O-])([O-])=O LWIHDJKSTIGBAC-UHFFFAOYSA-K 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 1
- 241000024287 Areas Species 0.000 description 1
- BVKZGUZCCUSVTD-UHFFFAOYSA-M Bicarbonate Chemical compound OC([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-M 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- 241000976924 Inca Species 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
- 229920003171 Poly (ethylene oxide) Polymers 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 239000013543 active substance Substances 0.000 description 1
- 125000000217 alkyl group Chemical group 0.000 description 1
- 235000012538 ammonium bicarbonate Nutrition 0.000 description 1
- LFVGISIMTYGQHF-UHFFFAOYSA-N ammonium dihydrogen phosphate Chemical compound [NH4+].OP(O)([O-])=O LFVGISIMTYGQHF-UHFFFAOYSA-N 0.000 description 1
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 description 1
- 229910052921 ammonium sulfate Inorganic materials 0.000 description 1
- 235000011130 ammonium sulphate Nutrition 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 238000004061 bleaching Methods 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 230000009194 climbing Effects 0.000 description 1
- 230000001143 conditioned effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 210000003298 dental enamel Anatomy 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- TXKMVPPZCYKFAC-UHFFFAOYSA-N disulfur monoxide Inorganic materials O=S=S TXKMVPPZCYKFAC-UHFFFAOYSA-N 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 239000000839 emulsion Substances 0.000 description 1
- 150000002191 fatty alcohols Chemical class 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 239000003317 industrial substance Substances 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 235000010755 mineral Nutrition 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- CHKVPAROMQMJNQ-UHFFFAOYSA-M potassium bisulfate Chemical compound [K+].OS([O-])(=O)=O CHKVPAROMQMJNQ-UHFFFAOYSA-M 0.000 description 1
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Substances [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 description 1
- 235000015320 potassium carbonate Nutrition 0.000 description 1
- GNSKLFRGEWLPPA-UHFFFAOYSA-M potassium dihydrogen phosphate Chemical compound [K+].OP(O)([O-])=O GNSKLFRGEWLPPA-UHFFFAOYSA-M 0.000 description 1
- 229940093916 potassium phosphate Drugs 0.000 description 1
- 229910000160 potassium phosphate Inorganic materials 0.000 description 1
- 235000011009 potassium phosphates Nutrition 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000005060 rubber Substances 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- XTQHKBHJIVJGKJ-UHFFFAOYSA-N sulfur monoxide Chemical compound S=O XTQHKBHJIVJGKJ-UHFFFAOYSA-N 0.000 description 1
- 238000004381 surface treatment Methods 0.000 description 1
- 238000003466 welding Methods 0.000 description 1
- 238000001238 wet grinding Methods 0.000 description 1
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- Pigments, Carbon Blacks, Or Wood Stains (AREA)
Abstract
The invention provides titanium dioxide, wherein the content of anatase titanium dioxide is not less than 99%, and the water dispersibility value is not less than 92%. The invention also provides a method for preparing the titanium dioxide, namely 0.1-0.4% of emulsifying dispersant is added in the existing production method. The titanium dioxide of the invention can keep the system stability of products such as paint, pigment and the like for a long time, is convenient for transportation and storage, can improve the covering power and mechanical strength of a coating film, and has strong market competitiveness. Meanwhile, the titanium dioxide of the invention can also be widely applied to other fields using anatase titanium dioxide. The method has the advantages of easily available process raw materials, low cost, low energy consumption, easily-reached calcination endpoint, stable and easily-controlled process flow, uniform product properties, no change of the original process flow and equipment, and suitability for large-scale popularization and application.
Description
Technical field
The invention belongs to chemical field, refer more particularly to a kind of high-dispersed titanium pigment and preparation method thereof.
Background technology
Titanium dioxide is one of most important mineral dye and industrial chemicals.The pigment-level titanium dioxide is mainly used in industries such as coating, papermaking, plastics, rubber, emulsion paint, printing-ink, chemical fibre, and non-pigment-level titanium dioxide is mainly used in enamel, electrical condenser, welding electrode etc.If the titanium dioxide water dispersible is bad, is easy to reunite after in coating, disperseing anti-thick phenomenon takes place, thereby produce layering; Have good water dispersible titanium dioxide and then can make the secular maintenance system of coating stable, be convenient to the transportation of coating and storage and can increase the mechanical property of filming etc.
At application number is 01107923.1, name is called that to disclose titanic liquid in the Chinese patent application of " a kind of method of producing nanometer anatase titania " be raw material, heat-up rate with 1～3 ℃/minute under normal pressure is heated to 50～100 ℃, forms metatitanic acid through hydrolysis in 3～8 hours and makes the method for titanium dioxide product through selecting branch and washing, dispersion, roasting, pulverizing.The titanium dioxide that this method is produced needs Raymond mill to pulverize grinding for a long time just can reach 85% water dispersible.
At application number is 200310112000.2, and name is called to disclose with metatitanic acid in the Chinese patent application of " sulfuric acid recycles the method for producing titanium dioxide " produces titanium dioxide through routine washing, bleaching, salt processing, calcining, wet-milling, classification, surface treatment, drying, pulverizing.This method complex process, cost height, and the water dispersible of product＜90%.
Because currently available products exists the not high critical defect of water dispersible, and also there is length consuming time in its preparation method, shortcomings such as the neutralizing agent consumption is big, production cost is high, complex process, energy consumption height.Therefore, need develop anatase titanium dioxide rate height, water dispersible value height, even, the low-cost titanium dioxide product of size distribution; Simultaneously also need to develop a kind of simple, the method for this high-dispersed anatase thpe white powder of feedstock production that economic with the metatitanic acid is.
Summary of the invention
First purpose of the present invention provides a kind of titanium dioxide.The mass percent of contained anatase titanium dioxide is not less than 99% in this titanium dioxide, and the water dispersible value is not less than 92%.
Further, the particle diameter of above-mentioned titanium dioxide 70% is distributed between 200nm～400nm.Second purpose of the present invention provides a kind of method for preparing above-mentioned titanium dioxide.This method is to be raw material with the metatitanic acid slurry, adds 0.1%～0.4% emulsifying dispersant in the process with salt facture production titanium dioxide, and wherein the add-on of emulsifying dispersant is meant and accounts for TiO in the metatitanic acid
2The mass percent of total amount.
Further, this method may further comprise the steps:
A, slurries are made in metatitanic acid making beating, added combination salt treatment agent, stir;
B, adding ammonium or ammoniacal liquor or ammonium salt or urea stir;
The emulsifying dispersant of c, adding 0.1%～0.4%, its add-on is meant and accounts for TiO
2The mass percent of the metatitanic acid total amount of meter stirs, and filters;
D, with step c gained filter cake 900～950 ℃ of calcinings, grind 1～2 hour promptly.
Preferably, the emulsifying dispersant described in the aforesaid method is a nonionogenic tenside.
Preferred, the emulsifying dispersant described in the aforesaid method is a Soxylat A 25-7.
Preferably, the neutralizing agent described in the aforesaid method step b is at least a in ammonium salt, ammoniacal liquor or the urea.
Wherein, the metatitanic acid slurries described in the aforesaid method step a are 200g/L～400g/L by the concentration of titanium dioxide.
Wherein, the combination salt treatment agent described in the aforesaid method step b comprises one or more in following component: a, sylvite, potassium oxide or the potassium hydroxide, and add-on is with TiO
20.35%～0.5% of the quality of the metatitanic acid of meter, quality is calculated with potassium oxide; In b, phosphoric acid or the phosphoric acid salt one or more, add-on are with TiO
20.2%～0.35% of the quality of the metatitanic acid of meter, quality is calculated with Vanadium Pentoxide in FLAKES; C, ANTIMONY TRIOXIDE SB 203 99.8 PCT, add-on are with TiO
20.35%～0.5% of the quality of the metatitanic acid of meter.
Employed salt treatment agent is by salt treatment agent a, sylvite or potassium oxide commonly used in the production process of titanium pigment of this area, in the potassium hydroxide one or more among the inventive method step a; In b, phosphoric acid or the phosphoric acid salt one or more; C, ANTIMONY TRIOXIDE SB 203 99.8 PCT are formed jointly.Sylvite wherein is one or more in salt of wormwood, saleratus, vitriolate of tartar, sal enixum, potassiumphosphate, potassium phosphate,monobasic, potassium primary phosphate, the Repone K; Phosphoric acid salt wherein is one or more in ammonium phosphate, ammonium hydrogen phosphate or the primary ammonium phosphate.
Used neutralizing agent ammonium salt, ammoniacal liquor or urea both can be used for the pH value of conditioned reaction system among the inventive method step b, react the discharging of the more volatile ammonium sulfate minimizing of generation sulfur oxide in the time of can in reaction system, having sulfate radical to exist again with it, improve water dispersible.Volatile salt, hydrogen-carbonate and urea etc. can also form a large amount of bubbles and help emulsification to disperse metatitanic acid is not condensed before calcining, the water dispersible of titanium dioxide is improved.
The present invention selects for use nonionic surface active agent as emulsifying dispersant, and these class tensio-active agent characteristics are unionization in the water, and hydrophilic group mostly is some amount oxy radical ethers or hydroxyl, and oleophilic group is formed for the chain alkyl, has emulsification, dispersion, washing performance.Soxylat A 25-7 is the nonionic surface active agent of using always, is applicable to the preparation of product of the present invention, wherein preferably the carbon chain lengths of oleophilic group at the product of 5-20.General commonly used is alkylphenol polyoxyethylene and this two series products of high fatty alcohol Soxylat A 25-7, such as in o π or the op series one or more: o π-10, o π-15, op-10 or op-15 etc.
The used emulsifying dispersant of the present invention can be in whipping process introducing air or keep gas and the organism that partial reaction produces here, metatitanic acid fully is isolated into small-particle each other to be dispersed in the system, still make the metatitanic acid small-particle do not condensed by many hollow structures are separate after filtering, make the calcining terminal point be easy to arrive, thereby the minimizing calcination time significantly reduces energy consumption and makes that calcining is even more, water dispersible is better.
Calcination process described in the inventive method steps d is to carry out with this areas such as resistance furnace calciner commonly used, generally at 900 ℃～950 ℃ calcining 40min～210min, the time that calcining is carried out can be produced the time grasp of titanium dioxide according to the general calcining in this area, is preferably 45min～85min.
Titanium dioxide of the present invention has high-dispersed and high anatase titanium dioxide concentration characteristics simultaneously, indexs such as the whiteness of this titanium dioxide, reducing power have reached the level of commercially available standard specimen, run-of-the-mill indexs such as oil number, water-soluble salt, pH value all meet country and industry standard, and its size distribution of 70% is in 200nm～400nm scope.Titanium dioxide of the present invention can make product maintenance systems for a long time such as coating and pigment stable, is convenient to transportation and storage and can improves film opacifying power and physical strength, and its performance is increased substantially, and has the very strong market competitiveness.Simultaneously, titanium dioxide of the present invention also can be widely used in other Application Areass of anatase thpe white powder.The inventive method raw materials technology is easy to get, cost is low, consume energy less, the calcining terminal point easily reaches, technological process is steadily easy to control, product property is even, and does not change former technical process and equipment, is fit to very much large-scale promotion application.
Description of drawings
Fig. 1 is a titanium dioxide x x ray diffration pattern x of the present invention, and its main peak is the characteristic peak of anatase titanium dioxide.
Fig. 2 is an anatase thpe white powder particle size distribution figure of the present invention, and prepared as seen from the figure titanium dioxide powder peak value is 307nm, and peak width is 294nm, and 70% is distributed in 200nm～400nm scope.
Obviously, according to foregoing of the present invention,,, can also make modification, replacement or the change of other various ways not breaking away under the above-mentioned basic fundamental thought of the present invention prerequisite according to the ordinary skill knowledge and the customary means of this area.
Foregoing of the present invention further being described in detail by embodiment below in conjunction with accompanying drawing, is limiting the scope of the invention but should not be construed as.
Embodiment
The preparation of embodiment 1 titanium dioxide of the present invention
Pigment-level metatitanic acid slurries are pulled an oar into the solution of 200g/L (in titanium dioxide), get 10 liters, adding with potassium oxide calculated mass percentage ratio is that metatitanic acid is (with TiO
2Meter) 0.35% vitriolate of tartar, be that metatitanic acid is (with TiO with Vanadium Pentoxide in FLAKES calculated mass percentage ratio
2Meter) 0.2% phosphoric acid, mass percent are that metatitanic acid is (with TiO
2Meter) 0.35% ANTIMONY TRIOXIDE SB 203 99.8 PCT stirs.Add ammoniacal liquor and regulate pH value to 8, adding mass percent is that metatitanic acid is (with TiO
2Meter) 0.4% o π-10.
Above-mentioned gained liquid is fully stirred, filters, get filter cake in resistance furnace at 930 ℃ down after the calcining, three-head grinding machine grinds and promptly got anatase thpe white powder A in 1 hour.
The preparation of embodiment 2 titanium dioxides of the present invention
Pigment-level metatitanic acid slurries are pulled an oar into the solution that concentration is 340g/L (in titanium dioxide), get 10 liters, adding mass percent is that metatitanic acid is (with TiO
2Meter) 0.5% vitriolate of tartar (in potassium oxide), mass percent is that metatitanic acid is (with TiO
2Meter) 0.3% phosphoric acid (in Vanadium Pentoxide in FLAKES), mass percent are that metatitanic acid is (with TiO
2Meter) 0.35% ANTIMONY TRIOXIDE SB 203 99.8 PCT stirs.Adding mass percent is the urea of titanium dioxide 5%, and adding mass percent again is that metatitanic acid is (with TiO
2Meter) 0.3% o π-10.
Above-mentioned gained is fully stirred, filters, get filter cake in resistance furnace at 900 ℃ down after the calcining, three-head grinding machine grinds and promptly got anatase thpe white powder B in 2 hours.
The preparation of embodiment 3 titanium dioxides of the present invention
Pigment-level metatitanic acid slurries are pulled an oar into the solution of 340g/L (in titanium dioxide), get 10 liters, adding with potassium oxide calculated mass percentage ratio is that metatitanic acid is (with TiO
2Meter) 0.45% vitriolate of tartar, be that metatitanic acid is (with TiO in the Vanadium Pentoxide in FLAKES mass percent
2Meter) 0.28% phosphoric acid, mass percent are that metatitanic acid is (with TiO
2Meter) 0.45% ANTIMONY TRIOXIDE SB 203 99.8 PCT stirs.Adding mass percent is the volatile salt of titanium dioxide 3%, and adding mass percent again is that metatitanic acid is (with TiO
2Meter) 0.2% o π-10.
Above-mentioned gained is fully stirred, filters, get filter cake in resistance furnace at 950 ℃ down after the calcining, three-head grinding machine grinds and promptly got anatase thpe white powder C in 2 hours.
The preparation of embodiment 4 titanium dioxides of the present invention
Pigment-level metatitanic acid slurries are pulled an oar into the solution of 300g/L (in titanium dioxide), get 10 liters, adding with potassium oxide calculated mass percentage ratio is that metatitanic acid is (with TiO
2Meter) 0.35% vitriolate of tartar, be that metatitanic acid is (with TiO with Vanadium Pentoxide in FLAKES calculated mass percentage ratio
2Meter) 0.28% phosphoric acid, mass percent are that metatitanic acid is (with TiO
2Meter) 0.5% ANTIMONY TRIOXIDE SB 203 99.8 PCT stirs.Adding mass percent is the bicarbonate of ammonia of titanium dioxide 6%, and adding mass percent is that metatitanic acid is (with TiO
2Meter) 0.1% o π-10.
Above-mentioned gained is fully stirred, filters, get filter cake in resistance furnace at 930 ℃ down after the calcining, three-head grinding machine grinds and promptly got anatase thpe white powder D in 2 hours.
The preparation of embodiment 5 titanium dioxides of the present invention
Pigment-level metatitanic acid slurries are pulled an oar into the solution of 400g/L (in titanium dioxide), get 10 liters, adding with potassium oxide calculated mass percentage ratio is that metatitanic acid is (with TiO
2Meter) 0.5% vitriolate of tartar, be that metatitanic acid is (with TiO with Vanadium Pentoxide in FLAKES calculated mass percentage ratio
2Meter) 0.35% ammonium phosphate, mass percent are that metatitanic acid is (with TiO
2Meter) 0.5% ANTIMONY TRIOXIDE SB 203 99.8 PCT stirs.Add ammoniacal liquor and regulate pH value to 5, adding mass percent again is that metatitanic acid is (with TiO
2Meter) 0.2% OP-15.
Above-mentioned gained is fully stirred, filters, get filter cake in resistance furnace at 900 ℃ down after the calcining, three-head grinding machine grinds and promptly got anatase thpe white powder E in 1.5 hours.
The quality examination of test example one titanium dioxide of the present invention
1, detects index and method
The detection method of water dispersible:
The titanium dioxide of getting 15g adds entry making beating and transfers volume to 100ml in the 100ml graduated cylinder, in 80ml scale place with syringe draw the oven dry of 2ml solution claim residue weight m
1, leave standstill after 5 hours again in the sampling 2ml of 80ml place dry resistates m2, the ratio of m2 and ml is the desired value of water dispersible.
Anatase titanium dioxide mass percentage content detecting instrument: D/max-Rc type X-ray diffractometer.
The detecting instrument of whiteness and reducing power: CR-300 type colour-difference meter (making standard specimen) with the titanium white PTA120 that climbs the production of steel titanium powder plant.
2, testing sample
Anatase titanium dioxide A, B, C, D, E that the foregoing description is prepared.
Sell (or prior art produce) coating in the market with climbing steel titanium dioxide PTA120 series of samples F.
Identical with other steps with the embodiment of the invention 3 methods, only do not add the prepared titanium dioxide G of method of emulsifying dispersant.
3, detected result
Table 1 quality examination result
| The water dispersible value | Anatase titanium dioxide content | Whiteness | Reducing power | |
| A | 92％ | 99％ | 100％ | 100％ |
| B | 94％ | 99％ | 100％ | 101％ |
| C | 94％ | 99％ | 100％ | 101％ |
| D | 94％ | 99％ | 100％ | 101％ |
| E | 92％ | 99％ | 100％ | 100％ |
| F | 80％ | 99％ | 100％ | 100％ |
| G | 79％ | 99％ | 100％ | 100％ |
The granularity Detection of test example two titanium dioxides of the present invention and transmission electron microscope observation
1, detects index and method
Granularity Detection instrument: ZETA-1000 type laser particle analyzer
Electron microscopy observation instrument: JSM-5600LV scanning electron microscope+INCA energy spectrometer
2, detected result
Choose the embodiment of the invention 4 prepared titanium dioxides and carry out above-mentioned detection, anatase titanium dioxide rate detected result is seen Fig. 1, and as can be seen from the figure, its main peak is the characteristic peak of anatase titanium dioxide, and its anatase titanium dioxide rate of integral and calculating is greater than 99%.Its size-grade distribution detected result sees Table 2 and Fig. 2, and as seen its particle diameter is distributed in more than 70% between 200nm～400nm, and median size is 270nm～300nm.The electron microscopy observation result shows that the granule-morphology of titanium dioxide of the present invention is the ellipsoid shape, and size evenly.
Table 2 embodiment TiO
2The size-grade distribution detected result
| Particle diameter (nm) | Content (%) | Particle diameter (nm) | Content (%) | Particle diameter (nm) | Content (%) |
| 41.3 | 0.0 | 145.5 | 4.4 | 512.8 | 5.4 |
| 48.3 | 0.0 | 170.3 | 7.3 | 600.2 | 3.0 |
| 56.6 | 0.0 | 199.4 | 10.7 | 702.6 | 1.4 |
| 66.2 | 0.0 | 233.4 | 13.5 | 822.4 | 0.6 |
| 77.5 | 0.1 | 273.1 | 14.8 | 962.6 | 0.2 |
| 90.7 | 0.4 | 319.7 | 14.2 | 1126.8 | 0.1 |
| 106.2 | 1.0 | 374.2 | 11.8 | 1318.9 | 0.0 |
| 124.3 | 2.3 | 438.1 | 8.6 | 1543.8 | 0.0 |
Therefore the water dispersible of titanium dioxide of the present invention is good, anatase titanium dioxide rate height; Granule-morphology is good, interval narrow, the good uniformity of size-grade distribution; Index such as reducing power and whiteness has reached the level of commercially available standard specimen, is a kind of novel high-quality titanium dioxide, is specially adapted to the preparation of coating and pigment.The inventive method raw material is easy to get, cost is low, consume energy less, the calcining terminal point easily reaches, technological process is steadily easy to control, product property even and do not change original technical process and equipment, and good application prospects is arranged.
Claims (10)
1, a kind of titanium dioxide is characterized in that wherein the mass percent of contained anatase titanium dioxide is not less than 99%, and the water dispersible value is not less than 92%.
2, titanium dioxide according to claim 1, the size distribution that it is characterized in that its titanium dioxide granule of 70% is between 200nm～400nm.
3, a kind of method for preparing claim 1 or 2 described titanium dioxides, it is characterized in that: add 0.1%～0.4% emulsifying dispersant in the process that with the metatitanic acid slurry is the raw material production titanium dioxide, wherein the add-on of emulsifying dispersant is meant and accounts for TiO in the metatitanic acid
2The mass percent of total amount.
4, the method for preparing titanium dioxide according to claim 3 is characterized in that may further comprise the steps:
A, slurries are made in metatitanic acid making beating, added combination salt treatment agent, stir;
B, adding neutralizing agent stir;
The emulsifying dispersant of c, adding 0.1%～0.4%, its add-on is meant and accounts for TiO
2The mass percent of the metatitanic acid total amount of meter stirs, and filters;
D, with step c gained filter cake 900～950 ℃ of calcinings, grind 1～2 hour promptly.
5,, it is characterized in that described emulsifying dispersant is a nonionogenic tenside according to claim 3 or the 4 described methods that prepare titanium dioxide.
6,, it is characterized in that described nonionogenic tenside is a Soxylat A 25-7 according to claim 3 or the 4 described methods that prepare titanium dioxide.
7, according to claim 3 or the 4 described methods that prepare titanium dioxide, the carbon chain lengths that it is characterized in that the oleophilic group of described Soxylat A 25-7 is 5～20.
8, the method for preparing titanium dioxide according to claim 4 is characterized in that the neutralizing agent described in the step b is at least a in ammonium salt, ammoniacal liquor or the urea.
9, the method for preparing titanium dioxide according to claim 4, the concentration that it is characterized in that the metatitanic acid slurries described in the step a is by titanium dioxide 200g/L～400g/L.
10, the method for preparing titanium dioxide according to claim 4 is characterized in that the combination salt treatment agent described in the step b comprises one or more in following component: a, sylvite, potassium oxide or the potassium hydroxide, and add-on is with TiO
20.35%～0.5% of the quality of the metatitanic acid of meter, quality is calculated with potassium oxide; In b, phosphoric acid or the phosphoric acid salt one or more, add-on are with TiO
20.2%～0.35% of the quality of the metatitanic acid of meter, quality is calculated with Vanadium Pentoxide in FLAKES; C, ANTIMONY TRIOXIDE SB 203 99.8 PCT, add-on are with TiO
20.35%～0.5% of the quality of the metatitanic acid of meter.
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