CN1752016A - A kind of novel nano-titanium dioxide powder preparation method - Google Patents
A kind of novel nano-titanium dioxide powder preparation method Download PDFInfo
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- CN1752016A CN1752016A CN 200510028250 CN200510028250A CN1752016A CN 1752016 A CN1752016 A CN 1752016A CN 200510028250 CN200510028250 CN 200510028250 CN 200510028250 A CN200510028250 A CN 200510028250A CN 1752016 A CN1752016 A CN 1752016A
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- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 title claims abstract description 24
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 239000000843 powder Substances 0.000 title abstract description 15
- 239000010936 titanium Substances 0.000 claims abstract description 51
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 39
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 37
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 30
- 239000002243 precursor Substances 0.000 claims abstract description 28
- 238000000034 method Methods 0.000 claims abstract description 21
- 239000000243 solution Substances 0.000 claims abstract description 12
- 239000000126 substance Substances 0.000 claims abstract description 11
- 150000007524 organic acids Chemical class 0.000 claims abstract description 10
- 239000007864 aqueous solution Substances 0.000 claims abstract description 5
- 239000007790 solid phase Substances 0.000 claims abstract description 3
- 239000002244 precipitate Substances 0.000 claims abstract 3
- 230000009466 transformation Effects 0.000 claims abstract 2
- 239000000047 product Substances 0.000 claims description 42
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 27
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 24
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 24
- 238000001354 calcination Methods 0.000 claims description 14
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 12
- 239000012043 crude product Substances 0.000 claims description 12
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 12
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 9
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 claims description 6
- XJDNKRIXUMDJCW-UHFFFAOYSA-J titanium tetrachloride Chemical compound Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 0.000 claims description 5
- FEWJPZIEWOKRBE-JCYAYHJZSA-N Dextrotartaric acid Chemical compound OC(=O)[C@H](O)[C@@H](O)C(O)=O FEWJPZIEWOKRBE-JCYAYHJZSA-N 0.000 claims description 4
- 238000010298 pulverizing process Methods 0.000 claims description 4
- 239000002994 raw material Substances 0.000 claims description 4
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 claims description 3
- 235000019253 formic acid Nutrition 0.000 claims description 3
- DCKVFVYPWDKYDN-UHFFFAOYSA-L oxygen(2-);titanium(4+);sulfate Chemical compound [O-2].[Ti+4].[O-]S([O-])(=O)=O DCKVFVYPWDKYDN-UHFFFAOYSA-L 0.000 claims description 3
- 150000003839 salts Chemical class 0.000 claims description 3
- 229910000348 titanium sulfate Inorganic materials 0.000 claims description 3
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims 5
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims 3
- YGSDEFSMJLZEOE-UHFFFAOYSA-N salicylic acid Chemical compound OC(=O)C1=CC=CC=C1O YGSDEFSMJLZEOE-UHFFFAOYSA-N 0.000 claims 2
- FEWJPZIEWOKRBE-UHFFFAOYSA-N Tartaric acid Natural products [H+].[H+].[O-]C(=O)C(O)C(O)C([O-])=O FEWJPZIEWOKRBE-UHFFFAOYSA-N 0.000 claims 1
- 235000011054 acetic acid Nutrition 0.000 claims 1
- 235000015165 citric acid Nutrition 0.000 claims 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 claims 1
- FJKROLUGYXJWQN-UHFFFAOYSA-N papa-hydroxy-benzoic acid Natural products OC(=O)C1=CC=C(O)C=C1 FJKROLUGYXJWQN-UHFFFAOYSA-N 0.000 claims 1
- 229960004889 salicylic acid Drugs 0.000 claims 1
- 239000011975 tartaric acid Substances 0.000 claims 1
- 235000002906 tartaric acid Nutrition 0.000 claims 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 abstract description 40
- 239000002245 particle Substances 0.000 abstract description 18
- -1 coatings Substances 0.000 abstract description 7
- 238000000576 coating method Methods 0.000 abstract description 2
- 239000004033 plastic Substances 0.000 abstract description 2
- 229920003023 plastic Polymers 0.000 abstract description 2
- 239000002537 cosmetic Substances 0.000 abstract 1
- 239000007789 gas Substances 0.000 description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 10
- 238000001556 precipitation Methods 0.000 description 9
- 235000017550 sodium carbonate Nutrition 0.000 description 7
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 7
- 238000004519 manufacturing process Methods 0.000 description 6
- 238000002156 mixing Methods 0.000 description 6
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 description 6
- 238000010792 warming Methods 0.000 description 6
- 241000370738 Chlorion Species 0.000 description 5
- 238000005054 agglomeration Methods 0.000 description 5
- 230000002776 aggregation Effects 0.000 description 5
- 230000007062 hydrolysis Effects 0.000 description 5
- 238000006460 hydrolysis reaction Methods 0.000 description 5
- 238000000634 powder X-ray diffraction Methods 0.000 description 5
- 238000005406 washing Methods 0.000 description 5
- 238000006243 chemical reaction Methods 0.000 description 4
- 238000001514 detection method Methods 0.000 description 4
- 239000006210 lotion Substances 0.000 description 4
- 229910052573 porcelain Inorganic materials 0.000 description 4
- 239000003795 chemical substances by application Substances 0.000 description 3
- 230000007812 deficiency Effects 0.000 description 3
- 229910001961 silver nitrate Inorganic materials 0.000 description 3
- 229940095064 tartrate Drugs 0.000 description 3
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 description 2
- 239000003513 alkali Substances 0.000 description 2
- CUBCNYWQJHBXIY-UHFFFAOYSA-N benzoic acid;2-hydroxybenzoic acid Chemical compound OC(=O)C1=CC=CC=C1.OC(=O)C1=CC=CC=C1O CUBCNYWQJHBXIY-UHFFFAOYSA-N 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000000354 decomposition reaction Methods 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000001027 hydrothermal synthesis Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000000593 microemulsion method Methods 0.000 description 2
- 239000012716 precipitator Substances 0.000 description 2
- 238000003980 solgel method Methods 0.000 description 2
- 150000003608 titanium Chemical class 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 1
- BDAGIHXWWSANSR-UHFFFAOYSA-M Formate Chemical compound [O-]C=O BDAGIHXWWSANSR-UHFFFAOYSA-M 0.000 description 1
- FKNQFGJONOIPTF-UHFFFAOYSA-N Sodium cation Chemical compound [Na+] FKNQFGJONOIPTF-UHFFFAOYSA-N 0.000 description 1
- 229910010413 TiO 2 Inorganic materials 0.000 description 1
- 230000003373 anti-fouling effect Effects 0.000 description 1
- 230000001857 anti-mycotic effect Effects 0.000 description 1
- 230000002421 anti-septic effect Effects 0.000 description 1
- 239000002543 antimycotic Substances 0.000 description 1
- WDIHJSXYQDMJHN-UHFFFAOYSA-L barium chloride Chemical compound [Cl-].[Cl-].[Ba+2] WDIHJSXYQDMJHN-UHFFFAOYSA-L 0.000 description 1
- 229940045511 barium chloride Drugs 0.000 description 1
- 229910001626 barium chloride Inorganic materials 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 235000011089 carbon dioxide Nutrition 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 210000003298 dental enamel Anatomy 0.000 description 1
- 238000004332 deodorization Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 239000012776 electronic material Substances 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 238000005755 formation reaction Methods 0.000 description 1
- 238000001879 gelation Methods 0.000 description 1
- 230000003301 hydrolyzing effect Effects 0.000 description 1
- 239000003317 industrial substance Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000004530 micro-emulsion Substances 0.000 description 1
- 230000001699 photocatalysis Effects 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 238000006068 polycondensation reaction Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 239000005060 rubber Substances 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 229910001415 sodium ion Inorganic materials 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 229920002994 synthetic fiber Polymers 0.000 description 1
- WRWQVSOJXAVREP-UHFFFAOYSA-J tetrachlorotitanium hydrochloride Chemical compound Cl.[Cl-].[Cl-].[Cl-].[Cl-].[Ti+4] WRWQVSOJXAVREP-UHFFFAOYSA-J 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
Landscapes
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
本发明属于化工技术领域，具体涉及一种新型的纳米二氧化钛粉体制备方法。本发明采用固－固相转化的方法，将相应量的钛源的盐酸溶液加入到适量碱性物质的水溶液中，控制体系pH为7～8，此时有白色的Ti(OH) 4沉淀生成，沉淀经过滤洗涤后，加入适量的有机酸，充分混合，获得前驱物。将前驱物在空气中550－650℃条件下煅烧0.5～1.5h，得到锐钛型的纳米二氧化钛，粒径为15～20nm；前驱物如果在750－850℃条件下煅烧0.5～2.5h，则获得金红石型纳米二氧化钛，粒径为20～25nm。制得的纳米二氧化钛可广泛应用于高档化妆品、涂料、塑料等领域。The invention belongs to the technical field of chemical industry, and in particular relates to a novel preparation method of nano titanium dioxide powder. The present invention adopts the method of solid-solid phase transformation, adding a corresponding amount of hydrochloric acid solution of titanium source into an appropriate amount of alkaline substance aqueous solution, and controlling the pH of the system to be 7-8, at this time, white Ti(OH) 4 precipitates to form , after the precipitate is filtered and washed, an appropriate amount of organic acid is added and mixed thoroughly to obtain a precursor. The precursor is calcined at 550-650°C in air for 0.5-1.5h to obtain anatase nano-titanium dioxide with a particle size of 15-20nm; if the precursor is calcined at 750-850°C for 0.5-2.5h, then The rutile-type nano-titanium dioxide is obtained, and the particle diameter is 20-25 nm. The prepared nano-titanium dioxide can be widely used in high-grade cosmetics, coatings, plastics and other fields.
Description
Technical field
The invention belongs to chemical technology field, be specifically related to a kind of novel nano-titanium dioxide powder preparation method.
Background technology
Nano titanium oxide is a kind of very important industrial chemicals, is divided into anatase titanium dioxide, rutile-type and three kinds of crystal formations of plate titanium type.Nanometer anatase titania is as a kind of novel photocatalysis agent, anti UV agent and photovoltaic effect agent, at antimycotic antiseptic, purify air, deodorization, water treatment, aspect such as antifouling demonstrate wide application prospect.Advantages such as rutile type nano titanic oxide has specific refractory power height, good weatherability, photochemical activity is little, opacifying power is big, physical and chemical performance is stable, be the indispensable raw materials in field such as electronics, light industry, chemical industry, be widely used in fields such as plastics, enamel, artificial fiber, electronic material, rubber, coating.
At present, the preparation method of relevant nano titanium oxide mainly contains: hydrothermal synthesis method, control hydrolysis method, sol-gel method, microemulsion method, the precipitator method, chemical Vapor deposition process etc.Hydrothermal synthesis method, the advantage of this method are that the product crystallization degree is good, and deficiency is that reaction conditions is high temperature, high pressure, thereby aspects such as equipment material, safety are required harsh.The control hydrolysis method makes titanium salt hydrolysis under the condition of strictness control by regulating the hydrolysis rate of titanium salt, can make nano-titanium dioxide powder.The advantage of this method is simple to operate, and cost is cheap relatively, easily takes place in washing and filtering and the drying process to run off and agglomeration but exist, and causes nano-TiO
2Yield and particle diameter all be affected.Sol-gel method is to be raw material with the titanium alkoxide, is hydrolyzed in organic medium, polycondensation, makes solution behind colloidal sol, gelation process, and gel drying is sintered into the method for powder.The nano titanium dioxide powder particle diameter of this method preparation is little, is evenly distributed good dispersity, but owing to will be raw material with the titanium alkoxide, add a large amount of organic reagents again, cost is higher, owing to the generation of gel, organic reagent is difficult for overflowing simultaneously, and dry, sintering process easily produces Prevent Carbon Contamination.Microemulsion method though the structure of microemulsion has fundamentally limited the particulate growth, makes the preparation of ultrafine powder become easy.But this method only is suitable for laboratory study, is not suitable for suitability for industrialized production.At present, main employing is the control hydrolysis method and the precipitator method in the production, the advantage of these two class methods is production efficiency height, cost is low, pollution is little, deficiency is that these two class methods will directly be calcined with the precursor that alkali precipitation or hydrolytic precipitation obtain, there are deficiencies such as particle diameter is inhomogeneous, product is easily reunited, purity is low, limited the performance of the many excellent properties of product.
Summary of the invention
The objective of the invention is to propose a kind of reducing production costs, solve the novel nano-titanium dioxide powder preparation method of traditional agglomeration traits.
The novel nano-titanium dioxide powder preparation method that the present invention proposes, the method that adopts solid-solid phase to transform makes the titanium dioxide powder material, and its concrete steps are: the titanium source is joined in the hydrochloric acid soln, obtain the hydrochloric acid soln in titanium source; Hydrochloric acid soln with the titanium source joins in the aqueous solution of alkaline matter then, and the pH of the hierarchy of control is 7～8, generates the Ti (OH) of white
4Precipitation is filtered, and cleans, and obtains precipitated product Ti (OH)
4Again to precipitated product Ti (OH)
4In add organic acid, thorough mixing makes the oxyhydroxide of titanium be converted into the organic salt of titanium, obtains precursor; The precursor that obtains is put into crucible place the retort furnace calcination, obtain thick finished product; Again thick finished product is pulverized, obtained required product.
Actual conditions is:
The volumetric molar concentration of the hydrochloric acid soln that dissolving titanium source is used is 2～4mol/L;
The hydrochloric acid soln volumetric molar concentration in titanium source is 0.1～8mol/L;
Alkaline matter can adopt a kind of of ammoniacal liquor, yellow soda ash, sodium hydroxide, potassium hydroxide etc., and when alkaline matter was ammoniacal liquor, the volume ratio in ammoniacal liquor and titanium source was 0.8: 1～1.4: 1; When alkaline matter was yellow soda ash, the mass ratio in yellow soda ash and titanium source was 0.8: 1～1.2: 1; When alkaline matter was sodium hydroxide or potassium hydroxide, the mass ratio in sodium hydroxide or potassium hydroxide and titanium source was: 1: 0.2～1: 0.6;
The mass ratio in organic acid and titanium source is 0.8: 1～1.4: 1;
Calcination: precursor was calcined 0.5～1.5 hour under 550～650 ℃ of conditions, obtained the nano titanium oxide of anatase titanium dioxide; Under 750～850 ℃ of conditions, calcined 0.5～2.5 hour, obtain the nano titanium oxide of rutile-type;
Above-mentioned titanium source is a kind of of titanium tetrachloride, titanium sulfate.
Among the present invention, described organic acid can be a kind of of formic acid, acetate, tartrate, citric acid, Whitfield's ointment etc.
Among the present invention, pulverizing can be adopted ball mill or micronizer mill.
The present invention's implementation condition preferably is:
Alkaline matter is a kind of of ammoniacal liquor, yellow soda ash.
The volume ratio in ammoniacal liquor and titanium source is 0.9: 1～1.1: 1.
The mass ratio in yellow soda ash and titanium source is 0.9: 1～1.1: 1.
The mass ratio in sodium hydroxide or potassium hydroxide and titanium source is: 1: 0.3～1: 0.5.
The mass ratio in organic acid and titanium source is 0.9: 1～1.1: 1.
Among the present invention, cleaning is in order effectively to remove foreign ion, as chlorion, ammonium ion or sodium ion etc.
Among the present invention, because the precursor of gained is organic acid salt (as the formate of titanium, a tartrate etc.), organic acid salt can produce a large amount of pollution-free gases in decomposition course, as gases such as carbonic acid gas, water vapors, make reaction system loose, prevented the generation of agglomeration effectively.
The product of the present invention through obtaining after calcining detects through transmission electron microscope, and the particle diameter of anatase titanium dioxide product is 15～20nm, and the particle diameter of rutile titanium dioxide product is 20～25nm.
The present invention has following advantage:
1, proposes first in the product that alkali precipitation obtains, to add organic acid, the organic acid salt that the oxyhydroxide of titanium is converted into titanium is prepared target product as precursor by solid-solid reaction.Because precursor is an organic salt, has produced a large amount of nonstaining property gases in decomposition course, make reaction system loose, effectively prevented the generation of agglomeration.
2, the used starting material of the present invention source is sufficient and cheap, and energy consumption is little in the production process, low production cost.
3, the product that utilizes the present invention to prepare is compared with like product, has the purity height, and whiteness is good, the little and homogeneous of particle diameter, and no agglomeration is easy to characteristics such as dispersion.
Embodiment
The present invention is further illustrated below by specific embodiment.
Embodiment 1:
Get 50ml, volumetric molar concentration is 0.1mol/L titanium tetrachloride hydrochloric acid (volumetric molar concentration is a 2mol/L) solution, join in the 400ml aqueous solution that contains 25ml ammoniacal liquor, this moment adularescent Ti (OH)
4Precipitation generates, and filters, and water cleans 2～3 times, till existing with the no chlorion of Silver Nitrate detection to washing lotion, obtains precipitated product.Add citric acid 1g in the precipitated product that obtains, thorough mixing obtains precursor.Precursor is put into porcelain crucible be placed on retort furnace, slowly be warming up to 600 ℃, calcining 1h obtains crude product.This crude product obtains nano-titanium dioxide powder 0.4g after pulverizing through ball mill pulverizer.X ray powder diffraction instrument (XRD) analytical results shows that this product is the anatase crystal structure; By tem study, the particle diameter of product is 17nm.If precursor ball mill pulverizing behind calcining 0.5h under 850 ℃ of conditions then obtains rutile type nano titanic oxide 0.4g, by tem study, the particle diameter of product is 22nm.
Embodiment 2:
Get 50ml, volumetric molar concentration is hydrochloric acid (volumetric molar concentration the is 3mol/L) solution of 5mol/L titanium sulfate, join in the 400ml water that contains 20g sodium hydroxide, this moment adularescent Ti (OH)
4Precipitation generates, and filters, and water cleans 2～3 times, till existing with the no chlorion of bariumchloride detection to washing lotion, obtains precipitated product.Add formic acid 55ml in the precipitated product that obtains, thorough mixing obtains precursor.Precursor is put into porcelain crucible be placed on retort furnace, slowly be warming up to 650 ℃, calcining 0.5h obtains the nano titanium oxide crude product.This crude product obtains nano-titanium dioxide powder 19g through comminution by gas stream.Analyze by x ray powder diffraction instrument (XRD), this product is a nanometer anatase titania; By tem study, the particle diameter of product is 20nm.If precursor is comminution by gas stream behind calcining 1.5h under 800 ℃ of conditions, then obtain rutile type nano titanic oxide, by tem study, the particle diameter of product is 25nm.
Embodiment 3:
Get 50ml, volumetric molar concentration is hydrochloric acid (volumetric molar concentration the is 4mol/L) solution of 5mol/L titanium tetrachloride, join in the 400ml water that contains 50g yellow soda ash, this moment adularescent Ti (OH)
4Precipitation generates, and filters, and water cleans 2-3 time, till existing with the no chlorion of Silver Nitrate detection to washing lotion, obtains precipitated product.Add Whitfield's ointment 27g in the precipitated product that obtains, thorough mixing obtains precursor, and precursor is placed porcelain crucible, again porcelain crucible is put into retort furnace, slowly is warming up to 600 ℃, and calcining 1h obtains the nano titanium oxide crude product.Crude product obtains end product 10g behind comminution by gas stream.Analyze by x ray powder diffraction instrument (XRD), this product is a nanometer anatase titania; By tem study, the particle diameter of product is 20nm.If precursor is comminution by gas stream behind calcining 2.5h under 750 ℃ of conditions, then obtain rutile type nano titanic oxide 10g, by tem study, the particle diameter of product is 25nm.
Embodiment 4:
Get 50ml, volumetric molar concentration is hydrochloric acid (volumetric molar concentration the is 4mol/L) solution of 5mol/L titanium tetrachloride, join in the 400ml water that contains 50g yellow soda ash, this moment adularescent Ti (OH)
4Precipitation generates, and filters, and water cleans 2-3 time, till existing with the no chlorion of Silver Nitrate detection to washing lotion, obtains precipitated product.Add acetate 55ml in the precipitated product that obtains, thorough mixing obtains precursor.Precursor is put into behind the crucible as for retort furnace, slowly be warming up to 650 ℃, calcining 0.5h obtains the nano titanium oxide crude product, pulverizes through micronizer mill, obtains final product 21g.Analyze by x ray powder diffraction instrument (XRD), this product is a nanometer anatase titania; By tem study, the particle diameter of product is 19nm.If precursor is comminution by gas stream again behind calcining 1h under 800 ℃ of conditions, then obtain rutile type nano titanic oxide, by tem study, the particle diameter of product is 24nm.
Embodiment 5:
Get 50ml, volumetric molar concentration is hydrochloric acid (volumetric molar concentration the is 4mol/L) solution of 8mol/L titanium tetrachloride, join in the 400ml aqueous solution that contains 100ml ammoniacal liquor, this moment adularescent Ti (OH)
4Precipitation generates, and filters, and water cleans 2-3 time, obtains precipitated product.Add tartrate 80g in the precipitated product that obtains, thorough mixing obtains precursor.Precursor is put into crucible be placed on retort furnace, slowly be warming up to 550 ℃, calcining 1.5h gets crude product.This crude product obtains nano-titanium dioxide powder 32g behind comminution by gas stream.Analyze by x ray powder diffraction instrument (XRD), this powder is an anatase titanium dioxide; By tem study, the particle diameter of product is 18nm.Slowly be warming up to 850 ℃ as precursor, calcining 0.5h, the crude product that obtains then obtains rutile type nano titanic oxide behind comminution by gas stream, and by tem study, the particle diameter of product is 40nm.
Claims (8)
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100453466C (en) * | 2006-12-20 | 2009-01-21 | 中国科学院山西煤炭化学研究所 | A kind of method for the synthesis of nano anatase titanium dioxide of non-aqueous system |
| CN101654280B (en) * | 2009-08-25 | 2011-04-13 | 苏州大学 | Preparation method of titanium dioxide nano powder |
| CN102600880A (en) * | 2012-01-29 | 2012-07-25 | 北京科技大学 | Preparation method of visible light-response titanium dioxide photocatalytic liquid |
| CN102107907B (en) * | 2009-12-28 | 2012-11-28 | 中国科学院金属研究所 | Porous nano hydrated titanium dioxide dearsenifying material and preparation method thereof |
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| US6440383B1 (en) * | 1999-06-24 | 2002-08-27 | Altair Nanomaterials Inc. | Processing aqueous titanium chloride solutions to ultrafine titanium dioxide |
| US6375923B1 (en) * | 1999-06-24 | 2002-04-23 | Altair Nanomaterials Inc. | Processing titaniferous ore to titanium dioxide pigment |
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| CN1363520A (en) * | 2001-01-09 | 2002-08-14 | 攀枝花市永禄科技开发有限责任公司 | Process for preparing rutile crystal type nano TiO2 |
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2005
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| CN100453466C (en) * | 2006-12-20 | 2009-01-21 | 中国科学院山西煤炭化学研究所 | A kind of method for the synthesis of nano anatase titanium dioxide of non-aqueous system |
| CN101654280B (en) * | 2009-08-25 | 2011-04-13 | 苏州大学 | Preparation method of titanium dioxide nano powder |
| CN102107907B (en) * | 2009-12-28 | 2012-11-28 | 中国科学院金属研究所 | Porous nano hydrated titanium dioxide dearsenifying material and preparation method thereof |
| CN102600880A (en) * | 2012-01-29 | 2012-07-25 | 北京科技大学 | Preparation method of visible light-response titanium dioxide photocatalytic liquid |
| CN103754930A (en) * | 2014-01-07 | 2014-04-30 | 福建师范大学 | An ordered superstructure of octahedral anatase TiO2 and its preparation and application |
| CN103754930B (en) * | 2014-01-07 | 2015-07-22 | 福建师范大学 | An ordered superstructure of octahedral anatase TiO2 and its preparation and application |
| CN108516584A (en) * | 2018-07-09 | 2018-09-11 | 江苏中研创星材料科技有限公司 | A kind of preparation method of high-purity super large specific surface poriferous titanium dioxide |
| CN108516584B (en) * | 2018-07-09 | 2020-05-08 | 江苏中研创星材料科技有限公司 | Preparation method of high-purity super-large specific surface porous titanium dioxide |
| CN110943171A (en) * | 2018-09-21 | 2020-03-31 | Tcl集团股份有限公司 | Quantum dot light-emitting diode and preparation method thereof |
| WO2021028769A1 (en) * | 2019-08-13 | 2021-02-18 | Vice Chancellor, Sabaragamuwa University Of Sri Lanka | Process and system for extarcting titanium dioxide nanomaterials from natural ilmenite |
| CN114105194A (en) * | 2021-12-24 | 2022-03-01 | 济南裕兴化工有限责任公司 | Method for promoting crystal form transformation of titanium white |
| CN114105194B (en) * | 2021-12-24 | 2023-10-24 | 济南裕兴化工有限责任公司 | A method to promote the transformation of titanium dioxide crystal form |
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