CN1511788A - Process for preparing nano titanium dioxide - Google Patents
Process for preparing nano titanium dioxide Download PDFInfo
- Publication number
- CN1511788A CN1511788A CNA021591474A CN02159147A CN1511788A CN 1511788 A CN1511788 A CN 1511788A CN A021591474 A CNA021591474 A CN A021591474A CN 02159147 A CN02159147 A CN 02159147A CN 1511788 A CN1511788 A CN 1511788A
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- CN
- China
- Prior art keywords
- titanium oxide
- nano titanium
- preparation
- nano
- potassium
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- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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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 description 4
- 238000004519 manufacturing process Methods 0.000 title description 3
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 57
- 238000002360 preparation method Methods 0.000 claims abstract description 14
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 11
- 239000013078 crystal Substances 0.000 claims abstract description 11
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000010936 titanium Substances 0.000 claims abstract description 8
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 8
- 230000007062 hydrolysis Effects 0.000 claims abstract description 5
- 238000006460 hydrolysis reaction Methods 0.000 claims abstract description 5
- 238000005406 washing Methods 0.000 claims abstract description 4
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims description 27
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims description 13
- 238000000034 method Methods 0.000 claims description 13
- 229910052700 potassium Inorganic materials 0.000 claims description 13
- 239000004408 titanium dioxide Substances 0.000 claims description 12
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical group C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 11
- 239000011734 sodium Substances 0.000 claims description 11
- 229910052708 sodium Inorganic materials 0.000 claims description 11
- 239000011591 potassium Substances 0.000 claims description 10
- 239000012141 concentrate Substances 0.000 claims description 9
- LOVWJAWJBUACDS-UHFFFAOYSA-N [Ti].[O].[Cl] Chemical compound [Ti].[O].[Cl] LOVWJAWJBUACDS-UHFFFAOYSA-N 0.000 claims description 7
- YDZQQRWRVYGNER-UHFFFAOYSA-N iron;titanium;trihydrate Chemical compound O.O.O.[Ti].[Fe] YDZQQRWRVYGNER-UHFFFAOYSA-N 0.000 claims description 6
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims description 5
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 5
- 238000010521 absorption reaction Methods 0.000 claims description 5
- 239000002994 raw material Substances 0.000 claims description 4
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 claims description 3
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 claims description 3
- 239000001099 ammonium carbonate Substances 0.000 claims description 3
- 235000012501 ammonium carbonate Nutrition 0.000 claims description 3
- 238000001354 calcination Methods 0.000 claims description 3
- 239000000796 flavoring agent Substances 0.000 claims description 3
- 235000019634 flavors Nutrition 0.000 claims description 3
- 230000003301 hydrolyzing effect Effects 0.000 claims description 3
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Substances [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 claims description 3
- 238000001914 filtration Methods 0.000 claims description 2
- 238000000967 suction filtration Methods 0.000 claims description 2
- 239000000543 intermediate Substances 0.000 claims 1
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 abstract description 45
- -1 roasting Substances 0.000 abstract description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 3
- 239000000463 material Substances 0.000 abstract description 2
- 239000003973 paint Substances 0.000 abstract description 2
- 239000004744 fabric Substances 0.000 abstract 1
- 239000013538 functional additive Substances 0.000 abstract 1
- 230000001089 mineralizing effect Effects 0.000 abstract 1
- 239000007789 gas Substances 0.000 description 8
- 239000000243 solution Substances 0.000 description 6
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 3
- 239000003153 chemical reaction reagent Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 2
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 235000011167 hydrochloric acid Nutrition 0.000 description 2
- AMWRITDGCCNYAT-UHFFFAOYSA-L hydroxy(oxo)manganese;manganese Chemical compound [Mn].O[Mn]=O.O[Mn]=O AMWRITDGCCNYAT-UHFFFAOYSA-L 0.000 description 2
- 150000002894 organic compounds Chemical class 0.000 description 2
- 230000001699 photocatalysis Effects 0.000 description 2
- 238000007146 photocatalysis Methods 0.000 description 2
- 238000004062 sedimentation Methods 0.000 description 2
- 229910000029 sodium carbonate Inorganic materials 0.000 description 2
- 235000017550 sodium carbonate Nutrition 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- 238000001308 synthesis method Methods 0.000 description 2
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 description 2
- WUPHOULIZUERAE-UHFFFAOYSA-N 3-(oxolan-2-yl)propanoic acid Chemical compound OC(=O)CCC1CCCO1 WUPHOULIZUERAE-UHFFFAOYSA-N 0.000 description 1
- 229910010413 TiO 2 Inorganic materials 0.000 description 1
- 239000005083 Zinc sulfide Substances 0.000 description 1
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 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
- 229910052980 cadmium sulfide Inorganic materials 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000007872 degassing Methods 0.000 description 1
- 230000000593 degrading effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- QGLKJKCYBOYXKC-UHFFFAOYSA-N nonaoxidotritungsten Chemical compound O=[W]1(=O)O[W](=O)(=O)O[W](=O)(=O)O1 QGLKJKCYBOYXKC-UHFFFAOYSA-N 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 229910052763 palladium Inorganic materials 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 150000003016 phosphoric acids Chemical class 0.000 description 1
- 239000010970 precious metal Substances 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 238000010223 real-time analysis Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 238000004088 simulation Methods 0.000 description 1
- 239000002594 sorbent Substances 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 229910001930 tungsten oxide Inorganic materials 0.000 description 1
- 238000009941 weaving Methods 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
- 239000011787 zinc oxide Substances 0.000 description 1
- DRDVZXDWVBGGMH-UHFFFAOYSA-N zinc;sulfide Chemical compound [S-2].[Zn+2] DRDVZXDWVBGGMH-UHFFFAOYSA-N 0.000 description 1
Landscapes
- Inorganic Compounds Of Heavy Metals (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The preparation process of nano titania with rutile type concentrated titanium ore with titanium content over 85 % as material includes the mixing with mineralizing agent, roasting, water washing, acidolysis and hydrolysis while adding external crystal seed. The nano titania product has excellent harmful gas adsorbing performance, can adsorb and degrade indoor harmful gas formaldehyde effectively, and may be used as formaldehyde collecting agent, adsorbing carrier for formaldehyde analysis and functional additive for paint, plastic, paper, timber and fabric to adsorbing the free formaldehyde.
Description
Technical field
The preparation method of inolrganic chemicals of the present invention, especially a kind of method for preparing nano titanium oxide.
Background technology
Nano titanium oxide more and more causes people's interest as a kind of novel inorganic functional material, especially You Yi photocatalysis characteristic.Along with the develop rapidly of modern industry, the environmental pollution of outside atmosphere has become the countries in the world problem demanding prompt solution.In addition, because the improving constantly of people's levels of substance, move in the superior of new home finishing and the severe contamination of the indoor harmful gas that brings, also more and more draw attention.Recently domestic and international improvement for environment harmful gas studies show that, nano titanium oxide is as having best photocatalysis performance in zinc oxide, zirconium white, Tungsten oxide 99.999, Cadmium Sulfide, zinc sulphide, manganese oxide, the stannic oxide and chemical stability is good in numerous nano materials, nontoxic, raw material sources are extensive, inexpensive.China is the big country of titanium ore reserves in the world, and more people are at simple, the with low cost nano titanium oxide with suitability for industrialized production value of a kind of technology of positive development research.At present, the employing colloidal sol more to the preparation method of nano titanium oxide-
Gel method, molten salt process, gas phase synthesis method, high pressure water thermal synthesis method etc.These methods are very effective for the nano titanium oxide preparation of different purposes.The starting material majority that it adopts is halogenide, the vitriol of the higher titanium of purity, the organic compound of titanium, so corresponding production cost is just than higher.
Japan's publication (patent No. JP2000325448) has been narrated a kind of formaldehyde remover of being made up of primary ammonium phosphate, gac etc., owing to contain phosphoric acid salt in its composition, so limited the range of application of this sorbent material.Japan's publication (patent No. JP2000321264) has been narrated the method for quantitatively determining of harmful organic compound, is to adopt 1% the palladium activatory TiO 2 sol carrier as catalyzer.Adopted precious metal in this invention, influenced it and used widely.
Summary of the invention
The objective of the invention is to overcome many weak points of prior art, provide a kind of technology simple, with low cost, to the absorption of indoor trace harmful gases formaldehyde and the preparation method of the highly effective nano titanium oxide of degrading.
Content of the present invention is:
It is starting raw material that employing contains the rutile titanium concentrate of titanium dioxide more than 85%, adds the oxyhydroxide of sodium or potassium to this rutile titanium concentrate; The carbonate of sodium or potassium or ammonium, supercarbonate is as molten ore deposit agent, high temperature 700--1300 ℃ of following roasting, adopt the technical hydrochloric acid of 30-36%, at 50--100 ℃ of following acidolysis 1-5 hour, obtain a kind of chlorine oxygen titanium solution, chlorine oxygen titanium solution behind hydrochloric acidolysis is hydrolyzed, and in hydrolytic process, add the nanometer crystal seed, at 60--110 ℃ of following hydrolysis 1-3 hour, thereby obtain nano hydrated titanium dioxide, to this nano hydrated titanium dioxide after filtration, washing, behind the suction filtration,, obtain obnoxious flavour is had the nano titanium oxide of high absorption property high temperature 200--850 ℃ of calcining down.This nano titanium oxide as the carrier sensitivity of the real-time analysis of indoor formaldehyde obnoxious flavour, fast.What also can be used as indoor formaldehyde pounces on the collection agent.
Advantage of the present invention and effect are fairly obvious:
1. adopt the big and inexpensive high-content golden red stone type ilmenite concentrate of domestic reserves, baking mixed with the agent of molten ore deposit, and then use industrial hydrochloric acidolysis, the chlorine oxygen titanium solution that obtains adopts the method hydrolysis that adds the nanometer crystal seed, obtain a kind of nano titanium oxide, technology is very simple, and raw material is cheap, product cost is low, is easy to realize large-scale industrial production.
2. the present invention as absorption carrier, adopts phenol reagent process can detect indoor harmful gas formaldehyde fast on the rapid detection of formaldehyde gas.
3. the present invention is very effective for the adsorption effect of formaldehyde, and especially the remover as formaldehyde can be applied to paint, coating, weaving, papermaking, timber numerous areas.
Embodiment
Embodiment (in 100 kilograms of nano titanium oxide finished products):
Taking by weighing 120 kg contains the ilmenite concentrate of titanium dioxide more than 85% and mixes for 180 kilograms as the yellow soda ash that melts the ore deposit agent, 850 ℃ of following roastings 3 hours, naturally cooling, wash with water to neutrality, filter, under 100 ℃, dry dry powder, dry powder is ground evenly, 500 kilograms of the technical hydrochloric acids of adding 35%, 60 ℃ of following acidolysis 4 hours, sedimentation was filtered, and got 600 kilograms of chlorine oxygen titanium aqueous solution, in the above-mentioned chlorine oxygen titanium aqueous solution, under 60--90 ℃, add and contain titanium dioxide 15 gram/liter nanometer crystal seeds 200 liters, continue to be heated to 110 ℃, its hydrolysis time is 3 hours, obtains the nanometer titanium dioxide titanyl hydrate.Titanium dioxide hydrates through sedimentation, washing, filter, drain, in the calcining down of 550 ℃ of high temperature, obtaining particle diameter is 100 kilograms of 20-50 nano-titanium dioxide powder finished products.
Molten ore deposit agent also can be selected the oxyhydroxide of sodium or potassium or ammonium for use, and potassium or ammonium carbonate, and the supercarbonate of sodium or potassium or ammonium is as molten ore deposit agent, its effect is identical with yellow soda ash, processing method is identical, but the weight ratio difference of adding, the ratio of its interpolation is: the oxyhydroxide of ilmenite concentrate/sodium or potassium=1/0.5-2 weight ratio; Ilmenite concentrate/sodium or potassium or ammonium carbonate, supercarbonate=1/1-3 weight ratio.
Described nanometer crystal seed is the nano titanium oxide crystal seed that commercially available nano titanium oxide prepares through ultrasonic method, and its concentration is for containing titanium dioxide 5-80 gram/liter.
Applying detection example: get nano titanium oxide 0.1 gram for preparing among the embodiment, pack long 50 millimeters into, in the Glass tubing that internal diameter is 2 millimeters, with the harmful formaldehyde gas (concentration of formaldehyde is 0.1 milligram/cubic metre in the case) in the degassing method absorption simulation indoor formaldehyde experimental box, the withdrawing gas volume is 50 milliliters, presses the phenol reagent process principle then, and a phenol reagent solution is splashed in the Glass tubing, add a ferric sulphate ammonium solution then, nano titanium oxide produces bluish voilet immediately in the pipe.Qualitative reaction explanation, nano titanium oxide active adsorption of the present invention air in trace formaldehyde.
Claims (7)
1. the preparation method of a nano titanium oxide is characterized in that: adopt that to contain the rutile titanium concentrate of titanium dioxide 85% or more be raw material, add molten ore deposit agent, through roasting, acidolysis, and add the nanometer crystal seed in hydrolytic process, the acquisition nano titanium oxide.
2. according to the preparation method of the described nano titanium oxide of claim 1, it is characterized in that: the oxyhydroxide that described molten ore deposit agent is sodium or potassium, receive or the carbonate or the supercarbonate of potassium or ammonium, the temperature of institute's roasting is 700--1300 ℃.
3. the preparation method of nano titanium oxide according to claim 1 is characterized in that: what the acidolysis of the intermediates after high-temperature roasting was adopted is the technical hydrochloric acid of 30-36%, at 50--100 ℃ of following acidolysis 1-5 hour, obtains chlorine oxygen titanium solution.
4. according to the preparation method of claim 1 and 3 described nano titanium oxides, it is characterized in that: the chlorine oxygen titanium solution behind hydrochloric acidolysis is hydrolyzed, in hydrolytic process, add the nanometer crystal seed,, thereby obtain nano hydrated titanium dioxide at 60--110 ℃ of following hydrolysis 1-3 hour.
5. the preparation method of nano titanium oxide according to claim 4, it is characterized in that: the nano hydrated titanium dioxide that adds nanometer crystal seed gained, after filtration, after the washing, suction filtration,, obtain obnoxious flavour is had the nano titanium oxide of high absorption property high temperature 200--850 ℃ of calcining down.
6. the preparation method of nano titanium oxide according to claim 2, it is characterized in that: the oxyhydroxide of described molten ore deposit agent sodium or potassium, the carbonate of sodium or potassium or ammonium, the add-on of supercarbonate are respectively: the oxyhydroxide of ilmenite concentrate/sodium or potassium=1/0.5-2 weight ratio; Ilmenite concentrate/sodium or potassium or ammonium carbonate, supercarbonate=1/1-3 weight ratio.
7. the preparation method of nano titanium oxide according to claim 4 is characterized in that: described nanometer crystal seed is the commercially available nano titanium oxide nano titanium oxide crystal seed through the ultrasonic method preparation, and its concentration is for containing titanium dioxide 5-80 gram/liter.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 02159147 CN1285513C (en) | 2002-12-30 | 2002-12-30 | Process for preparing nano titanium dioxide |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 02159147 CN1285513C (en) | 2002-12-30 | 2002-12-30 | Process for preparing nano titanium dioxide |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1511788A true CN1511788A (en) | 2004-07-14 |
| CN1285513C CN1285513C (en) | 2006-11-22 |
Family
ID=34237335
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 02159147 Expired - Fee Related CN1285513C (en) | 2002-12-30 | 2002-12-30 | Process for preparing nano titanium dioxide |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1285513C (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101768384B (en) * | 2008-12-30 | 2012-03-07 | 辽宁石油化工大学 | Nanoscale coating additive for effectively decomposing formaldehyde and application thereof |
| CN107572584A (en) * | 2017-09-29 | 2018-01-12 | 福州琪宁精细化工有限公司 | A kind of preparation method of titanium dioxide |
-
2002
- 2002-12-30 CN CN 02159147 patent/CN1285513C/en not_active Expired - Fee Related
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101768384B (en) * | 2008-12-30 | 2012-03-07 | 辽宁石油化工大学 | Nanoscale coating additive for effectively decomposing formaldehyde and application thereof |
| CN107572584A (en) * | 2017-09-29 | 2018-01-12 | 福州琪宁精细化工有限公司 | A kind of preparation method of titanium dioxide |
| CN107572584B (en) * | 2017-09-29 | 2019-05-10 | 福州琪宁精细化工有限公司 | A kind of preparation method of titanium dioxide |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1285513C (en) | 2006-11-22 |
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