SE543124C2 - Manufacture of a titanium compound structure and a structure - Google Patents
Manufacture of a titanium compound structure and a structureInfo
- Publication number
- SE543124C2 SE543124C2 SE1950193A SE1950193A SE543124C2 SE 543124 C2 SE543124 C2 SE 543124C2 SE 1950193 A SE1950193 A SE 1950193A SE 1950193 A SE1950193 A SE 1950193A SE 543124 C2 SE543124 C2 SE 543124C2
- Authority
- SE
- Sweden
- Prior art keywords
- tio2
- titanium dioxide
- dispersion
- range
- sol
- Prior art date
Links
- 238000004519 manufacturing process Methods 0.000 title claims abstract 3
- 150000003609 titanium compounds Chemical group 0.000 title claims abstract 3
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract 46
- 238000000034 method Methods 0.000 claims abstract 22
- 239000004408 titanium dioxide Substances 0.000 claims abstract 11
- 239000003381 stabilizer Substances 0.000 claims abstract 8
- 239000002245 particle Substances 0.000 claims abstract 7
- 239000013067 intermediate product Substances 0.000 claims abstract 6
- 238000001556 precipitation Methods 0.000 claims abstract 3
- 238000003756 stirring Methods 0.000 claims abstract 3
- LLZRNZOLAXHGLL-UHFFFAOYSA-J titanic acid Chemical compound O[Ti](O)(O)O LLZRNZOLAXHGLL-UHFFFAOYSA-J 0.000 claims abstract 3
- 150000008044 alkali metal hydroxides Chemical class 0.000 claims abstract 2
- 229910001413 alkali metal ion Inorganic materials 0.000 claims abstract 2
- 239000006185 dispersion Substances 0.000 claims 9
- 230000002378 acidificating effect Effects 0.000 claims 7
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims 6
- -1 hydroxide ions Chemical class 0.000 claims 5
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical class [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims 4
- 150000001735 carboxylic acids Chemical class 0.000 claims 4
- 229910052783 alkali metal Inorganic materials 0.000 claims 3
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims 3
- 239000000243 solution Substances 0.000 claims 3
- 229910010270 TiOCl2 Inorganic materials 0.000 claims 2
- 238000004090 dissolution Methods 0.000 claims 2
- 150000001261 hydroxy acids Chemical class 0.000 claims 2
- JVTAAEKCZFNVCJ-UHFFFAOYSA-N lactic acid Chemical compound CC(O)C(O)=O JVTAAEKCZFNVCJ-UHFFFAOYSA-N 0.000 claims 2
- 229910052719 titanium Inorganic materials 0.000 claims 2
- 239000010936 titanium Substances 0.000 claims 2
- FKNQFGJONOIPTF-UHFFFAOYSA-N Sodium cation Chemical compound [Na+] FKNQFGJONOIPTF-UHFFFAOYSA-N 0.000 claims 1
- 229910010269 TiOb Inorganic materials 0.000 claims 1
- 229910003087 TiOx Inorganic materials 0.000 claims 1
- 229940061720 alpha hydroxy acid Drugs 0.000 claims 1
- 150000001280 alpha hydroxy acids Chemical class 0.000 claims 1
- 239000007864 aqueous solution Substances 0.000 claims 1
- 210000000988 bone and bone Anatomy 0.000 claims 1
- 230000003247 decreasing effect Effects 0.000 claims 1
- 238000001035 drying Methods 0.000 claims 1
- 239000007943 implant Substances 0.000 claims 1
- 150000002500 ions Chemical class 0.000 claims 1
- 239000004310 lactic acid Substances 0.000 claims 1
- 235000014655 lactic acid Nutrition 0.000 claims 1
- 239000007788 liquid Substances 0.000 claims 1
- 229910001416 lithium ion Inorganic materials 0.000 claims 1
- 230000004048 modification Effects 0.000 claims 1
- 238000012986 modification Methods 0.000 claims 1
- 238000006386 neutralization reaction Methods 0.000 claims 1
- 230000001699 photocatalysis Effects 0.000 claims 1
- 229910001415 sodium ion Inorganic materials 0.000 claims 1
- HLLICFJUWSZHRJ-UHFFFAOYSA-N tioxidazole Chemical compound CCCOC1=CC=C2N=C(NC(=O)OC)SC2=C1 HLLICFJUWSZHRJ-UHFFFAOYSA-N 0.000 claims 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims 1
- 229910001428 transition metal ion Inorganic materials 0.000 claims 1
- 239000002253 acid Substances 0.000 abstract 1
- 238000010438 heat treatment Methods 0.000 abstract 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G23/00—Compounds of titanium
- C01G23/003—Titanates
- C01G23/005—Alkali titanates
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61F—FILTERS IMPLANTABLE INTO BLOOD VESSELS; PROSTHESES; DEVICES PROVIDING PATENCY TO, OR PREVENTING COLLAPSING OF, TUBULAR STRUCTURES OF THE BODY, e.g. STENTS; ORTHOPAEDIC, NURSING OR CONTRACEPTIVE DEVICES; FOMENTATION; TREATMENT OR PROTECTION OF EYES OR EARS; BANDAGES, DRESSINGS OR ABSORBENT PADS; FIRST-AID KITS
- A61F2/00—Filters implantable into blood vessels; Prostheses, i.e. artificial substitutes or replacements for parts of the body; Appliances for connecting them with the body; Devices providing patency to, or preventing collapsing of, tubular structures of the body, e.g. stents
- A61F2/02—Prostheses implantable into the body
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
- B01J21/06—Silicon, titanium, zirconium or hafnium; Oxides or hydroxides thereof
- B01J21/063—Titanium; Oxides or hydroxides thereof
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/485—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of mixed oxides or hydroxides for inserting or intercalating light metals, e.g. LiTi2O4 or LiTi2OxFy
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Inorganic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Life Sciences & Earth Sciences (AREA)
- Environmental & Geological Engineering (AREA)
- Biomedical Technology (AREA)
- General Life Sciences & Earth Sciences (AREA)
- General Chemical & Material Sciences (AREA)
- Materials Engineering (AREA)
- Electrochemistry (AREA)
- Cardiology (AREA)
- Oral & Maxillofacial Surgery (AREA)
- Transplantation (AREA)
- Geology (AREA)
- Heart & Thoracic Surgery (AREA)
- Vascular Medicine (AREA)
- Animal Behavior & Ethology (AREA)
- General Health & Medical Sciences (AREA)
- Public Health (AREA)
- Veterinary Medicine (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The present invention relates to a method for manufacturing a structure of a titanium compound selected from the group consisting of sheets, wires and tubes. Titanic acid is dissolved in an acid below pH 1, TiO2 particles are formed by addition of a stabilizer and precipitation by heating to 68-85°C and stirring, an alkali metal hydroxide is added followed by treatment at 90-170°C during 6-72 hours, then the alkali metal ions are exchanged with protons. The present invention also relates to intermediate products and structures comprising titanium dioxide obtainable by the method. The invention provides an improved method giving improved yield as well as other advantages.
Description
69
Claims (24)
1. l. A method for manufacturing a structure of a titanium compound selected from the group consisting of sheets, method wires and tubes, characterized in that the compríses the steps of: a)providing at least one titanic acid with the general formula [TiOX(OH)44X]n and dissolving it in anaqueous solution comprising at least one compoundselected from the group consisting of TiOCl2, TiCl@and HCl so that a clear solution is obtained,wherein the pH of the clear solution is lower than l after dissolution, increasing the temperature of the clear solutionuntil reaching a temperature in the interval 68-85°C where precipitation starts to occur, adding atleast one acidic stabilizer before the precipitationstarts to occur, and holding that temperature duringat least l minute during stirring to obtain adispersion of particles comprising TiO2 as an intermediate product, adjusting the concentration of hydroxide ions in thedispersion from step b) to at least 8 M by adding an alkali metal hydroxide MOH, treating the dispersion from step c) at atemperature in the interval 90-170 °C during 6-72hours to obtain a plurality of first structures comprising alkali metal titanate, treating the plurality of first structurescomprising alkali metal titanate to exchange at least a part of the alkali metal ions M* with H* to obtain a plurality of second structures comprising protonated titanate.
2. The method according to claim l, furthercomprising, after step b) and before step c), thesteps of:bl) decreasing the content of ions in thedispersion preferably such that the ionconcentration is lowered to a point where a sol isformed, wherein the average diameter of theparticles in the sol is 3-20 nm, preferably 4-l5nm, more preferably, 4.5-7 nm; andb2) adjusting the concentration of TiO2 in thedispersion preferably to a value within the rangeof l0-80%, more preferably to a value within therange 20-70%, most preferably to a value within the range 30-50%.
3. The method according to l or 2, wherein thedispersion after step b) or the sol after steps bl)and b2) comprises at least l5 wt% titanium dioxide,preferably at least l7 wt% titanium dioxide, morepreferably at least 25 wt% titanium dioxide, even morepreferably at least 30 wt% titanium dioxide, and evenmore preferably at least 40 wt% titanium dioxide, and most preferably at least 50 wt% titanium dioxide.
4. The method according to any one of claims l-3,wherein the plurality of second structures comprisingprotonated titanate obtained after step e) are heatedto a temperature in the range 300 - 700 °C, preferably300 - 600 °C, more preferably 300 - 450 °C, mostpreferably 300 - 400 °C to obtain a plurality of third structures comprising titanium dioxide.
5. The method according to any one of claims 1-4,wherein the at least one acidic stabilizer is selected from a carboxylic acid, and an alpha hydroxy acid.
6. The method according to any one of claims 1-5, wherein at least one alkanolamine and the at least one acidic stabilizer are added together before step c).
7. The method according to any one of claims 5-6,wherein the carboxylic acid is selected from the group consisting of citric acid, and lactic acid.
8. The method according to any one of claims 1-7, wherein stirring is performed during step d).
9. The method according to any one of claims 1-8,wherein the dispersion has remained in a dispersedstate without drying and subsequent redispersion between steps b) and c).
10. The method according to any one of claims 1-8,wherein the dispersion is dried and redispersed between steps b) and c).
11. The method according to any one of claims 1-8and 10, wherein the specific surface area, as measuredaccording to ISO 9277 of the particles dried from the dispersion obtained after step b), is in the range 200-300 m?/g.
12. The method according to any one of claims 1-11, wherein the pH after dissolution in step a) is lower than 0.
13. l3. The method according to any one of claims l-l2, wherein the pH of the dispersion resulting fromstep b) or the sol resulting from steps bl) and b2) is adjusted to a value in the range 0.5-l.5.
14. l4. The method according to any one of claims l-l3, wherein the concentration of hydroxide ions is adjusted in step c) using NaOH.
15. l5. The method according to any one of claims l-l4, wherein the titanic acid provided in step a) ismade from a TiOCl2 by neutralisation until precipitation by an aqueous solution of NaOH.
16. l6. The method according to any one of claims l-l5, wherein the plurality of first structurescomprising alkali metal titanate are separated from the remaining liquid between steps d) and e).
17. l7. The method according to any one of claims l-l6, wherein the treatment of the dispersion in step d) is performed at autogenous pressure.
18. l8. The method according to any one of claims l-l7, wherein no transition metal ions except titanium are added.
19. l9. An intermediate product characterized in that it is obtained after step b) in any one of claims l-l8, being a dispersion of particles comprising TiO2and comprising at least one acidic stabilizer andwherein the intermediate product optionally exhibitsone or more of the following features: - the dispersion comprises at least l5 wt% TiO@ preferably at least l7 wt% TiO2, more preferably at least 25 wt% TiO2, even more preferably at
20. it is obtained after steps bl) claims 2-l8, least 30 wt% TiO2, even more preferably at least 40 wt% TiO2, and most preferably at least 50 wt% titanium dioxide; the at least one acidic stabilizer is at leastone selected from a carboxylic acid, and analpha hydroxy acid; the pH is in the range 0.5 - 9; the specific surface area measured according toISO 9277 of the particles dried from the dispersion is in the range 200-300 m?/g. An intermediate product characterized in that and b2) of any one of being a sol of particles comprising TiO2 and comprising at least one acidic stabilizer and wherein the intermediate product optionally exhibits one or more of the following features:
21. 2l. structure being one of a sheet, the sol comprises at least l5 wt% TiOb preferably at least l7 wt% TiO2, more preferably at least 25 wt% TiO2, even more preferably atleast 30 wt% TiO2, even more preferably at least 40 wt% TiO2, and most preferably at least 50 wt% titanium dioxide;the at least one acidic stabilizer is at leastone selected from a carboxylic acid, and analpha hydroxy acid; the pH is in the range 0.5 - 9; the specific surface area measured according toISO 9277 of the particles dried from the sol isin the range 200-300 m?/g. A structure comprising titanium dioxide, said a wire, and a tube, characterized in that said structure being made according to claim 4.
22. The structure according to claim 21, whereinthe structure constitutes a part of a Li ion or sodium ion battery anode.
23. The structure according to claim 21, whereinthe structure constitutes a part of a photocatalytic object.
24. The structure according to claim 21, whereinthe structure constitutes a surface modification or treatment of a titanium dental or bone implant.
Priority Applications (11)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| SE1950193A SE543124C2 (en) | 2019-02-15 | 2019-02-15 | Manufacture of a titanium compound structure and a structure |
| JP2021547337A JP7520858B2 (en) | 2019-02-15 | 2020-02-14 | Preparation of titanium dioxide structures |
| US17/429,829 US20220119272A1 (en) | 2019-02-15 | 2020-02-14 | Manufacture of titanium dioxide structures |
| EP20705359.6A EP3924301B1 (en) | 2019-02-15 | 2020-02-14 | Manufacture of titanium dioxide structures |
| CA3130020A CA3130020A1 (en) | 2019-02-15 | 2020-02-14 | Manufacture of titanium dioxide structures |
| PCT/EP2020/053922 WO2020165419A1 (en) | 2019-02-15 | 2020-02-14 | Manufacture of titanium dioxide structures |
| IL285576A IL285576B2 (en) | 2019-02-15 | 2020-02-14 | Manufacture of titanium dioxide structures |
| CN202080014410.5A CN113490642B (en) | 2019-02-15 | 2020-02-14 | Fabrication of titanium dioxide structures |
| KR1020217027727A KR102865962B1 (en) | 2019-02-15 | 2020-02-14 | Method for manufacturing titanium dioxide structure |
| AU2020223518A AU2020223518B2 (en) | 2019-02-15 | 2020-02-14 | Manufacture of titanium dioxide structures |
| BR112021015883-9A BR112021015883A2 (en) | 2019-02-15 | 2020-02-14 | MANUFACTURE OF TITANIUM DIOXIDE STRUCTURES |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| SE1950193A SE543124C2 (en) | 2019-02-15 | 2019-02-15 | Manufacture of a titanium compound structure and a structure |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| SE1950193A1 SE1950193A1 (en) | 2020-08-16 |
| SE543124C2 true SE543124C2 (en) | 2020-10-13 |
Family
ID=72425098
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| SE1950193A SE543124C2 (en) | 2019-02-15 | 2019-02-15 | Manufacture of a titanium compound structure and a structure |
Country Status (1)
| Country | Link |
|---|---|
| SE (1) | SE543124C2 (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| SE544707C2 (en) * | 2020-08-14 | 2022-10-18 | Tiotech As | Manufacture of a titanium dioxide bronze material |
| CN115444980A (en) * | 2021-06-08 | 2022-12-09 | 中国科学院上海硅酸盐研究所 | Metal ion doped titanium dioxide nano coating, preparation method and application thereof in nerve and bone tissue repair |
-
2019
- 2019-02-15 SE SE1950193A patent/SE543124C2/en unknown
Also Published As
| Publication number | Publication date |
|---|---|
| SE1950193A1 (en) | 2020-08-16 |
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