CN113998731A - A kind of production method of titanyl sulfate and nano titanium dioxide - Google Patents
A kind of production method of titanyl sulfate and nano titanium dioxide Download PDFInfo
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- CN113998731A CN113998731A CN202111424728.3A CN202111424728A CN113998731A CN 113998731 A CN113998731 A CN 113998731A CN 202111424728 A CN202111424728 A CN 202111424728A CN 113998731 A CN113998731 A CN 113998731A
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- titanium dioxide
- titanyl sulfate
- sulfuric acid
- titanium
- feed liquid
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- 229910000349 titanium oxysulfate Inorganic materials 0.000 title claims abstract description 46
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 21
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 title claims abstract description 20
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 83
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 63
- 239000013078 crystal Substances 0.000 claims abstract description 38
- 239000004408 titanium dioxide Substances 0.000 claims abstract description 36
- 238000002425 crystallisation Methods 0.000 claims abstract description 30
- 230000008025 crystallization Effects 0.000 claims abstract description 30
- 239000007788 liquid Substances 0.000 claims abstract description 22
- 238000000034 method Methods 0.000 claims abstract description 19
- 239000002253 acid Substances 0.000 claims abstract description 15
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 12
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 12
- 239000010936 titanium Substances 0.000 claims abstract description 12
- 238000001354 calcination Methods 0.000 claims abstract description 10
- YDZQQRWRVYGNER-UHFFFAOYSA-N iron;titanium;trihydrate Chemical compound O.O.O.[Ti].[Fe] YDZQQRWRVYGNER-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000012452 mother liquor Substances 0.000 claims abstract description 8
- 238000002386 leaching Methods 0.000 claims abstract description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 13
- 239000000463 material Substances 0.000 claims description 9
- 238000001816 cooling Methods 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 3
- 238000009413 insulation Methods 0.000 claims 1
- 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 1
- 238000011282 treatment Methods 0.000 abstract description 9
- 239000002994 raw material Substances 0.000 abstract description 4
- 238000005516 engineering process Methods 0.000 abstract description 2
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 8
- 238000004321 preservation Methods 0.000 description 5
- 230000008569 process Effects 0.000 description 5
- 238000000576 coating method Methods 0.000 description 4
- 239000011248 coating agent Substances 0.000 description 3
- 238000000227 grinding Methods 0.000 description 3
- 239000002699 waste material Substances 0.000 description 3
- RAHZWNYVWXNFOC-UHFFFAOYSA-N Sulphur dioxide Chemical compound O=S=O RAHZWNYVWXNFOC-UHFFFAOYSA-N 0.000 description 2
- 238000001704 evaporation Methods 0.000 description 2
- 230000008020 evaporation Effects 0.000 description 2
- 239000004744 fabric Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- AKEJUJNQAAGONA-UHFFFAOYSA-N sulfur trioxide Chemical compound O=S(=O)=O AKEJUJNQAAGONA-UHFFFAOYSA-N 0.000 description 2
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 2
- 239000002351 wastewater Substances 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
- 229910010298 TiOSO4 Inorganic materials 0.000 description 1
- 230000006750 UV protection Effects 0.000 description 1
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 1
- 239000004202 carbamide Substances 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 239000002808 molecular sieve Substances 0.000 description 1
- KADRTWZQWGIUGO-UHFFFAOYSA-L oxotitanium(2+);sulfate Chemical compound [Ti+2]=O.[O-]S([O-])(=O)=O KADRTWZQWGIUGO-UHFFFAOYSA-L 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000012716 precipitator Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000004224 protection Effects 0.000 description 1
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000003643 water by type Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G23/00—Compounds of titanium
- C01G23/008—Titanium- and titanyl sulfate
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G23/00—Compounds of titanium
- C01G23/04—Oxides; Hydroxides
- C01G23/047—Titanium dioxide
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G23/00—Compounds of titanium
- C01G23/04—Oxides; Hydroxides
- C01G23/047—Titanium dioxide
- C01G23/08—Drying; Calcining ; After treatment of titanium oxide
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/30—Three-dimensional structures
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Nanotechnology (AREA)
- Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Environmental & Geological Engineering (AREA)
- Inorganic Chemistry (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Crystallography & Structural Chemistry (AREA)
- Physics & Mathematics (AREA)
- Composite Materials (AREA)
- Materials Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention provides a method for producing titanyl sulfate and nano titanium dioxide, which takes ilmenite, metatitanic acid or other sulfuric acid leaching solutions containing titanium as raw materials, adds a certain amount of concentrated sulfuric acid into feed liquid, heats the feed liquid to ensure that titanium is supersaturated to separate out titanyl sulfate crystals, and separates out crystallization mother liquor to obtain commercial titanyl sulfate; and calcining titanyl sulfate to obtain anatase or rutile type nano titanium dioxide products, and carrying out post-treatment to obtain the commercial nano titanium dioxide. The technology can completely utilize equipment of the traditional sulfuric acid method titanium dioxide production process, does not need additional equipment investment, and has the advantages of better product quality, higher crystallization speed, wide application range of feed liquid and the like compared with the existing sulfuric acid method titanium dioxide production process.
Description
Technical Field
The invention belongs to the field of metallurgy and chemical industry, and particularly relates to a method for producing titanyl sulfate and nano titanium dioxide.
Background
Titanyl sulfate is a white loose white powder with a long-strip microstructure, usually containing two crystal waters, and has the molecular formula: TiOSO4·2H2And O. The titanyl sulfate has wide application, can be used as a mordant, a reducing agent, a water treatment agent and the like of fiber fabrics, and can be dissolved and added with a precipitator such as urea to ensure that precipitated nano titanium dioxide and the like are attached to fabrics, active carbon and molecular sieves, so that the carrier has the capabilities of ultraviolet resistance, high catalytic activity and the like. Titanyl sulfate can be decomposed to obtain titanium dioxide and sulfur dioxide/sulfur trioxide by direct calcination.
Titanium dioxide is a white powder of the formula: TiO 22It is the main component of titanium dioxide. Titanium dioxide is widely applied to the fields of chemical industry, coatings and the like, more than 90% of titanium dioxide in China is produced by using a sulfuric acid method at present, the titanium dioxide in the traditional sulfuric acid method is obtained by crystallizing metatitanic acid after evaporation and concentration of sulfuric acid leaching solution of ilmenite and the like, then calcining the metatitanic acid to obtain titanium dioxide, and performing post-treatment procedures of grinding, coating and the like to obtain the titanium dioxide.
Disclosure of Invention
The invention mainly aims to provide a method for producing titanyl sulfate and nano titanium dioxide, and aims to solve the technical problems of long crystallization time, high requirement on titanium concentration of raw material liquid and low product quality in the existing technology for producing titanium dioxide by a sulfuric acid method.
In order to achieve the purpose, the technical scheme of the invention is as follows: the method for preparing titanium dioxide by crystallizing and calcining metatitanic acid in the traditional sulfate process titanium dioxide process is changed, titanyl sulfate is prepared from raw material liquid, and nano titanium dioxide is prepared by calcining. The invention provides a production method of titanyl sulfate and nano titanium dioxide, which comprises the following steps:
(1) Adding sulfuric acid into sulfuric acid leaching solution of ilmenite or other titanium-containing material such as metatitanic acid to make the sulfuric acid concentration of feed liquid be 5-8 mol/L and the titanium concentration of feed liquid be TiO2Meter) is 100g/L and above;
(2) heating the feed liquid to 80-130 ℃, adding pure and uniform titanyl sulfate seed crystals, wherein the addition amount of the seed crystals is 0.1-5% of the mass of titanium dioxide contained in the feed liquid, and carrying out heat preservation crystallization for 1-2.5 h; and cooling to room temperature after crystallization is finished, and separating out crystallization mother liquor to obtain titanyl sulfate crystals. Removing free water from the obtained crystal, and drying at 50-120 ℃;
(3) the dried crystal can be sold as commercial titanyl sulfate, or calcined at 650-1000 ℃ for 2.5-5 h to decompose titanyl sulfate to obtain anatase type or rutile type titanium dioxide, and the nano titanium dioxide is obtained after subsequent grinding, coating and other treatments. The chemical reaction equation for the calcination process is as follows:
the preparation method of the titanyl sulfate and the nano titanium dioxide has the innovation points that:
the new process does not change the main production equipment for preparing the titanium dioxide by the traditional sulfuric acid method, and has the following advantages compared with the traditional sulfuric acid method:
(1) the raw materials have wider adaptability. TiO can be prepared by the traditional crystallization process2The concentration is reduced to about 220g/L to about 100g/L, the evaporation and concentration process is reduced, and the adaptability to low-grade ores is stronger.
(2) The production efficiency is higher. The same crystallization rate is achieved, the traditional metatitanic acid crystallization needs more than 5 hours, and the new method only needs 1-2.5 hours.
(3) The discharge amount of the waste water is lower. The waste acid concentration of the crystallized residual liquid is very high, and the waste acid can be returned to be used for acidolysis and leaching of titanium ore, so that the treatment cost of waste water and waste acid is reduced.
(4) The product quality is better: the nanometer titanium dioxide with finer granularity can be obtained, the titanium dioxide particles of the traditional sulfuric acid method titanium dioxide are more than 250 nanometers, and the granularity of the titanium dioxide prepared by the method of the invention is 30-50 nanometers.
(5) The product is more diversified: the crystallized titanyl sulfate can be sold as a product, and can produce high-quality titanium dioxide after calcination.
Detailed Description
The present invention will be further illustrated by the following examples, but is not limited thereto.
Example 1
The production method of titanyl sulfate and nano titanium dioxide comprises the following steps:
(1) sulfuric acid is added to sulfuric acid leach liquor of ilmenite or other titaniferous material such as metatitanic acid so that the sulfuric acid concentration of the feed liquor is 8mol/L and the titanium dioxide concentration of the feed liquor is 100 g/L.
(2) Heating the feed liquid to 120 ℃, adding pure and uniform titanyl sulfate seed crystals, wherein the addition amount of the seed crystals is 5 percent of the mass of titanium dioxide contained in the feed liquid, and carrying out heat preservation and crystallization for 150 min.
(3) And cooling to room temperature after crystallization is finished, and separating out crystallization mother liquor to obtain titanyl sulfate crystals, wherein the crystallization rate is over 90 percent.
(4) The obtained crystals are washed by ethanol/methanol with anhydrous or low water content to remove the crystal entrained free water and dried at 80 ℃, otherwise, the product is dissolved in the entrained trace water to form viscous semi-solid titanyl sulfate during calcination, and the calcined product has poor quality.
(5) The dried crystal can be sold as a commodity of titanyl sulfate, or calcined for 5 hours at 700 ℃ to obtain anatase titanium dioxide with the granularity of 30-40 nanometers, and the nano titanium dioxide is obtained through subsequent grinding, coating and other treatments.
Example 2
The production method of titanyl sulfate and nano titanium dioxide comprises the following steps:
(1) sulfuric acid is added to sulfuric acid leach liquor of ilmenite or other titaniferous material such as metatitanic acid so that the sulfuric acid concentration of the feed liquor is 7mol/L and the titanium dioxide concentration of the feed liquor is 140 g/L.
(2) Heating the feed liquid to 100 ℃, adding pure and uniform titanyl sulfate seed crystals, wherein the addition amount of the seed crystals is 2% of the mass of titanium dioxide contained in the feed liquid, and carrying out heat preservation and crystallization for 120 min.
(3) And cooling to room temperature after crystallization is finished, and separating out crystallization mother liquor to obtain titanyl sulfate crystals, wherein the crystallization rate reaches 93%.
(4) The obtained crystals are washed by ethanol/methanol with anhydrous or low water content to remove the free water carried by the crystals and dried at 80 ℃.
(5) The dried crystal can be sold as a commodity of titanyl sulfate, or calcined for 4 hours at 750 ℃ to obtain 30-40 nm anatase titanium dioxide, and the titanium dioxide is obtained after treatment.
Example 3
The production method of titanyl sulfate and nano titanium dioxide comprises the following steps:
(1) sulfuric acid is added to sulfuric acid leach liquor of ilmenite or other titaniferous material such as metatitanic acid so that the sulfuric acid concentration of the feed liquor is 6mol/L and the titanium dioxide concentration of the feed liquor is 180 g/L.
(2) Heating the feed liquid to 100 ℃, adding pure and uniform titanyl sulfate seed crystals, wherein the addition amount of the seed crystals is 1 percent of the mass of titanium dioxide contained in the feed liquid, and carrying out heat preservation and crystallization for 90 min.
(3) And cooling to room temperature after crystallization is finished, and separating out crystallization mother liquor to obtain titanyl sulfate crystals with the crystallization rate of 93.5%.
(4) The obtained crystals are washed by ethanol/methanol with anhydrous or low water content to remove the free water carried by the crystals and dried at 100 ℃.
(5) The dried crystal can be sold as commercial titanyl sulfate, or calcined for 3h at 850 ℃ to obtain 30-50 nanometer rutile type titanium dioxide, and the titanium dioxide is obtained after treatment.
Example 4
The production method of titanyl sulfate and nano titanium dioxide comprises the following steps:
(1) sulfuric acid is added to sulfuric acid leach liquor of ilmenite or other titaniferous material such as metatitanic acid so that the sulfuric acid concentration of the feed liquor is 5mol/L and the titanium dioxide concentration of the feed liquor is 220 g/L.
(2) Heating the feed liquid to 90 ℃, adding pure and uniform titanyl sulfate seed crystals, wherein the addition amount of the seed crystals is 0.1 percent of the mass of titanium dioxide contained in the feed liquid, and carrying out heat preservation and crystallization for 60 min.
(3) And cooling to room temperature after crystallization is finished, and separating out crystallization mother liquor to obtain titanyl sulfate crystals, wherein the crystallization rate is 90%.
(4) The obtained crystals are washed by ethanol/methanol with anhydrous or low water content to remove the free water carried by the crystals and dried at 100 ℃.
(5) The dried crystal can be sold as commercial titanyl sulfate, or calcined at 900 ℃ for 2.5h to obtain 40-50 nano rutile type titanium dioxide, and the titanium dioxide is obtained after treatment.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that those skilled in the art can make various improvements and modifications without departing from the principle of the present invention, and these improvements and modifications should also be construed as the protection scope of the present invention.
Claims (7)
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|---|---|---|---|
| CN202111424728.3A CN113998731A (en) | 2021-11-26 | 2021-11-26 | A kind of production method of titanyl sulfate and nano titanium dioxide |
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| CN202111424728.3A CN113998731A (en) | 2021-11-26 | 2021-11-26 | A kind of production method of titanyl sulfate and nano titanium dioxide |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114573021A (en) * | 2022-03-14 | 2022-06-03 | 淮安市鸿洋钛业有限公司 | High-purity mixed crystal titanium dioxide and production method thereof |
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2021
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