CN115893484B - Preparation method of rod-shaped rutile titanium dioxide - Google Patents
Preparation method of rod-shaped rutile titanium dioxide Download PDFInfo
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- CN115893484B CN115893484B CN202211726700.XA CN202211726700A CN115893484B CN 115893484 B CN115893484 B CN 115893484B CN 202211726700 A CN202211726700 A CN 202211726700A CN 115893484 B CN115893484 B CN 115893484B
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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims abstract description 96
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- NJLLQSBAHIKGKF-UHFFFAOYSA-N dipotassium dioxido(oxo)titanium Chemical compound [K+].[K+].[O-][Ti]([O-])=O NJLLQSBAHIKGKF-UHFFFAOYSA-N 0.000 claims abstract description 34
- 239000004408 titanium dioxide Substances 0.000 claims abstract description 25
- XJDNKRIXUMDJCW-UHFFFAOYSA-J titanium tetrachloride Chemical compound Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 0.000 claims abstract description 14
- 238000005342 ion exchange Methods 0.000 claims abstract description 13
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000011591 potassium Substances 0.000 claims abstract description 12
- 229910052700 potassium Inorganic materials 0.000 claims abstract description 12
- 239000013078 crystal Substances 0.000 claims abstract description 7
- 230000004927 fusion Effects 0.000 claims abstract description 4
- 230000009466 transformation Effects 0.000 claims abstract description 4
- 238000010438 heat treatment Methods 0.000 claims description 32
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 24
- 239000008367 deionised water Substances 0.000 claims description 24
- 229910021641 deionized water Inorganic materials 0.000 claims description 24
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 24
- 239000012065 filter cake Substances 0.000 claims description 22
- 239000011268 mixed slurry Substances 0.000 claims description 20
- 239000007787 solid Substances 0.000 claims description 20
- 150000001875 compounds Chemical class 0.000 claims description 16
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 claims description 14
- 238000001914 filtration Methods 0.000 claims description 12
- 239000002243 precursor Substances 0.000 claims description 12
- 238000004321 preservation Methods 0.000 claims description 12
- 238000005406 washing Methods 0.000 claims description 12
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 11
- 238000000034 method Methods 0.000 claims description 11
- 229910052719 titanium Inorganic materials 0.000 claims description 11
- 239000010936 titanium Substances 0.000 claims description 11
- 239000000706 filtrate Substances 0.000 claims description 9
- 238000002156 mixing Methods 0.000 claims description 9
- 239000000203 mixture Substances 0.000 claims description 8
- 238000001035 drying Methods 0.000 claims description 7
- 229910000027 potassium carbonate Inorganic materials 0.000 claims description 7
- 235000011181 potassium carbonates Nutrition 0.000 claims description 7
- 238000003746 solid phase reaction Methods 0.000 claims description 7
- 238000003756 stirring Methods 0.000 claims description 7
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 claims description 4
- 229910010413 TiO 2 Inorganic materials 0.000 claims description 4
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 claims description 4
- KYNKUCOQLYEJPH-UHFFFAOYSA-N [K][Ti] Chemical compound [K][Ti] KYNKUCOQLYEJPH-UHFFFAOYSA-N 0.000 claims description 2
- 239000002253 acid Substances 0.000 claims description 2
- 235000015497 potassium bicarbonate Nutrition 0.000 claims description 2
- 239000011736 potassium bicarbonate Substances 0.000 claims description 2
- 229910000028 potassium bicarbonate Inorganic materials 0.000 claims description 2
- VKJKEPKFPUWCAS-UHFFFAOYSA-M potassium chlorate Chemical compound [K+].[O-]Cl(=O)=O VKJKEPKFPUWCAS-UHFFFAOYSA-M 0.000 claims description 2
- 239000001103 potassium chloride Substances 0.000 claims description 2
- 235000011164 potassium chloride Nutrition 0.000 claims description 2
- TYJJADVDDVDEDZ-UHFFFAOYSA-M potassium hydrogencarbonate Chemical compound [K+].OC([O-])=O TYJJADVDDVDEDZ-UHFFFAOYSA-M 0.000 claims description 2
- 239000004323 potassium nitrate Substances 0.000 claims description 2
- 235000010333 potassium nitrate Nutrition 0.000 claims description 2
- 229960003975 potassium Drugs 0.000 claims 5
- 229940086066 potassium hydrogencarbonate Drugs 0.000 claims 1
- 230000004913 activation Effects 0.000 abstract description 2
- 238000002425 crystallisation Methods 0.000 abstract description 2
- 230000008025 crystallization Effects 0.000 abstract description 2
- 239000008204 material by function Substances 0.000 abstract description 2
- 238000010899 nucleation Methods 0.000 abstract description 2
- 230000006911 nucleation Effects 0.000 abstract description 2
- 238000006243 chemical reaction Methods 0.000 description 11
- 239000000835 fiber Substances 0.000 description 5
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 description 5
- 239000000047 product Substances 0.000 description 5
- 238000001027 hydrothermal synthesis Methods 0.000 description 4
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 3
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 239000004372 Polyvinyl alcohol Substances 0.000 description 1
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- YHWCPXVTRSHPNY-UHFFFAOYSA-N butan-1-olate;titanium(4+) Chemical compound [Ti+4].CCCC[O-].CCCC[O-].CCCC[O-].CCCC[O-] YHWCPXVTRSHPNY-UHFFFAOYSA-N 0.000 description 1
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 229920002451 polyvinyl alcohol Polymers 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
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- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention discloses a preparation method of rod-shaped rutile titanium dioxide, belonging to the field of inorganic nonmetallic novel functional materials. The invention firstly carries out depolymerization and ion exchange potassium removal activation treatment on potassium titanate, then takes the potassium titanate as a rod-shaped structural template, carries out ion exchange, nucleation, crystallization and lattice reconstruction on titanium tetrachloride solution, and finally prepares the rod-shaped rutile type titanium dioxide through high-temperature crystal transformation and fusion.
Description
Technical Field
The invention belongs to the field of inorganic nonmetallic novel functional materials, and particularly relates to a preparation method of rod-shaped rutile titanium dioxide.
Background
The rod-shaped titanium dioxide has the characteristics of excellent mechanical property, high whiteness, stable performance and the like, and is applied to a plurality of high-end fields. The double-crystal phase rod-shaped titanium dioxide is prepared by twice hydrothermal reactions in the Chinese patent 202010747696.X, the diameter is 20-50 nm, and the length is 400-1000 nm. The patent has harsh reaction conditions and complex process. The method comprises the steps of adding a potassium hydroxide solution into a tetrabutyl titanate solution, mixing, and performing hydrothermal reaction to obtain potassium titanate fibers in Chinese patent ZL 201710534115.2; then dispersing potassium titanate fiber in 1-1.5M nitric acid solution, adding polyvinyl alcohol solution, mixing, and performing hydrothermal reaction to obtain mixed crystal titania fiber composed of anatase type and rutile type, wherein a large amount of gaps exist in the fiber structure, and the strength of the mixed crystal titania fiber is seriously affected. The Chinese patent ZL 201610299669.4 prepares the mixture of organic titanium and glycerol or glycol into solution, and reacts under hydrothermal condition to obtain anatase type rod-shaped titanium dioxide with average length of 0.5-50 μm. The Chinese patent ZL 96117084.0 proposes a method for hydrothermally synthesizing titanium dioxide whisker, the whisker length of the rutile structure is 15-30 mu m, the diameter is 1-3 mu m, and the length-diameter ratio is more than 10. Although the rod-shaped rutile titanium dioxide is successfully synthesized by the method, the preparation process needs to carry out high-temperature high-pressure hydrothermal reaction in a closed reaction kettle, and the method has potential danger.
Disclosure of Invention
Aiming at the problems existing in the background technology, the invention provides a preparation method of rod-shaped rutile titanium dioxide, which is safe in reaction condition operation and low in manufacturing cost.
The technical scheme adopted by the invention is as follows:
A preparation method of rod-shaped rutile titanium dioxide comprises the following steps:
(1) Preparation of potassium titanate: uniformly mixing a titanium-containing compound and a potassium-containing compound, putting the titanium-potassium mixture into a heating furnace, heating to 900-1200 ℃, and carrying out solid phase reaction for 1-10 hours at a constant temperature to obtain a potassium titanate solid;
(2) Depolymerization and ion exchange: adding deionized water and hydrochloric acid into the potassium titanate obtained in the step (1), preparing mixed slurry, stirring and dispersing, depolymerizing and ion exchanging the agglomerates, filtering, and repeatedly washing with deionized water until the conductivity of the filtrate is less than 100 mu S/cm to obtain a pretreated potassium titanate filter cake;
(3) Lattice reconstruction: adding deionized water and titanium tetrachloride into the pretreated potassium titanate filter cake obtained in the step (2), preparing mixed slurry, heating and preserving heat in sections, filtering, washing the filter cake by using the deionized water repeatedly until the conductivity of the filter cake is less than 100 mu S/cm, and drying the filter cake to obtain a rod-shaped rutile type titanium dioxide precursor;
(4) Crystal transformation and fusion: and (3) performing heat treatment on the rod-shaped rutile type titanium dioxide precursor obtained in the step (3) for 2-6 hours at 800-1000 ℃ to obtain the rod-shaped rutile type titanium dioxide.
The titanium-containing compound in the step (1) comprises titanium dioxide and metatitanic acid; the potassium-containing compound is selected from one or more of potassium carbonate, potassium bicarbonate, potassium chloride, potassium nitrate and potassium chlorate.
Further, the molar number of potassium in the potassium-containing compound in the step (1) is converted into K 2 O, the molar number of titanium in the titanium-containing compound is converted into TiO 2, and the molar ratio of the titanium-containing compound to the potassium-containing compound is as follows: n (TiO 2)：n(K2 O) =2 to 4:1.
The mixed slurry in the step (2) is mixed slurry with 3-15% of solid content and 1-3 mol/L of hydrochloric acid concentration, and is stirred and dispersed for 10-20 hours at 60-90 ℃ to carry out agglomerate depolymerization and ion exchange.
The mixed slurry in the step (3) is mixed slurry with the solid content of 10-30% and the titanium tetrachloride concentration of 1.2-2.0 mol/L; the sectional heating and heat preservation is to react at 20-40 ℃ for 10-20 hours, then heat to 80-100 ℃ at the heating rate of 0.1-0.3 ℃/min, and react at the heat preservation for 30-60 hours.
The rod-shaped rutile type titanium dioxide prepared by the method has the diameter of 0.1-0.6 micron and the length of 5-50 microns.
The invention has the beneficial effects that:
1. The invention firstly carries out depolymerization and ion exchange potassium removal activation treatment on potassium titanate, then takes the potassium titanate as a rod-shaped structural template, carries out ion exchange, nucleation, crystallization and lattice reconstruction on titanium tetrachloride solution, and finally prepares the rod-shaped rutile type titanium dioxide through high-temperature crystal transformation and fusion.
2. The invention has short process flow and simple and convenient operation.
Drawings
FIG. 1 is an SEM photograph of the product obtained in example 1;
FIG. 2 is an SEM photograph of the product obtained in example 2;
FIG. 3 is an SEM photograph of the product obtained in example 3;
FIG. 4X-ray diffraction patterns of the products obtained in example 1, example 2 and example 3.
Detailed Description
The invention is further described in detail below in connection with the examples: these examples are provided only to illustrate the invention and are not intended to limit the scope of the invention.
Example 1
1. Uniformly mixing 20 moles of rutile type nano titanium dioxide and 10 moles of potassium carbonate, putting the mixture into a heating furnace, heating to 900 ℃, and carrying out solid phase reaction for 10 hours while maintaining the temperature to obtain a potassium titanate solid.
2. Adding deionized water and hydrochloric acid into the potassium titanate obtained in the step 1 to prepare mixed slurry with 3% of solid content and 1 mol/liter of hydrochloric acid concentration, stirring and dispersing for 20 hours at 60 ℃, depolymerizing and ion exchanging the aggregates, filtering, and repeatedly washing with deionized water until the electric conductivity of the filtrate is 80 mu S/cm to obtain a pretreated potassium titanate filter cake.
3. Adding deionized water and titanium tetrachloride into the pretreated potassium titanate filter cake obtained in the step 2 to prepare mixed slurry with the solid content of 10% and the titanium tetrachloride concentration of 1.2 mol/liter, carrying out heat preservation reaction at 20 ℃ for 20 hours, heating to 80 ℃ at the heating rate of 0.1 ℃/min, carrying out heat preservation reaction for 60 hours, filtering, washing the filter cake by multiplexing deionized water repeatedly until the electric conductivity of the filter cake is 50 mu S/cm, and drying the filter cake to obtain the rod-shaped rutile type titanium dioxide precursor.
4. And (3) heat-treating the rod-shaped rutile titanium dioxide precursor obtained in the step (3) at 800 ℃ for 6 hours to obtain the rod-shaped rutile titanium dioxide.
Example 2
1. Uniformly mixing 20 moles of rutile type nano titanium dioxide and 10 moles of potassium carbonate, putting the mixture into a heating furnace, heating to 1200 ℃, and carrying out solid phase reaction for 1 hour while maintaining the temperature to obtain a potassium titanate solid.
2. Adding deionized water and hydrochloric acid into the potassium titanate obtained in the step 1 to prepare mixed slurry with the solid content of 15% and the hydrochloric acid concentration of 3 mol/liter, stirring and dispersing for 10 hours at 90 ℃, depolymerizing and ion exchanging the aggregates, filtering, and repeatedly washing with deionized water until the electric conductivity of the filtrate is 65 mu S/cm, thus obtaining a pretreated potassium titanate filter cake.
3. Adding deionized water and titanium tetrachloride into the pretreated potassium titanate filter cake obtained in the step 2 to prepare mixed slurry with the solid content of 30% and the titanium tetrachloride concentration of 2.0 mol/liter, carrying out heat preservation reaction at 40 ℃ for 10 hours, heating to 100 ℃ at the heating rate of 3 ℃/min, carrying out heat preservation reaction for 30 hours, filtering, washing by using deionized water repeatedly until the electric conductivity of the filtrate is 55 mu S/cm, and drying the filter cake to obtain the rod-shaped rutile type titanium dioxide precursor.
4. And (3) carrying out heat treatment on the rod-shaped rutile type titanium dioxide precursor obtained in the step (3) for 2 hours at the temperature of 1000 ℃ to obtain the micron rod-shaped rutile type titanium dioxide.
Example 3
1. Uniformly mixing 30 moles of rutile type nano titanium dioxide and 10 moles of potassium carbonate, putting the mixture into a heating furnace, heating to 1100 ℃, and carrying out solid phase reaction for 5 hours while maintaining the temperature to obtain a potassium titanate solid.
2. Adding deionized water and hydrochloric acid into the potassium titanate obtained in the step 1 to prepare mixed slurry with the solid content of 10% and the hydrochloric acid concentration of 2 mol/liter, stirring and dispersing for 15 hours at 80 ℃, depolymerizing and ion exchanging the aggregates, filtering, and repeatedly washing with deionized water until the electric conductivity of the filtrate is 70 mu S/cm to obtain a pretreated potassium titanate filter cake.
3. Adding deionized water and titanium tetrachloride into the pretreated potassium titanate filter cake obtained in the step 2 to prepare mixed slurry with the solid content of 20% and the titanium tetrachloride concentration of 1.5 mol/liter, carrying out heat preservation reaction for 16 hours at the temperature of 30 ℃, heating to 90 ℃ at the heating rate of 0.2 ℃/min, carrying out heat preservation reaction for 45 hours, filtering, washing by using the deionized water repeatedly until the electric conductivity of the filtrate is 66 mu S/cm, and drying the filter cake to obtain the rod-shaped rutile type titanium dioxide precursor.
4. And (3) carrying out heat treatment on the rod-shaped rutile type titanium dioxide precursor obtained in the step (3) for 5 hours at 900 ℃ to obtain the rod-shaped rutile type titanium dioxide.
Comparative example 1
1. Uniformly mixing 30 moles of rutile type nano titanium dioxide and 10 moles of potassium carbonate, putting the mixture into a heating furnace, heating to 1100 ℃, and carrying out solid phase reaction for 5 hours while maintaining the temperature to obtain a potassium titanate solid.
2. Adding deionized water and hydrochloric acid into the potassium titanate obtained in the step 1 to prepare mixed slurry with the solid content of 10% and the hydrochloric acid concentration of 2 mol/L, stirring and dispersing for 15 hours at 80 ℃, depolymerizing and ion exchanging the aggregates, filtering, washing by using deionized water repeatedly until the electric conductivity of the filtrate is 45 mu S/cm, and drying to obtain pretreated potassium titanate.
3. And (3) heat-treating the pretreated potassium titanate obtained in the step (2) for 5 hours at 900 ℃ to obtain the rod-shaped anatase titanium dioxide.
Comparative example 2
1. Uniformly mixing 30 moles of rutile type nano titanium dioxide and 10 moles of potassium carbonate, putting the mixture into a heating furnace, heating to 1100 ℃, and carrying out solid phase reaction for 5 hours while maintaining the temperature to obtain a potassium titanate solid.
2. Adding deionized water and titanium tetrachloride into the potassium titanate solid obtained in the step 1 to prepare mixed slurry with the solid content of 20% and the titanium tetrachloride concentration of 1.5 mol/liter, carrying out heat preservation reaction at 30 ℃ for 16 hours, heating to 90 ℃ at the heating rate of 0.2 ℃/min, carrying out heat preservation reaction for 45 hours, filtering, washing by using deionized water repeatedly until the filtrate conductivity is 63 mu S/cm, and drying a filter cake to obtain a rod-shaped titanium dioxide precursor.
3. The precursor of rod-shaped titanium dioxide obtained in the step 2 was heat-treated at 900℃for 5 hours to obtain rod-shaped titanium dioxide, but the product was approximately 68% rutile and 32% anatase.
Claims (5)
1. The preparation method of the rod-shaped rutile titanium dioxide is characterized by comprising the following steps of:
(1) Preparation of potassium titanate: uniformly mixing a titanium-containing compound and a potassium-containing compound, putting the titanium-potassium mixture into a heating furnace, heating to 900-1200 ℃, and carrying out solid phase reaction for 1-10 hours at a constant temperature to obtain a potassium titanate solid;
(2) Depolymerization and ion exchange: adding deionized water and hydrochloric acid into the potassium titanate obtained in the step (1) to prepare mixed slurry 1, stirring and dispersing, carrying out depolymerization and ion exchange of agglomerates, filtering, and repeatedly washing with deionized water until the conductivity of the filtrate is less than 100 mu S/cm to obtain a pretreated potassium titanate filter cake; the mixed slurry 1 is mixed slurry with 3-15% of solid content and 1-3 mol/L of hydrochloric acid concentration;
(3) Lattice reconstruction: adding deionized water and titanium tetrachloride into the pretreated potassium titanate filter cake obtained in the step (2), preparing mixed slurry 2, heating and preserving heat in sections, filtering, washing the filter cake by using the deionized water repeatedly until the electric conductivity of the filter cake is less than 100 mu S/cm, and drying the filter cake to obtain a rod-shaped rutile type titanium dioxide precursor; the mixed slurry 2 is mixed slurry with the solid content of 10-30% and the titanium tetrachloride concentration of 1.2-2.0 mol/L; the sectional heating and heat preservation is to react at 20-40 ℃ for 10-20 hours, then heat to 80-100 ℃ at the heating rate of 0.1-0.3 ℃/min, and react at the heat preservation for 30-60 hours;
(4) Crystal transformation and fusion: and (3) performing heat treatment on the rod-shaped rutile type titanium dioxide precursor obtained in the step (3) for 2-6 hours at 800-1000 ℃ to obtain the rod-shaped rutile type titanium dioxide.
2. The process for producing a rod-like rutile titanium dioxide according to claim 1, wherein the titanium-containing compound in the step (1) comprises titanium dioxide or metatitanic acid.
3. The process for producing a rod-like rutile titanium dioxide according to claim 1, wherein the potassium-containing compound in the step (1) is one or more selected from the group consisting of potassium carbonate, potassium hydrogencarbonate, potassium chloride, potassium nitrate and potassium chlorate.
4. The method of producing a rod-like rutile titanium dioxide according to claim 1, wherein the molar amount of potassium in the potassium-containing compound in the step (1) is reduced to K 2 O, the molar amount of titanium in the titanium-containing compound is reduced to TiO 2, and the molar ratio of the titanium-containing compound to the potassium-containing compound is: n (TiO 2)：n(K2 O) =2 to 4:1.
5. The process for producing rod-like rutile titanium dioxide according to claim 1, wherein the stirring and dispersing in the step (2) is carried out at 60 to 90℃for 10 to 20 hours.
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| CN102012379A (en) * | 2010-10-19 | 2011-04-13 | 攀钢集团钢铁钒钛股份有限公司 | Method for characterizing activity of titanium tetrachloride hydrolytic seed crystal |
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| CN108585037A (en) * | 2018-08-07 | 2018-09-28 | 天能工程复合材料制品(昆山)有限公司 | A kind of preparation method of high pure gold redrock type titanium dioxide crystal whisker |
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| CN102012379A (en) * | 2010-10-19 | 2011-04-13 | 攀钢集团钢铁钒钛股份有限公司 | Method for characterizing activity of titanium tetrachloride hydrolytic seed crystal |
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| 二次烧结法制备纳米TiO_2晶须的性能研究;马慧;高强;刘婉婉;葛明桥;;化工新型材料;20170415(第04期);第226-227页 * |
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