CN102304762A - Preparation method of potassium hexatitanate whiskers - Google Patents
Preparation method of potassium hexatitanate whiskers Download PDFInfo
- Publication number
- CN102304762A CN102304762A CN201110289501A CN201110289501A CN102304762A CN 102304762 A CN102304762 A CN 102304762A CN 201110289501 A CN201110289501 A CN 201110289501A CN 201110289501 A CN201110289501 A CN 201110289501A CN 102304762 A CN102304762 A CN 102304762A
- Authority
- CN
- China
- Prior art keywords
- hours
- product
- potassium
- roasting
- preparation
- Prior art date
- 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.)
- Pending
Links
Images
Landscapes
- Inorganic Compounds Of Heavy Metals (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The invention relates to a preparation method of potassium hexatitanate whiskers and belongs to the technical field of preparation of chemical products. The method is characterized by comprising the following steps: evenly mixing K2CO3 with metatitanic acid containing 40wt% of TiO2 at the room temperature, wherein the molar ratio of K2CO3 to TiO2 is 1:3.5; placing the mixture into a 150 DEG C drying oven, stirring regularly, and drying for 24 hours to obtain a reaction precursor; placing 100 g of the precursor into a 250 ml crucible, placing the crucible in a muffle furnace, and roasting at 150 DEG C, 400 DEG C, 600 DEG C, 800 DEG C, 1000 DEG C and 1150 DEG C respectively for 2 hours, 4 hours, 7 hours and 10 hours; and placing the products which are obtained by roasting at 1000 DEG C and 1150 DEG for different time in a constant boiling water bath to perform water leaching treatment for 10 hours, performing suction filtering on the product, and drying the obtained product in a 150 DEG C drying oven for 24 hours to obtain the potassium hexatitanate whisker product.
Description
Technical field
The invention belongs to chemical product preparation technical field, refer in particular to a kind of crystal whisker of hexa potassium titanate preparation method.
Background technology
Potassium titanate is one type, and to have chemical formula be K
2OnTiO
2The compound of (n=1,2,4,6,8).Potassium tetratitanate has the excellent in chemical activity, can be used as ion-exchange, liquid waste disposal etc., can be used as the Nuclear power plants liquid waste disposal like potassium tetratitanate; Six potassium titanate chemical property are the most stable, have good physical properties, like corrosion-resistant, high temperature resistant, wear resistance, lower thermal conductivity and high infrared reflection rate etc.Can be used as heat insulation, heat-resisting, insulating material, friction materials, the application of reinforced composite.Eight potassium titanates have good electrified performance, can do anode material, semiconductor material and the photochemical catalysis etc. of Li battery.Potassium titanate is developed as the rocket nozzle lagging material by NASA at first.
The synthesis method of potassium titanate mainly contains sintering process, flux method, scorification, hydrothermal method, KDC method, microwave method and ion exchange method at present.The raw material of synthetic potassium titanate all adopts rutile or anatase titanium dioxide usually, and raw materials cost is higher, for the popularization and application of potassium titanate brings difficulty.How to make full use of resource, reduce cost, reduce environmental pollution, become the problem that to consider.Metatitanic acid is the intermediate that ilmenite is produced titanium dioxide, needs to get rutile or anatase titanium dioxide through pyroprocessing, and the price of metatitanic acid is far below titanium dioxide.The present invention develops and adopts metatitanic acid is that raw material passes through a step sintering process and synthesized crystal whisker of hexa potassium titanate, can effectively reduce raw materials cost and environmental pollution.
Summary of the invention
The objective of the invention is to develop a kind of crystal whisker of hexa potassium titanate preparation method, it is characterized by: K
2CO
3(contain TiO with metatitanic acid
2[n (K 40wt%) in molar ratio
2CO
3)/n (TiO
2)] be at room temperature to mix at 1: 3.5, put into 150 ℃ of loft drier, regularly to stir, be 24h time of drying, must react precursor.In the 250ml crucible, put into the 100g precursor, in 150 ℃, 400 ℃, 600 ℃, 800 ℃, 1000 ℃, 1150 ℃ following roastings, roasting time is got 2h, 4h, 7h, 10h respectively in retort furnace.To temperature is that 1000 ℃, 1150 ℃ roasting different time products therefroms carry out water logging processing 10h in the azeotropic water-bath, and product filters after water logging is handled, and puts into to obtain the crystal whisker of hexa potassium titanate product after 150 ℃ of loft drier are dried 24h.
Crystal whisker of hexa potassium titanate samples using Bruker-AXS D8 type x-ray powder diffraction instrument is analyzed, Cu target K α (ray of λ=0.15406nm), graphite monochromator, tube voltage are 40kV, tube current is 200mA, sweep velocity be 4 (°)/min.The pattern of sample adopts the analysis of JSM7001F scanning electron microscope observation.
With K
2CO
3(contain TiO with metatitanic acid
2[n (K 40wt%) in molar ratio
2CO
3)/n (TiO
2)] be 1: 3.5, the XRD spectra of roasting 10h products therefrom is as shown in Figure 1 under differing temps.Product by Fig. 1 can get under the different maturing temperatures is formed: the principal product under 150 ℃ of roastings is TiO
2And K
2SO
4(acid of titanium attitude is that the ilmenite and the vitriol oil are produced TiO partially
2Intermediate, contain due to the sulfuric acid of not washing off); When temperature was elevated to 400 ℃, principal product was still TiO
2And K
2SO
4When temperature is 600 ℃, the generation of eight potassium titanates is arranged in the product and be accompanied by TiO
2Minimizing; When temperature is raised to 800 ℃, generated six potassium titanates and potassium tetratitanate, and four metatitanic acid clocks are suitable with six potassium titanate content, and are accompanied by TiO
2Further minimizing; The content of six potassium titanates increases and potassium tetratitanate content reduces relatively in the product when temperature is 1000 ℃, and the oriented six potassium titanates conversion of potassium tetratitanate in the reaction be described; When temperature reaches 1150 ℃; Obvious increase of six potassium titanate content and potassium tetratitanate obviously reduce in the product; Further specify potassium tetratitanate and at high temperature transform, and the XRD absorption peak of six potassium titanates is very strong under this temperature, illustrate at high temperature to make the more perfection of its crystalline form to six potassium titanates.
Visible by Fig. 1, when temperature has been found the sign that potassium tetratitanate transforms to six potassium titanates 1000 ℃ and 1150 ℃ of following times, so compare being reflected at 1000 ℃ and 1150 ℃ of following roasting different times, roasting time is got 2h, 4h, 7h, 10h respectively.Gained XRD spectra such as Fig. 2 and shown in Figure 3.As shown in Figure 2, be reflected under 1000 ℃, along with the growth of roasting time, six potassium titanate content increase to some extent, and being illustrated in the K/Ti ratio is when maturing temperature was 1000 ℃ in 1: 3.5, and existing potassium tetratitanate transforms to six potassium titanates.Along with the growth of roasting time, six potassium titanates obviously increase and follow the minimizing of potassium tetratitanate when temperature is 1150 ℃, and high temperature makes that the crystalline form of six potassium titanates is more regular, as shown in Figure 3.
Fig. 4 for potassium titanium ratio be 1: 3.5 in the XRD spectra of 1150 ℃ of following roasting different times after water logging is handled; Potassium tetratitanate disappears after water logging is handled; And then generation be the generation of hydration eight potassium titanates, and another material six potassium titanates do not change because of the water logging treating processes in the product.
Fig. 5 is 1: 3.5 SEM pattern at 1150 ℃ of following roasting different times filtering and washing products therefrom after water logging is handled for potassium titanium ratio.When being reflected at this roasting temperature 2h, the more tiny (see figure 6) of product grain diameter.
Can be preferably in the above-mentioned preparation process, potassium titanium ratio is [n (K in molar ratio
2CO
3)/n (TiO
2)] be 1: 3.5, when maturing temperature reached 1150 ℃, roasting time was got 10h, and products therefrom carries out water logging and handles 10h in the azeotropic water-bath, and product filters after water logging is handled, and puts into to obtain the crystal whisker of hexa potassium titanate product after 150 ℃ of loft drier are dried 24h.
Description of drawings
Fig. 1 potassium titanium is the XRD spectra of roasting 10h products therefrom under 1: 3.5 differing temps
Fig. 2 potassium titanium ratio is 1: 3.5 XRD spectra at 1000 ℃ of following roasting different time gained samples
◆：K
2Ti
4O
9 
：K
2Ti
6O
13
Fig. 3 potassium titanium ratio is 1: 3.5 XRD spectra at 1150 ℃ of following roasting different time gained samples
◆：K
2Ti
4O
9 ：K
2Ti
6O
13
Fig. 4 potassium titanium ratio is 1: 3.5 XRD spectra at 1150 ℃ of following roasting different times product after water extraction is handled
：K
2Ti
6O
13 
：K
2(H
2O)
0.66Ti
8O
16(OH)
2
Fig. 5 potassium titanium ratio is 1: 3.5 SEM pattern at 1150 ℃ of following roasting different time products therefroms
Embodiment
With K
2CO
3(contain TiO with metatitanic acid
2[n (K 40wt%) in molar ratio
2CO
3)/n (TiO
2)] be at room temperature to mix at 1: 3.5, put into 150 ℃ of loft drier, regularly to stir, time of drying, 24h must react precursor.In the 250ml crucible, put into the 100g precursor; In retort furnace in 1150 ℃ of following roasting 10h; To temperature is that 1150 ℃ of roasting products therefroms carry out water logging processing 10h in the azeotropic water-bath, and product filters after water logging is handled, and puts into to obtain the crystal whisker of hexa potassium titanate product after 150 ℃ of loft drier are dried 24h.
Claims (2)
1. a crystal whisker of hexa potassium titanate preparation method is characterized by: with K
2CO
3(contain TiO with metatitanic acid
2[n (K 40wt%) in molar ratio
2CO
3)/n (TiO
2)] be at room temperature to mix at 1: 3.5, put into 150 ℃ of loft drier, regularly to stir, be 24h time of drying, must react precursor; In the 250ml crucible, put into the 100g precursor, in 150 ℃, 400 ℃, 600 ℃, 800 ℃, 1000 ℃, 1150 ℃ following roastings, roasting time is got 2h, 4h, 7h, 10h respectively in retort furnace; To temperature is that 1000 ℃, 1150 ℃ roasting different time products therefroms carry out water logging processing 10h in the azeotropic water-bath, and product filters after water logging is handled, and puts into to obtain the crystal whisker of hexa potassium titanate product after 150 ℃ of loft drier are dried 24h.
2. according to the said a kind of crystal whisker of hexa potassium titanate preparation method of claim 1, preparation technology can be preferably, with K
2CO
3(contain TiO with metatitanic acid
2[n (K 40wt%) in molar ratio
2CO
3)/n (TiO
2)] be 1: 3.5, when maturing temperature reached 1150 ℃, roasting time was got 10h, and products therefrom carries out water logging and handles 10h in the azeotropic water-bath, and product filters after water logging is handled, and puts into to obtain the crystal whisker of hexa potassium titanate product after 150 ℃ of loft drier are dried 24h.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110289501A CN102304762A (en) | 2011-09-21 | 2011-09-21 | Preparation method of potassium hexatitanate whiskers |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110289501A CN102304762A (en) | 2011-09-21 | 2011-09-21 | Preparation method of potassium hexatitanate whiskers |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN102304762A true CN102304762A (en) | 2012-01-04 |
Family
ID=45378673
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201110289501A Pending CN102304762A (en) | 2011-09-21 | 2011-09-21 | Preparation method of potassium hexatitanate whiskers |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102304762A (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102839424A (en) * | 2012-09-27 | 2012-12-26 | 攀枝花学院 | Method for preparing potassium hexatitanate whisker |
| CN104846429A (en) * | 2015-04-14 | 2015-08-19 | 张家港大塚化学有限公司 | Preparation method of potassium hexatitanate crystal plates |
| CN104843774A (en) * | 2015-04-14 | 2015-08-19 | 张家港大塚化学有限公司 | Preparation method of large-particle-size potassium titanate material |
| CN108166051A (en) * | 2018-03-08 | 2018-06-15 | 合肥工业大学 | A kind of morphology controllable potassium hexatitanate powder crystal material and its low energy consumption preparation method |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101250751A (en) * | 2007-11-30 | 2008-08-27 | 江苏大学 | Method for preparing crystal wisker of potassium hexatitanate |
-
2011
- 2011-09-21 CN CN201110289501A patent/CN102304762A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101250751A (en) * | 2007-11-30 | 2008-08-27 | 江苏大学 | Method for preparing crystal wisker of potassium hexatitanate |
Non-Patent Citations (1)
| Title |
|---|
| 柳春艳等: "偏钛酸为原料烧结法制备超细六钛酸钾晶须", 《中国有色金属学报》 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102839424A (en) * | 2012-09-27 | 2012-12-26 | 攀枝花学院 | Method for preparing potassium hexatitanate whisker |
| CN102839424B (en) * | 2012-09-27 | 2015-06-17 | 攀枝花学院 | Method for preparing potassium hexatitanate whisker |
| CN104846429A (en) * | 2015-04-14 | 2015-08-19 | 张家港大塚化学有限公司 | Preparation method of potassium hexatitanate crystal plates |
| CN104843774A (en) * | 2015-04-14 | 2015-08-19 | 张家港大塚化学有限公司 | Preparation method of large-particle-size potassium titanate material |
| CN104846429B (en) * | 2015-04-14 | 2017-05-10 | 张家港大塚化学有限公司 | Preparation method of potassium hexatitanate crystal plates |
| CN108166051A (en) * | 2018-03-08 | 2018-06-15 | 合肥工业大学 | A kind of morphology controllable potassium hexatitanate powder crystal material and its low energy consumption preparation method |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Wang et al. | Novel process for titanium dioxide production from titanium slag: NaOH-KOH binary molten salt roasting and water leaching | |
| Rehan et al. | Hydrothermal synthesis of titanium dioxide nanoparticles studied employing in situ energy dispersive X-ray diffraction | |
| Baldassari et al. | Microwave-hydrothermal process for the synthesis of rutile | |
| Wang et al. | Preparation of rutile titanium dioxide white pigment via doping and calcination of metatitanic acid obtained by the NaOH molten salt method | |
| Bao et al. | High quality and yield in potassium titanate whiskers synthesized by calcination from hydrous titania | |
| CN102304762A (en) | Preparation method of potassium hexatitanate whiskers | |
| CN102701277A (en) | Method for preparing rutile titanium dioxide | |
| CN100334000C (en) | Process for preparing rutile-phase nano-titanium dioxide | |
| Zhang et al. | Titanium extraction from spent selective catalytic reduction catalysts in a NaOH molten-salt system: Thermodynamic, experimental, and kinetic studies | |
| CN102583324A (en) | Preparation method of amorphous state carbon nano tube | |
| Laptash et al. | Fluoride processing of titanium-containing minerals | |
| CN105967229B (en) | A kind of bar-shaped titanium dioxide and preparation method thereof | |
| CN106801256A (en) | A kind of method that solid phase method prepares potassium hexatitanate platelet | |
| Hou et al. | Efficient fabrication of spinel copper ferrite with enhanced high infrared radiation properties | |
| CN104603059B (en) | Ultrafine particles of titanium dioxide and method for producing same | |
| CN104192890A (en) | Method for preparing carbon-dope zinc oxide nanopillars | |
| CN106629840A (en) | Preparation method of truncated cylinder-shaped octahedral anatase type TiO2 | |
| CN101811677B (en) | Method for preparing hollow porous quadruped titanium nitride | |
| Chacko et al. | Effect of growth techniques on the structural and optical properties of TiO2 nanostructures | |
| Aristanti et al. | Decomposition of banten ilmenite by caustic fusion process for TiO2 photocatalytic applications | |
| Fan et al. | Nitrogen doped anatase TiO2 sheets with dominant {001} facets for enhancing visible-light photocatalytic activity | |
| Carlucci et al. | Controllable one-pot synthesis of anatase TiO2 nanorods with the microwave-solvothermal method | |
| CN103130270A (en) | Preparation method of titanium dioxide nanometer powder | |
| CN105819503A (en) | Preparation method of uniform-sized mixed-crystal TiO2 microspheres | |
| de Salazar et al. | Research of obtaining TiO2 by sol-gel method using titanium isopropoxide TIP and tetra-n-butyl orthotitanate TNB |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20120104 |