CN101033062A - Method of preparing layered alpha-titanium phosphate - Google Patents
Method of preparing layered alpha-titanium phosphate Download PDFInfo
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- CN101033062A CN101033062A CN 200710064070 CN200710064070A CN101033062A CN 101033062 A CN101033062 A CN 101033062A CN 200710064070 CN200710064070 CN 200710064070 CN 200710064070 A CN200710064070 A CN 200710064070A CN 101033062 A CN101033062 A CN 101033062A
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Abstract
This invention discloses a method for preparing laminated alpha-Ti3(PO4)2, which mixes Ti salt with deionized water in the proportion of 1 :4-10 to get deposit after being hydrolyzed fully to be cleaned and mixed in the proportion of 1 : 20-30 : 3-15, then the concentration of H3PO4 in the mixed solution is 4-12mol/L, then transfers the mixed solution into a high pressure kettle and reacts for 4-24 h under 150-200deg.C to be cooled to room temperature t obe cleaned to 3-7 pH value to be dried to get laminated alpha-Ti3(PO4)2.
Description
Technical field
The present invention relates to the preparation method of compound, particularly relate to a kind of preparation method of layered alpha-titanium phosphate.
Background technology
Layered alpha-titanium phosphate (α-Ti (HPO
4)
2H
2O) be a kind of cationic compound, it has high temperature resistant, radiation hardness, anti-strong acid, is insoluble in characteristics such as water and organic solvent, in addition, this compound had both had the ion-exchange performance as ion exchange resin, as can be used for reclaiming separation caesium, strontium isotope, and from seawater, extract potassium, caesium etc., have selective adsorption and catalytic performance again as zeolite, simultaneously, its phosphoric acid salt laminate still prepares the matrix of intercalation compound and layer post catalytic material.Compare with laminar alpha zirconium phosphate, layered alpha-titanium phosphate is easier to leafing and gelatinizing, more help preparing the layer post catalytic material of high-ratio surface, and the preparation cost of material is cheap, therefore, has broad application prospects.The method that prepare at present the stratiform titanium phosphate mainly contains circumfluence method and hydrofluoric acid method, but these two kinds of methods exist long reaction time, product degree of crystallinity low, have a shortcoming such as potential safety hazard to equipment corrosion resistance nature requirement height and to operator.
Summary of the invention
The purpose of this invention is to provide a kind of reaction times short, product degree of crystallinity is better, and the preparation method of the higher layered alpha-titanium phosphate of production security.
For solving the problems of the technologies described above, the present invention takes following technical scheme: a kind of preparation method of layered alpha-titanium phosphate, and be to be 1 by volume with titanium salt with deionized water: 4-10 mixes, and fully obtains throw out after the hydrolysis, washing precipitate is again with throw out, deionized water and dense H
3PO
4In molar ratio 1: 20-30: 3-15 mixes, and makes H in the mixed solution
3PO
4Concentration be 4-12mol/L, subsequently mixed solution is transferred in the autoclave, 150-200 ℃ of down reaction 4-24 hour, be cooled to room temperature, being washed with water to pH value is 3-7, drying obtains layered alpha-titanium phosphate.
In the preparation method of above-mentioned layered alpha-titanium phosphate, the selection of titanium salt is diversified, as tetrabutyl titanate, titanium isopropylate, titanium ethanolate, titanium tetrachloride or titanyl sulfate etc.
When titanium salt is mixed with water, preferably titanium salt is slowly dripped in the entry.
The washing methods of the hydrolytic precipitation thing of described titanium salt is preferably filtering and washing, and washing times is preferably 2-5 time, derives from foreign ion in the presoma with removal.
Described hydrolysis and bath water all are preferably deionized water.
Described drying temperature can be 50-80 ℃.
The invention provides a kind of preparation method of layered alpha-titanium phosphate.Compare with the preparation method of existing layered alpha-titanium phosphate, that preparation method of the present invention has is simple to operate, the reaction times short, low for equipment requirements, low production cost, and avoided using the hydrofluoric acid of severe corrosive, thereby guaranteed the security of producing, feasibility with suitability for industrialized production, in addition, the layered alpha-titanium phosphate that obtains with this method has degree of crystallinity height, pattern rule evenly (be hexagon is laminar, particle diameter evenly tiny) and the high advantage of thermostability.The present invention will play a significant role in the production of layered alpha-titanium phosphate, have a extensive future.
Below in conjunction with specific embodiment the present invention is described in further details.
Description of drawings
Fig. 1 is the SEM microstructure figure with the alpha-titanium phosphate of the inventive method preparation
Fig. 2 is the x-ray diffraction pattern with the alpha-titanium phosphate of the inventive method preparation
Embodiment
Method therefor is ordinary method if no special instructions among the following embodiment.
The preparation of embodiment 1, layered alpha-titanium phosphate
The 8.5g tetrabutyl titanate slowly is added dropwise to makes it abundant hydrolysis in the 50mL deionized water, behind the filtering and washing hydrolytic precipitation thing 3 times, in throw out, add 9.8g concentration and be 85% H
3PO
4Solution and 10mL deionized water, H in the mixed solution at this moment
3PO
4Concentration be 5.5mol/L, mixed solution is transferred in the teflon-lined stainless steel autoclave then, put into thermostat container, after reacting 16 hours under 180 ℃, be cooled to room temperature, with deionized water centrifuge washing to pH value is 3.8, at last that product is dry under 50 ℃, obtains layered alpha-titanium phosphate.
Sampling, layered alpha-titanium phosphate with method for preparing is carried out scanning electron microscope (SEM) and X-ray diffraction (XRD) analysis, (figure A is a pattern under the low power to the scanning electron microscope observation result as shown in Figure 1, figure B is a pattern under the high power), (X-coordinate is represented diffraction angle to x-ray diffraction pattern, and ordinate zou is represented diffracted intensity as shown in Figure 2; (002) diffraction crystal face correspondence the interlamellar spacing of layered alpha-titanium phosphate, and corresponding diffraction angle 2 θ=11.6 ° draw the interlamellar spacing size and are 0.76nm.Show with method of the present invention to have obtained better crystallinity degree, the pattern rule is even, and particle diameter is evenly tiny, and median size is about 400nm, the thick laminar alpha-titanium phosphate crystal of hexagon that is about 60nm of sheet, and have higher thermostability.
The preparation of embodiment 2, layered alpha-titanium phosphate
The 7.11g titanium isopropylate slowly is added dropwise to makes it abundant hydrolysis in the 40mL deionized water, behind the filtering and washing hydrolytic precipitation thing 5 times, in throw out, add 31.16g concentration and be 85% H
3PO
4Solution and 10mL deionized water, H in the mixed solution at this moment
3PO
4Volumetric molar concentration be 10mol/L, mixed solution is transferred in the teflon-lined stainless steel autoclave, put into thermostat container, after reacting 24 hours under 150 ℃, be cooled to room temperature, with deionized water centrifuge washing to pH value is 7, at last that product is dry under 60 ℃, obtains layered alpha-titanium phosphate.
Sampling, layered alpha-titanium phosphate with method for preparing is carried out scanning electron microscope and X-ray diffraction analysis, detected result shows with aforesaid method and has obtained better crystallinity degree, the pattern rule evenly, particle diameter is evenly tiny, and median size is about 300nm, the thick 60nm that is about of sheet, the interlamellar spacing size is the laminar alpha-titanium phosphate crystal of hexagon of 0.76nm, and has higher thermostability.
The preparation of embodiment 3, layered alpha-titanium phosphate
The 5.70g titanium ethanolate slowly is added dropwise to makes it abundant hydrolysis in the 30mL deionized water, behind the filtering and washing hydrolytic precipitation thing 4 times, in throw out, add 14.3g concentration and be 85% H
3PO
4Solution and 10mL deionized water, H in the mixed solution at this moment
3PO
4Volumetric molar concentration be 7mol/L, mixed solution is transferred in the teflon-lined stainless steel autoclave, put into thermostat container, being cooled to room temperature in reaction under 200 ℃ after 4 hours, is 6 with deionized water centrifuge washing to pH value, at last that product is dry under 70 ℃, obtain layered alpha-titanium phosphate.
Sampling, layered alpha-titanium phosphate with method for preparing is carried out scanning electron microscope and X-ray diffraction analysis, detected result shows with aforesaid method and has obtained better crystallinity degree, the pattern rule evenly, particle diameter is evenly tiny, and median size is about 500nm, the thick 60nm that is about of sheet, the interlamellar spacing size is the laminar alpha-titanium phosphate crystal of hexagon of 0.76nm, and has higher thermostability.
The preparation of embodiment 4, layered alpha-titanium phosphate
The 4.74g titanium tetrachloride slowly is added dropwise to makes it abundant hydrolysis in the 30mL deionized water, behind the filtering and washing hydrolytic precipitation thing 3 times, in throw out, add 18.67g concentration and be 85% H
3PO
4Solution and 10mL deionized water, H in the mixed solution at this moment
3PO
4Volumetric molar concentration be 8mol/L, mixed solution is transferred in the teflon-lined stainless steel autoclave, put into thermostat container, after reacting 10 hours under 170 ℃, be cooled to room temperature, with deionized water centrifuge washing to pH value is 5, at last that product is dry under 80 ℃, obtains layered alpha-titanium phosphate.
Sampling, layered alpha-titanium phosphate with method for preparing is carried out scanning electron microscope and X-ray diffraction analysis, detected result shows with aforesaid method and has obtained better crystallinity degree, the pattern rule evenly, particle diameter is evenly tiny, and median size is about 400nm, the thick 60nm that is about of sheet, the interlamellar spacing size is the laminar alpha-titanium phosphate crystal of hexagon of 0.76nm, and has higher thermostability.
The preparation of embodiment 5, layered alpha-titanium phosphate
The 4.90g titanyl sulfate slowly is added dropwise to makes it abundant hydrolysis in the 30mL deionized water, behind the filtering and washing hydrolytic precipitation thing 3 times, in throw out, add 23.84g concentration and be 85% H
3PO
4Solution and 10mL deionized water, H in the mixed solution at this moment
3PO
4Volumetric molar concentration be 9mol/L, mixed solution is transferred in the teflon-lined stainless steel autoclave, put into thermostat container, after reacting 12 hours under 160 ℃, be cooled to room temperature, with deionized water centrifuge washing to pH value is 4, at last that product is dry under 60 ℃, obtains layered alpha-titanium phosphate.
Sampling, layered alpha-titanium phosphate with method for preparing is carried out scanning electron microscope and X-ray diffraction analysis, detected result shows with aforesaid method and has obtained better crystallinity degree, the pattern rule evenly, particle diameter is evenly tiny, and median size is about 350nm, the thick 60nm that is about of sheet, the interlamellar spacing size is the laminar alpha-titanium phosphate crystal of hexagon of 0.76nm, and has higher thermostability.
Claims (7)
1, a kind of preparation method of layered alpha-titanium phosphate, be to be 1 by volume with titanium salt with deionized water: 4-10 mixes, and fully obtains throw out after the hydrolysis, and washing precipitate is again with throw out, deionized water and dense H
3PO
4In molar ratio 1: 20-30: 3-15 mixes, and makes H in the mixed solution
3PO
4Concentration be 4-12mol/L, subsequently mixed solution is transferred in the autoclave, 150-200 ℃ of down reaction 4-24 hour, be cooled to room temperature, being washed with water to pH value is 3-7, drying obtains layered alpha-titanium phosphate.
2, preparation method according to claim 1 is characterized in that: described titanium salt is tetrabutyl titanate, titanium isopropylate, titanium ethanolate, titanium tetrachloride or titanyl sulfate.
3, preparation method according to claim 1 is characterized in that: described when titanium salt is mixed with water, titanium salt is slowly dripped in the entry.
4, preparation method according to claim 1 is characterized in that: the method for the hydrolytic precipitation thing of described washing titanium salt is a filtering and washing, and washing times is 2-5 time.
5, preparation method according to claim 1 is characterized in that: described hydrolysis and bath water are deionized water.
6, according to each described preparation method of claim 1-5, it is characterized in that: described drying temperature is 50-80 ℃.
7, the layered alpha-titanium phosphate for preparing with each described method of claim 1-6.
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| CN103626145A (en) * | 2013-12-04 | 2014-03-12 | 中国科学院化学研究所 | Titanium phosphate nano material as well as preparation method and application thereof |
| CN107311137A (en) * | 2017-08-04 | 2017-11-03 | 武汉理工大学 | A kind of method of utilization titanium tetrachloride solvent-thermally synthesizing nano Titanium pyrophosphate |
| CN108383095A (en) * | 2018-03-13 | 2018-08-10 | 河北工业大学 | A kind of method that ion-exchange prepares intercalation alpha-titanium phosphate |
| JPWO2018180797A1 (en) * | 2017-03-30 | 2019-11-07 | 株式会社フジミインコーポレーテッド | Titanium phosphate powder and production method thereof, white pigment for cosmetics |
| CN110499138A (en) * | 2019-08-02 | 2019-11-26 | 上海嗣高新材料科技有限公司 | A kind of halon-free intumescent fire stopping mastic and preparation method thereof |
| CN111348634A (en) * | 2020-03-31 | 2020-06-30 | 龙佰四川钛业有限公司 | Preparation method of layered α -titanium phosphate |
| CN112739647A (en) * | 2018-09-20 | 2021-04-30 | 福吉米株式会社 | White pigment for cosmetic and cosmetic |
| CN112771001A (en) * | 2018-09-20 | 2021-05-07 | 福吉米株式会社 | White pigment for cosmetic and cosmetic |
| CN112928276A (en) * | 2019-12-06 | 2021-06-08 | 中国科学院大连化学物理研究所 | Composite sulfur positive electrode material and preparation method and application thereof |
| WO2022185648A1 (en) * | 2021-03-04 | 2022-09-09 | 株式会社フジミインコーポレーテッド | Powder, filler, composition, and filler production method |
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| CN103626145A (en) * | 2013-12-04 | 2014-03-12 | 中国科学院化学研究所 | Titanium phosphate nano material as well as preparation method and application thereof |
| CN103626145B (en) * | 2013-12-04 | 2016-02-24 | 中国科学院化学研究所 | Titanium phosphate nano material and preparation method thereof and application |
| US11345596B2 (en) | 2017-03-30 | 2022-05-31 | Fujimi Incorporated | Titanium phosphate powder, production method therefor, and white pigment for cosmetics |
| CN112499611A (en) * | 2017-03-30 | 2021-03-16 | 福吉米株式会社 | Titanium phosphate powder, method for producing same, and white pigment for cosmetics |
| JPWO2018180797A1 (en) * | 2017-03-30 | 2019-11-07 | 株式会社フジミインコーポレーテッド | Titanium phosphate powder and production method thereof, white pigment for cosmetics |
| CN110461765A (en) * | 2017-03-30 | 2019-11-15 | 福吉米株式会社 | Titanium phosphate powder and its manufacturing method, white pigment used for cosmetic |
| CN111994888B (en) * | 2017-03-30 | 2023-11-17 | 福吉米株式会社 | Titanium phosphate powder, process for producing the same, and white pigment for cosmetics |
| JP2020079284A (en) * | 2017-03-30 | 2020-05-28 | 株式会社フジミインコーポレーテッド | White pigment for cosmetics comprising titanium phosphate powder |
| JP7165469B2 (en) | 2017-03-30 | 2022-11-04 | 株式会社フジミインコーポレーテッド | White pigment for cosmetics composed of titanium phosphate powder |
| CN111994888A (en) * | 2017-03-30 | 2020-11-27 | 福吉米株式会社 | Titanium phosphate powder, method for producing same, and white pigment for cosmetics |
| CN107311137A (en) * | 2017-08-04 | 2017-11-03 | 武汉理工大学 | A kind of method of utilization titanium tetrachloride solvent-thermally synthesizing nano Titanium pyrophosphate |
| CN108383095B (en) * | 2018-03-13 | 2021-01-19 | 河北工业大学 | Method for preparing intercalation alpha-titanium phosphate by ion exchange method |
| CN108383095A (en) * | 2018-03-13 | 2018-08-10 | 河北工业大学 | A kind of method that ion-exchange prepares intercalation alpha-titanium phosphate |
| CN112739647A (en) * | 2018-09-20 | 2021-04-30 | 福吉米株式会社 | White pigment for cosmetic and cosmetic |
| CN112771001A (en) * | 2018-09-20 | 2021-05-07 | 福吉米株式会社 | White pigment for cosmetic and cosmetic |
| US11638681B2 (en) | 2018-09-20 | 2023-05-02 | Fujimi Incorporated | White pigment for cosmetics, and cosmetic |
| CN112739647B (en) * | 2018-09-20 | 2023-11-21 | 福吉米株式会社 | White pigment for cosmetics and cosmetics |
| CN110499138A (en) * | 2019-08-02 | 2019-11-26 | 上海嗣高新材料科技有限公司 | A kind of halon-free intumescent fire stopping mastic and preparation method thereof |
| CN112928276A (en) * | 2019-12-06 | 2021-06-08 | 中国科学院大连化学物理研究所 | Composite sulfur positive electrode material and preparation method and application thereof |
| CN111348634A (en) * | 2020-03-31 | 2020-06-30 | 龙佰四川钛业有限公司 | Preparation method of layered α -titanium phosphate |
| WO2022185648A1 (en) * | 2021-03-04 | 2022-09-09 | 株式会社フジミインコーポレーテッド | Powder, filler, composition, and filler production method |
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