CN104724764A - Platinum oxide nano powder and preparation method thereof - Google Patents
Platinum oxide nano powder and preparation method thereof Download PDFInfo
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- CN104724764A CN104724764A CN201510083549.6A CN201510083549A CN104724764A CN 104724764 A CN104724764 A CN 104724764A CN 201510083549 A CN201510083549 A CN 201510083549A CN 104724764 A CN104724764 A CN 104724764A
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Abstract
The invention relates to platinum oxide nano powder and a preparation method thereof, for solving the problems of complicated process, relatively high cost and the like in the prior art. The platinum oxide nano powder is obtained by the steps of performing hydrothermal reaction on platinum sheets in a mixed solution of hydrogen peroxide and hydrogen fluoride, then evaporating all solvents to obtain white powder, flushing and drying. The particle diameter of platinum oxide is 10-50nm. The process is simple, surfactants and complicated processes are not needed, and the preparation method is suitable for large-scale batch production of the platinum oxide nano powder.
Description
Technical field
The present invention relates to platinum oxide nano-powder, especially preparation method's technical field of platinum oxide nano-powder.
Background technology
The heterogeneous A dams catalyzer that platinum dioxide (PtO2) is famous, have that catalytic performance is excellent, activity is high, selectivity is high, long service life and the advantage such as recyclable, Adams catalyzer plays an important role always in hydrogenating catalytic reaction, the multiple group of its energy hydrogenation, is usually used in hydrogenation or the hydrogenolysis of ethylene linkage, hydroxyl, aldehyde radical, imido grpup, aromatic nitro and aromatic ring.
Nineteen twenty-two Adams has prepared platinum oxide solid catalyst at 450 DEG C with Platinic chloride and SODIUMNITRATE reaction, Reetz in 1999 etc. with quaternary amine tensio-active agent for stablizer, the basic solution of PtCl4 is hydrolyzed 7d at 50 DEG C, obtain the water soluble oxidized platinum nano-powder that particle diameter is 1.9nm, and for catalytic reduction amination reaction, result display colloidal silica platinum catalysis activity is approximately 4 ~ 5 times of commercial catalysts.Polyvinylpyrrolidone (PVP) used as stabilizers such as Chen Yi virtuous grade in 2004, adds acetic acid by after platinum chloride aqueous solution in the basic conditions ebuillition of heated, and reaction for some time obtains platinum oxide colloid, and particle diameter reaches 51.7nm, but is attended by White Flocculus.Within 2005, breathing out sunlight etc. and use PVP used as stabilizers equally, by regulating the pH value of reaction system, obtaining the platinum oxide nano-powder that particle diameter is 0.94nm when pH value is 6.92.
At present, preparation method's existence of most of platinum oxide nano-powder is not suitable for large-scale production, the problems such as cost is higher, easy reunion.
Summary of the invention
The shortcoming of prior art in view of the above, the object of the present invention is to provide platinum dioxide nano-powder prepared by a kind of preparation method of platinum dioxide nano-powder and the method, it has, and method equipment is simple, cost is low, do not need to add tensio-active agent, experiment condition is controlled, be easy to suitability for industrialized production, and prepared platinum oxide particle diameter of nanometer powder is little, narrowly distributing and the feature such as should not to reunite.
For achieving the above object and other relevant objects, the invention provides a kind of preparation method of platinum oxide nano-powder, it is characterized in that, described preparation method at least comprises the following steps:
(1) process in early stage of platinized platinum;
(2) mixing solutions is configured: in the container of mixing solutions filling hydrogen peroxide and deionized water, add hydrogen fluoride solution, fully dissolve, be configured to mixing solutions;
(3) hydrothermal treatment consists: the platinized platinum in being walked by a tiltedly puts into autoclave, the mixing solutions got in step 2 moves into reactor inner bag, is then sealed by still; Autoclave is incubated 10-30h at 150 DEG C-220 DEG C, naturally cools to room temperature, open reactor afterwards, heat and solution in still is evaporated completely, bottom reactor He on platinized platinum, generate white powder;
(4) dry: the white powder bottom reactor and on platinized platinum is taken out, repeatedly rinses with deionized water, dry to obtain nano oxidized platinum.
Preferably, the early stage of platinized platinum described in step 1 is treated to carries out ultrasonic cleaning successively by platinized platinum in deionized water, alcohol, acetone soln, dries up for subsequent use in air.
Preferably, in step 2, the concentration of hydrogen peroxide is 30wt%, and the volume ratio of hydrogen peroxide and deionized water is 1:1.
Preferably, in mixing solutions described in step 2, hydrofluoric concentration is 0.025mol/L.
Preferably, in step 3, after opening reaction kettle cover, with the heating temperatures reactor of 60-80 DEG C until solution evaporates completely.
Platinum oxide nano-powder prepared by method according to claim 1, its particle diameter is 10-50nm.。
As mentioned above, complete denomination of invention of the present invention, have following beneficial effect: the present invention adopts hydrothermal oxidization method, being matrix with platinized platinum, take hydrogen peroxide as oxygenant, platinum oxide nano-powder is obtained by reacting under liquid phase, preparation process is simple, it is low, high without particular requirement, product purity to equipment to consume energy, and experiment proves, the platinum oxide nano-powder grain diameter obtained is little, narrowly distributing and should not reuniting, has satisfactory stability.
Accompanying drawing explanation
Fig. 1 is transmission electron microscope (TEM) photo of the platinum oxide nano-powder that the present invention synthesizes.
Embodiment
Unless specified or limited otherwise, all chemical kit materials of following examples are chemical pure.
Embodiment 1
The preparation method of platinum oxide nano-powder:
(1) process in early stage of platinized platinum; Platinized platinum is carried out ultrasonic cleaning successively in deionized water, alcohol, acetone soln, dries up for subsequent use in air;
(2) in mixing solutions (20ml hydrogen peroxide (30wt%) and the 20ml deionized water) container filling hydrogen peroxide and deionized water, add hydrogen fluoride, abundant dissolving, is configured to mixing solutions, and in mixing solutions, hydrofluoric concentration is 0.025mol/L;
(3) hydrothermal treatment consists: the platinized platinum in being walked by a tiltedly puts into autoclave, the mixing solutions got in step 2 moves into reactor inner bag, is then sealed by still; Autoclave is incubated 15h at 150 DEG C, naturally cools to room temperature, open reactor afterwards, solution in still evaporates by 60 DEG C of heating completely, bottom reactor He on platinized platinum, generate white powder;
(4) dry: taken out by the white powder bottom reactor and on platinized platinum, repeatedly rinse with deionized water, dry to obtain platinum oxide powder, its particle diameter is 10-50nm.
Embodiment 2
The preparation method of platinum oxide nano-powder:
(1) process in early stage of platinized platinum; Platinized platinum is carried out ultrasonic cleaning successively in deionized water, alcohol, acetone soln, dries up for subsequent use in air;
(2) in mixing solutions (20ml hydrogen peroxide (30wt%) and the 20ml deionized water) container filling hydrogen peroxide and deionized water, add hydrogen fluoride, abundant dissolving, is configured to mixing solutions, and in mixing solutions, hydrofluoric concentration is 0.025mol/L;
(3) hydrothermal treatment consists: the platinized platinum in being walked by a tiltedly puts into autoclave, the mixing solutions got in step 2 moves into reactor inner bag, is then sealed by still; Autoclave is incubated 15h at 180 DEG C, naturally cools to room temperature, open reactor afterwards, solution in still evaporates by 70 DEG C of heating completely, bottom reactor He on platinized platinum, generate white powder;
(4) dry: taken out by the white powder bottom reactor and on platinized platinum, repeatedly rinse with deionized water, dry to obtain platinum oxide nano-powder, its particle diameter is 10-50nm.。
Embodiment 3
The preparation method of platinum oxide nano-powder:
(1) process in early stage of platinized platinum; Platinized platinum is carried out ultrasonic cleaning successively in deionized water, alcohol, acetone soln, dries up for subsequent use in air;
(2) in mixing solutions (20ml hydrogen peroxide (30wt%) and the 20ml deionized water) container filling hydrogen peroxide and deionized water, add hydrogen fluoride, abundant dissolving, is configured to mixing solutions, and in mixing solutions, hydrofluoric concentration is 0.025mol/L;
(3) hydrothermal treatment consists: the platinized platinum in being walked by a tiltedly puts into autoclave, the mixing solutions got in step 2 moves into reactor inner bag, is then sealed by still; Autoclave is incubated 15h at 220 DEG C, naturally cools to room temperature, open reactor afterwards, solution in still evaporates by 80 DEG C of heating completely, bottom reactor He on platinized platinum, generate white powder;
(4) dry: taken out by the white powder bottom reactor and on platinized platinum, repeatedly rinse with deionized water, dry to obtain platinum oxide nano-powder, its particle diameter is 10-50nm.
Above-described embodiment is illustrative principle of the present invention and effect thereof only, but not for limiting the present invention.Any person skilled in the art scholar all without prejudice under spirit of the present invention and category, can modify above-described embodiment or changes.Therefore, such as have in art usually know the knowledgeable do not depart from complete under disclosed spirit and technological thought all equivalence modify or change, must be contained by claim of the present invention.
Claims (6)
1. a preparation method for platinum oxide nano-powder, is characterized in that, described preparation method at least comprises the following steps:
(1) process in early stage of platinized platinum;
(2) mixing solutions is configured: in the container of mixing solutions filling hydrogen peroxide and deionized water, add hydrogen fluoride solution, fully dissolve, be configured to mixing solutions;
(3) hydrothermal treatment consists: the platinized platinum in being walked by a tiltedly puts into autoclave, the mixing solutions got in step 2 moves into reactor inner bag, is then sealed by still; Autoclave is incubated 15h at 150 DEG C-220 DEG C, naturally cools to room temperature, open reactor afterwards, heat and solution in still is evaporated completely, bottom reactor He on platinized platinum, generate white powder;
(4) dry: the white powder bottom reactor and on platinized platinum is taken out, repeatedly rinses with deionized water, dry to obtain platinum oxide nano-powder.
2. the preparation method of platinum oxide nano-powder according to claim 1, is characterized in that: the early stage of described platinized platinum is treated to carries out ultrasonic cleaning successively by platinized platinum in deionized water, alcohol, acetone soln, dries up for subsequent use in air.
3. the preparation method of platinum oxide nano-powder according to claim 1, is characterized in that: in step 2, the concentration of hydrogen peroxide is 30wt%, and the volume ratio of hydrogen peroxide and deionized water is 1:1.
4. the preparation method of platinum oxide nano-powder according to claim 1, is characterized in that: in mixing solutions described in step 2, hydrofluoric concentration is 0.025mol/L.
5. the preparation method of platinum oxide nano-powder according to claim 1, is characterized in that: in step 3, with the heating temperatures of 60-80 DEG C until solution evaporates completely.
6. the platinum oxide nano-powder prepared by method according to claim 1, is characterized in that: the particle diameter of platinum oxide nanometer powder is 10-50nm.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2019064931A1 (en) * | 2017-09-29 | 2019-04-04 | 日立Ｇｅニュークリア・エナジー株式会社 | Platinum oxide colloidal solution, platinum oxide colloidal solution production method, and platinum oxide colloidal solution injector device |
| CN110217835A (en) * | 2019-07-09 | 2019-09-10 | 中国科学院广州地球化学研究所 | A kind of PtO2The preparation method of tapered nano-particle material |
| CN114029051A (en) * | 2021-12-23 | 2022-02-11 | 浙江微通催化新材料有限公司 | Platinum dioxide catalyst and preparation method thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103265085A (en) * | 2013-06-04 | 2013-08-28 | 西安凯立化工有限公司 | Method for preparing platinum dioxide by adopting liquid phase process |
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103265085A (en) * | 2013-06-04 | 2013-08-28 | 西安凯立化工有限公司 | Method for preparing platinum dioxide by adopting liquid phase process |
Non-Patent Citations (3)
| Title |
|---|
| REZAEI-ZARCHI ET AL.: "Study of bactericidal properties of carbohydrate-stabilized platinum oxide nanoparticles", 《INTERNATIONAL NANO LETTERS》 * |
| 哈曜等: "高分子稳定的水溶性铂氧化物纳米颗粒的制备", 《中南民族大学学报(自然科学版)》 * |
| 陈益贤等: "高分子稳定的钯、铂氧化物水溶性纳米颗粒的制备与表征", 《中南民族大学学报(自然科学版)》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2019064931A1 (en) * | 2017-09-29 | 2019-04-04 | 日立Ｇｅニュークリア・エナジー株式会社 | Platinum oxide colloidal solution, platinum oxide colloidal solution production method, and platinum oxide colloidal solution injector device |
| CN110217835A (en) * | 2019-07-09 | 2019-09-10 | 中国科学院广州地球化学研究所 | A kind of PtO2The preparation method of tapered nano-particle material |
| CN110217835B (en) * | 2019-07-09 | 2020-08-07 | 中国科学院广州地球化学研究所 | PtO (PtO)2Preparation method of tapered nano-particle material |
| CN114029051A (en) * | 2021-12-23 | 2022-02-11 | 浙江微通催化新材料有限公司 | Platinum dioxide catalyst and preparation method thereof |
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