CN101862673A - New method for preparing loaded Ru2P under mild condition - Google Patents
New method for preparing loaded Ru2P under mild condition Download PDFInfo
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- CN101862673A CN101862673A CN 201010211175 CN201010211175A CN101862673A CN 101862673 A CN101862673 A CN 101862673A CN 201010211175 CN201010211175 CN 201010211175 CN 201010211175 A CN201010211175 A CN 201010211175A CN 101862673 A CN101862673 A CN 101862673A
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- support type
- precursor
- sodium hypophosphite
- ruthenium trichloride
- ru2p
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Abstract
The invention provides a new method for preparing loaded Ru2P by taking ruthenium trichloride as a precursor at a low temperature. The loaded Ru2P is successfully prepared by taking ruthenium trichloride and sodium hypophosphite as a fixed precursor. The preparation method has the characteristics of simpleness, safety, low required equipment cost, no need of flowing protective gas in the preparation process, no need of complex steps such as temperature programming and the like, and simple heat treatment required under normal pressure; and the loaded Ru2P can be used for hydrodesulfurization and hydrodenitrogeneration reactions of oil.
Description
Technical field
It is preceding body hypothermia preparation support type Ru down that the present invention proposes a kind of ruthenium trichloride that utilizes
2The new method of P.This method adopts ruthenium trichloride successfully to prepare support type Ru with sodium hypophosphite for mixing precursor
2P; Characteristics of the present invention are that the preparation method who is adopted is simple, safety, and the equipment needed thereby cost is low, does not need to use flowing protective gas in the preparation process, does not need complicated steps such as temperature programming, only needs simple heat treatment under the normal pressure.Gained support type Ru
2P can be used for the sharp hydrodenitrogeneration reaction of hydrodesulfurization of oil product.
Background technology
In recent years, petroleum resources day by day reduce in the world wide, and the heaviness of crude oil, inferiorization trend constantly enlarge.Develop profit efficiently and utilize existing petroleum resources, produce the clean fuel that disappears the sustainable development of various countries is all had the important strategic meaning.In current catalysis material research, the noble metal phosphide all has excellent catalytic performance in many hydrogen-involved reactions, caused people's extensive concern as new catalyst.Particularly, support type Ru
2The P catalyst all has very high catalytic activity in the sharp hydrodenitrogeneration reaction of the hydrodesulfurization of oil product.Therefore, carry out support type Ru
2The research of P catalyst all has the sharp potential application prospect of important significance for theories in the sharp material of catalysis field.
Youngster does not have bibliographical information support type Ru at present
2The P Preparation of catalysts.Traditional metal phosphide Preparation of catalysts method can not be synthesized support type Ru
2The P catalyst.Proposed the sharp ruthenium trichloride of employing sodium hypophosphite among the present invention and successfully prepared support type Ru for mixing precursor
2The P catalyst.The technology that it adopted is simple, Ru
2The P preparation temperature is low, and is with short production cycle, do not need to use flowing protective gas in the preparation process, do not need complicated steps such as temperature programming, only needs simple heat treatment under the normal pressure.
Summary of the invention
It is preceding body hypothermia preparation support type Ru down that the present invention proposes a kind of ruthenium trichloride that utilizes
2The new method of P.This method adopts ruthenium trichloride successfully to prepare support type Ru with sodium hypophosphite for mixing precursor
2P; Characteristics of the present invention are that the preparation method who is adopted is simple, safety, and the equipment needed thereby cost is low, does not need to use flowing protective gas in the preparation process, does not need complicated steps such as temperature programming, only needs simple heat treatment under the normal pressure.
Support type Ru
2The P synthesis step is as follows:
Under the stirring at room state, according to certain stoichiometric relationship, the sodium hypophosphite of aequum is dissolved in the deionized water, the ruthenium trichloride with aequum after the stirring and dissolving joins in the solution, fully stirs after 1 hour required carrier joined in the solution to flood.Flood and after 1 hour it is dried at a certain temperature, the precursor after will drying is then pulverized in the last tubular reactor of packing into, in the nitrogen protection atmosphere of static state with precursor temperature required roasting down 1 hour.At last products therefrom washing back oven dry is promptly obtained required support type Ru
2P.
Stoichiometric relationship described in the synthesis step is Ru
3+: H
2PO
2 -In 1: 5～1: 7 scope; Described ruthenium trichloride is to analyze pure three hydrate ruthenium trichlorides; Described sodium hypophosphite is to analyze pure sodium hypophosphite; The bake out temperature of precursor solution is 100～120 ℃; The precursor sintering temperature is 500～600 ℃.
Description of drawings
Accompanying drawing 1 is the support type Ru that is synthesized
2The x-ray diffractogram of powder of P sample A.
Accompanying drawing 2 is the support type Ru that synthesized
2The x-ray diffractogram of powder of P sample B.
Accompanying drawing 3 is the support type Ru that synthesized
2The x-ray diffractogram of powder of P sample C.
The specific embodiment
The present invention can describe in detail by embodiment, but they are not that the present invention is done any restriction.In these embodiments, XRD spectra is measured by Japan's D/MAX-2500 type of science x-ray diffractometer, and pipe is pressed 40kV, pipe stream 100mA, 8 °/min of sweep speed.
These embodiment have illustrated support type Ru
2The building-up process of P.
Embodiment 1
At first under the stirring at room state with the sodium hypophosphite (NaH of 0.529g
2PO
2.H
2O) join in the 3.9mL deionized water, add the RuCl of 0.258g after the dissolving 10min
33H
2O.Continue to stir after 1 hour, the MCM-41 molecular sieve of 1g is joined in the above-mentioned solution flood.Flood after 1 hour it 100 ℃ of oven dry down, the precursor after will drying is then pulverized in the last tubular reactor of packing into, in the nitrogen protection atmosphere of static state with precursor 500 ℃ of roastings 1 hour.With products therefrom washing back oven dry, the gained sample is named as A at last, and A has the feature of accompanying drawing 1.
Embodiment 2
Preparation process is identical with the preparation process of sample A, only changes NaH
2PO
2.H
2The amount of O is 0.741g, and other condition is constant.The gained sample is named as B, and B has the feature of accompanying drawing 2.
Embodiment 3
Preparation process is identical with the preparation process of sample A, and only changing the precursor sintering temperature is 600 ℃, and other condition is constant.The gained sample is named as C, and C has the feature of accompanying drawing 3.
Claims (7)
- The present invention propose a kind of utilize ruthenium trichloride to be before the following preparation support type Ru of body hypothermia 2The new method of P.This method adopts ruthenium trichloride successfully to prepare support type Ru with sodium hypophosphite for mixing precursor 2P; Characteristics of the present invention are that the preparation method who is adopted is simple, safety.Gained support type Ru 2P can be used for the hydrodesulfurization and the hydrodenitrogeneration reaction of oil product.Support type Ru 2The P synthesis step is as follows:Under the stirring at room state, according to certain stoichiometric relationship, the sodium hypophosphite of aequum is dissolved in the deionized water, the ruthenium trichloride with aequum after the stirring and dissolving joins in the solution, fully stirs after 1 hour required carrier joined in the solution to flood.Flood and after 1 hour it is dried at a certain temperature, the precursor after will drying is then pulverized in the last tubular reactor of packing into, in the nitrogen protection atmosphere of static state with precursor temperature required roasting down 1 hour.At last products therefrom washing back oven dry is promptly obtained required support type Ru 2P.
- 2. according in the described stoichiometric relationship of claim 1, Ru 3+: H 2PO 2 -In 1: 5～1: 7 scope.
- 3. be to analyze pure three hydrate ruthenium trichlorides according to the described ruthenium trichloride of claim 1.
- 4. be to analyze pure sodium hypophosphite according to the described sodium hypophosphite of claim 1.
- 5. the bake out temperature according to the described precursor solution of claim 1 is 100～120 ℃.
- 6. it is 500～600 ℃ according to the described precursor sintering temperature of claim 1.
- 7. be support type Ru according to the synthetic product of claim 1 2P.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010102111759A CN101862673B (en) | 2010-06-28 | 2010-06-28 | New method for preparing loaded Ru2P under mild condition |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010102111759A CN101862673B (en) | 2010-06-28 | 2010-06-28 | New method for preparing loaded Ru2P under mild condition |
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| Publication Number | Publication Date |
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| CN101862673A true CN101862673A (en) | 2010-10-20 |
| CN101862673B CN101862673B (en) | 2012-06-27 |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110639567A (en) * | 2019-10-10 | 2020-01-03 | 浙江工业大学 | Carbon-supported ruthenium phosphide nanocluster bifunctional catalyst and preparation method and application thereof |
| CN110860301A (en) * | 2019-11-26 | 2020-03-06 | 中国科学技术大学 | Ruthenium phosphide-loaded carbon micron sheet dual-functional electrocatalyst, preparation method thereof and application of dual-functional electrocatalyst in efficient electrolytic hydrogen production |
| CN113410472A (en) * | 2021-06-03 | 2021-09-17 | 扬州大学 | Alcohol fuel cell anode catalyst and preparation method thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101584990A (en) * | 2009-06-19 | 2009-11-25 | 上海师范大学 | Ru-P nano hollow ball catalyst in amorphous state as well as preparation and application thereof |
-
2010
- 2010-06-28 CN CN2010102111759A patent/CN101862673B/en active Active
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101584990A (en) * | 2009-06-19 | 2009-11-25 | 上海师范大学 | Ru-P nano hollow ball catalyst in amorphous state as well as preparation and application thereof |
Non-Patent Citations (1)
| Title |
|---|
| 《Journal of Catalysis》 20090224 Qingxin Guan et al. Alternative synthesis of bulk and supported nickel phosphide from the thermal decomposition of hypophosphites 1-3 1-7 第263卷, 2 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110639567A (en) * | 2019-10-10 | 2020-01-03 | 浙江工业大学 | Carbon-supported ruthenium phosphide nanocluster bifunctional catalyst and preparation method and application thereof |
| CN110860301A (en) * | 2019-11-26 | 2020-03-06 | 中国科学技术大学 | Ruthenium phosphide-loaded carbon micron sheet dual-functional electrocatalyst, preparation method thereof and application of dual-functional electrocatalyst in efficient electrolytic hydrogen production |
| CN113410472A (en) * | 2021-06-03 | 2021-09-17 | 扬州大学 | Alcohol fuel cell anode catalyst and preparation method thereof |
| CN113410472B (en) * | 2021-06-03 | 2024-05-07 | 扬州大学 | Anode catalyst of alcohol fuel cell and preparation method thereof |
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| Publication number | Publication date |
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| CN101862673B (en) | 2012-06-27 |
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