CN102172536A - Method for preparing loaded phosphide catalyst by taking red phosphorus as phosphorus source - Google Patents
Method for preparing loaded phosphide catalyst by taking red phosphorus as phosphorus source Download PDFInfo
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- CN102172536A CN102172536A CN 201110063142 CN201110063142A CN102172536A CN 102172536 A CN102172536 A CN 102172536A CN 201110063142 CN201110063142 CN 201110063142 CN 201110063142 A CN201110063142 A CN 201110063142A CN 102172536 A CN102172536 A CN 102172536A
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Abstract
The invention relates to a method for preparing a phosphide catalyst by directly heating and thermally treating a mechanical mixture of red phosphorus and a loaded metal or metal salt, belonging to the technical field of a preparation process of an inorganic nanomaterial and relating to a method for preparing a corresponding phosphide catalyst by taking the mechanical mixture of the red phosphorus and the loaded metal or metal salt as a precursor and making liquid phosphorus react with a metal or metal salt. By adopting the method, different phosphide catalysts can be prepared by adjusting the types of metals or metal salts. The method is a universal preparation method of the loaded phosphide catalyst.
Description
Technical field
The invention belongs to the inorganic nano material preparation process technology field, relate to the preparation method of inorganic nano material, the mechanical impurity with red phosphorus and load type metal or slaine is the new method of precursor preparation phosphide catalyst specifically.The hydrodesulfurization and denitrogenation, the hydrazine hydrate that can be applicable to oil product decompose the catalysis material of aspects such as preparation nitrogen and hydrogen.
Background technology
At present, the report for the preparation method of transition metal phosphide catalyst has had a lot.The preparation method of phosphide catalyst mainly comprises: it is precursor with the metal orthophosphates that report was just arranged as far back as 1958, the method for preparing transition metal phosphide catalyst by temperature programmed reduction, this method to later report in 1996 increase gradually, be a kind of widely accepted preparation method; Cecilia, people such as J.A. have reported the method for preparing nickel phosphide and phosphatization Co catalysts by the hydrogen reducing phosphite; Wang Zhi waits the people to report the method for the compound precursor preparation catalyst of phosphatizing nickel of heat treatment triphenylphosphine under hydrogen atmosphere by force; People such as Guan Qingxin have reported with the nickelous hypophosphite to be the method for precursor preparation catalyst of phosphatizing nickel; Robinson, people such as W.R.A.M. prepare the method for catalyst of phosphatizing nickel by thermal decomposition D2EHDTPA nickel; People such as Wang Anjie handle the method for nickel oxide and phosphorus pentoxide precursor preparation nickel phosphide by hydrogen plasma; Yang, people such as S. prepare the method for catalyst of phosphatizing nickel by the mist reducing metal simple substance of hydrogen phosphide and hydrogen.
The present invention is a precursor with the mechanical impurity of red phosphorus and load type metal or slaine, and a kind of pervasive support type phosphide catalyst novel preparation method is provided.
Summary of the invention
Meaning of the present invention is to provide a kind of synthetic method of support type phosphide catalyst, and the precursor preparation of this method is very simple, only need analytically pure red phosphorus and load type metal or slaine mechanically be mixed with key.Handling safety is simple, and phosphide degree of crystallinity is very high, good reproducibility.
Characteristics of the present invention are to provide a kind of novel preparation method of support type phosphide catalyst.
Synthesis step is as follows:
A certain amount of carrier was stirred dipping 3 hours in a certain amount of aqueous metal salt, then with the carrier suction filtration, filter cake obtained corresponding load type metal salt precursor in 3 hours 60 ℃ of vacuum drying.Perhaps with load type metal salt precursor at a certain temperature the hydrogen reducing certain hour obtain the load type metal precursor.A certain amount of precursor and red phosphorus are put into tube furnace according to certain mol proportion, feed nitrogen, be warmed up to uniform temperature after, the heat treatment certain hour.After reaction finishes furnace is reduced to room temperature, obtain corresponding phosphide catalyst.Above-mentioned slaine or metal are any slaine or metal or their mixture in the periodic table.Carrier is alundum (Al, silica, molecular sieve, graphite, active carbon, titanium dioxide, zirconium dioxide.
Specific embodiments
Embodiment 1
Is that 2: 1 usefulness key mechanicals mix with red phosphorus and silicon dioxide carried nickel chloride by phosphorus nickel mol ratio; pack into then in the little porcelain boat; put into tube furnace; flow velocity with 10ml/min feeds nitrogen; directly be warming up to 700 ℃ then; reaction is 30 hours under this temperature, and the back drops to room temperature in nitrogen protection, obtains silicon dioxide carried nickel phosphide.
Embodiment 2
Nickel chloride in the embodiment 1 is become cobalt chloride, and other condition is constant, obtains silicon dioxide carried phosphatization cobalt.
Embodiment 3
Nickel chloride in the embodiment 1 is become frerrous chloride, and other condition is constant, obtains silicon dioxide carried iron phosphide.
Embodiment 4
Nickel chloride in the embodiment 1 is become copper chloride, and other condition is constant, obtains silicon dioxide carried phosphorized copper.
Embodiment 5
Carrier in the embodiment 1 is become MCM41, and other condition is constant.
Embodiment 6
Temperature in the embodiment 1 is become alundum (Al, and other condition is constant.
Embodiment 7
Temperature in the embodiment 1 is become 750 ℃, and other condition is constant.
Embodiment 8
Temperature in the embodiment 1 is become 800 ℃, and other condition is constant.
Embodiment 9
Phosphorus nickel mol ratio in the embodiment 1 is become 1: 1, and other condition is constant.
Embodiment 10
Phosphorus nickel mol ratio in the embodiment 1 is become 3: 1, and other condition is constant.
Embodiment 11
Phosphorus nickel mol ratio in the embodiment 1 is become 1: 2, and other condition is constant.
Embodiment 11
Nickel chloride in the embodiment 1 is become metallic nickel, and other condition is constant.
Claims (3)
1. a method for preparing the support type phosphide catalyst with red phosphorus for the phosphorus source is characterized in that comprising the steps:
A certain amount of carrier was stirred dipping 3 hours in a certain amount of aqueous metal salt, then with the carrier suction filtration, filter cake obtained corresponding load type metal salt precursor in 3 hours 60 ℃ of vacuum drying; Perhaps with load type metal salt precursor at a certain temperature the hydrogen reducing certain hour obtain the load type metal precursor; A certain amount of precursor and red phosphorus are put into tube furnace according to certain mol proportion, feed nitrogen, be warmed up to uniform temperature after, the heat treatment certain hour; After reaction finishes furnace is reduced to room temperature, obtain corresponding phosphide catalyst;
2. according to a kind of method for preparing the support type phosphide catalyst with red phosphorus for the phosphorus source of claim 1, it is characterized in that described slaine or metal are any slaine or metal or their mixture in the periodic table;
3. according to a kind of method for preparing the support type phosphide catalyst with red phosphorus for the phosphorus source of claim 1, it is characterized in that described carrier is alundum (Al, silica, molecular sieve, graphite, active carbon, titanium dioxide, zirconium dioxide.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN 201110063142 CN102172536A (en) | 2011-03-16 | 2011-03-16 | Method for preparing loaded phosphide catalyst by taking red phosphorus as phosphorus source |
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| Application Number | Priority Date | Filing Date | Title |
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| CN 201110063142 CN102172536A (en) | 2011-03-16 | 2011-03-16 | Method for preparing loaded phosphide catalyst by taking red phosphorus as phosphorus source |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105688958A (en) * | 2016-01-15 | 2016-06-22 | 复旦大学 | Polyhedron cobalt phosphide/graphite carbon hybrid material and preparing method and application thereof |
| CN106279930A (en) * | 2016-09-12 | 2017-01-04 | 山东理工大学 | The preparation method of chabasie red phosphorus synergistic fire retardant |
| CN108160092A (en) * | 2017-10-09 | 2018-06-15 | 江苏大学 | A kind of compound Electrocatalytic Activity for Hydrogen Evolution Reaction agent of nano-particle/carbon black and preparation method thereof |
Citations (5)
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| CN1124759A (en) * | 1994-11-09 | 1996-06-19 | 中国石油化工总公司抚顺石油化工研究院 | Hydrogen refining catalyst |
| CN1330982A (en) * | 2000-07-05 | 2002-01-16 | 中国石油化工股份有限公司 | P-contained Y-zeolite and its preparing process |
| US20060246217A1 (en) * | 2005-03-18 | 2006-11-02 | Weidman Timothy W | Electroless deposition process on a silicide contact |
| CN101376108A (en) * | 2007-08-29 | 2009-03-04 | 中国科学院大连化学物理研究所 | Nickel phosphide catalyst as well as preparation method and application |
| CN101391223A (en) * | 2007-09-19 | 2009-03-25 | 中国科学院大连化学物理研究所 | Preparation method of no-loaded nickel phosphide catalyst |
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2011
- 2011-03-16 CN CN 201110063142 patent/CN102172536A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1124759A (en) * | 1994-11-09 | 1996-06-19 | 中国石油化工总公司抚顺石油化工研究院 | Hydrogen refining catalyst |
| CN1330982A (en) * | 2000-07-05 | 2002-01-16 | 中国石油化工股份有限公司 | P-contained Y-zeolite and its preparing process |
| US20060246217A1 (en) * | 2005-03-18 | 2006-11-02 | Weidman Timothy W | Electroless deposition process on a silicide contact |
| CN101376108A (en) * | 2007-08-29 | 2009-03-04 | 中国科学院大连化学物理研究所 | Nickel phosphide catalyst as well as preparation method and application |
| CN101391223A (en) * | 2007-09-19 | 2009-03-25 | 中国科学院大连化学物理研究所 | Preparation method of no-loaded nickel phosphide catalyst |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105688958A (en) * | 2016-01-15 | 2016-06-22 | 复旦大学 | Polyhedron cobalt phosphide/graphite carbon hybrid material and preparing method and application thereof |
| CN105688958B (en) * | 2016-01-15 | 2019-01-15 | 复旦大学 | Polyhedron shape phosphatization cobalt/graphitic carbon hybrid material and its preparation method and application |
| CN106279930A (en) * | 2016-09-12 | 2017-01-04 | 山东理工大学 | The preparation method of chabasie red phosphorus synergistic fire retardant |
| CN106279930B (en) * | 2016-09-12 | 2018-07-17 | 山东理工大学 | The preparation method of chabasie-red phosphorus synergistic fire retardant |
| CN108160092A (en) * | 2017-10-09 | 2018-06-15 | 江苏大学 | A kind of compound Electrocatalytic Activity for Hydrogen Evolution Reaction agent of nano-particle/carbon black and preparation method thereof |
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Application publication date: 20110907 |