CN104174418A - Method for synthesizing nickel phosphide catalyst with high hydrodesulfurization activity based on nickel sulfide - Google Patents
Method for synthesizing nickel phosphide catalyst with high hydrodesulfurization activity based on nickel sulfide Download PDFInfo
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- CN104174418A CN104174418A CN201410458161.5A CN201410458161A CN104174418A CN 104174418 A CN104174418 A CN 104174418A CN 201410458161 A CN201410458161 A CN 201410458161A CN 104174418 A CN104174418 A CN 104174418A
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- nickel
- nickel sulfide
- nickel phosphide
- phosphide
- sulfide
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Abstract
The invention relates to an in-situ synthesis method of nickel phosphide and belongs to the technical field of inorganic material preparation processes. According to the in-situ synthesis method of the nickel phosphide, a mechanical mixture of nickel sulfide and sodium hypophosphite is taken as a precursor; the nickel phosphide is formed by using reaction of nickel ions and hydrogen phosphide; meanwhile, generated hydrogen sulfide can be used for building an active phase of NiPS on the surface of the nickel phosphide. The in-situ synthesis method of the nickel phosphide is simple to operate, good in process repeatability, stable in quality of products and suitable for large-scale production.
Description
Technical field
The invention belongs to inorganic material preparation process technical field, relate to the preparation method of inorganic material, specifically the synthetic method of high activity nickel phosphide.Can be applicable to the aspects such as hydrodesulfurization catalysis material.
Background technology
In recent years, nickel phosphide as outstanding Hydrobon catalyst by scholars' extensive concern.Recently, scholars study discovery, why active high nickel phosphide is in hydrodesulfurization reaction, and the reason that the life-span is lasting, the hydrogen sulfide that is exactly hydrodesulfurization reaction generation can make nickel phosphide surface form this material of NiPS, and further this NiPS of research discovery is likely the active phase of hydrodesulfurization reaction.Therefore, we taking sulfide as raw material, utilize preparing the hydrogen sulfide in-situ treatment nickel phosphide producing in nickel phosphide process on original basis of walking altogether, thereby form the active phase of NiPS at its surface in situ, and then significantly improve the hydrodesulfurization activity of nickel phosphide.
Summary of the invention
Meaning of the present invention is to provide a kind of synthetic method of high activity nickel phosphide, and this method can, in forming nickel phosphide, build the active phase of NiPS at its surface in situ, thereby significantly improve the activity of the hydrodesulfurization of nickel phosphide.And have simple to operately, the reaction time is of short duration, and reaction temperature is lower, good process repeatability, the advantage of constant product quality.
Pure nickel phosphide synthesis step is as follows:
A certain amount of nickel sulfide powder and sodium hypophosphite are mixed, then said mixture is packed in little porcelain boat, put into tube furnace, pass into nitrogen as protective gas, be then directly warmed up to after 350 DEG C heat treatment 120 minutes.Under inert gas shielding, furnace is down to room temperature after completion of the reaction, with the nitrogen passivation that contains 1% oxygen 3 hours, the catalyst obtaining was for subsequent use.
The synthesis step of support type nickel phosphide is as follows:
A certain amount of nickel chloride is dissolved in a certain amount of water, then adds a certain amount of carrier, impregnated carrier is after 3 hours, add a certain amount of vulcanized sodium, then continue to stir after 3 hours, the precipitation obtaining is filtered, be dried, grind, finally obtain the nickel sulfide powder of load.Then repeat the synthesis step of pure nickel phosphide.Carrier is silica, molecular sieve, alundum (Al2O3) etc.
Specific embodiments
Embodiment 1
By after 1 gram of nickel sulfide and the mixing of 0.68g sodium hypophosphite, put into tube furnace, be directly warmed up to 350 DEG C, keep, after 120 minutes, dropping to room temperature, with the nitrogen passivation that contains 1% oxygen 3 hours, the catalyst obtaining was for subsequent use.
Embodiment 2
By 1gNiS/SiO
2mix with 1.01g sodium hypophosphite,, put into tube furnace, be directly warmed up to 350 DEG C, keep, after 120 minutes, dropping to room temperature, with the nitrogen passivation that contains 1% oxygen 3 hours, the catalyst obtaining was for subsequent use.
Claims (1)
1. the method for preparing high activity nickel sulfide based on nickel sulfide, is characterized in that comprising the steps:
A certain amount of nickel sulfide powder and sodium hypophosphite are mixed, then said mixture is packed in little porcelain boat, put into tube furnace, pass into nitrogen as protective gas, be then directly warmed up to after 350 DEG C heat treatment 120 minutes.Under inert gas shielding, furnace is down to room temperature after completion of the reaction, with the nitrogen passivation that contains 1% oxygen 3 hours, the catalyst obtaining was for subsequent use.If nickel sulfide is replaced to the nickel sulfide of support type, can obtain the nickel phosphide of support type.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410458161.5A CN104174418A (en) | 2014-09-10 | 2014-09-10 | Method for synthesizing nickel phosphide catalyst with high hydrodesulfurization activity based on nickel sulfide |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201410458161.5A CN104174418A (en) | 2014-09-10 | 2014-09-10 | Method for synthesizing nickel phosphide catalyst with high hydrodesulfurization activity based on nickel sulfide |
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| CN104174418A true CN104174418A (en) | 2014-12-03 |
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| CN201410458161.5A Pending CN104174418A (en) | 2014-09-10 | 2014-09-10 | Method for synthesizing nickel phosphide catalyst with high hydrodesulfurization activity based on nickel sulfide |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108380228A (en) * | 2018-02-12 | 2018-08-10 | 华东理工大学 | A kind of preparation method and applications of nickel sulfide/nickel phosphide of 1 dimension/1 dimension nanometer construction assembling |
| CN110538667A (en) * | 2019-08-28 | 2019-12-06 | 天津科技大学 | Preparation method of transition metal phosphorus sulfide active phase |
| CN110876949A (en) * | 2019-11-27 | 2020-03-13 | 西安交通大学 | Ni for total hydrolysis2P/NiS @ C heterojunction photocatalyst and preparation method thereof |
-
2014
- 2014-09-10 CN CN201410458161.5A patent/CN104174418A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108380228A (en) * | 2018-02-12 | 2018-08-10 | 华东理工大学 | A kind of preparation method and applications of nickel sulfide/nickel phosphide of 1 dimension/1 dimension nanometer construction assembling |
| CN110538667A (en) * | 2019-08-28 | 2019-12-06 | 天津科技大学 | Preparation method of transition metal phosphorus sulfide active phase |
| CN110538667B (en) * | 2019-08-28 | 2022-04-05 | 天津科技大学 | Preparation method of transition metal phosphorus sulfide active phase |
| CN110876949A (en) * | 2019-11-27 | 2020-03-13 | 西安交通大学 | Ni for total hydrolysis2P/NiS @ C heterojunction photocatalyst and preparation method thereof |
| CN110876949B (en) * | 2019-11-27 | 2021-05-28 | 西安交通大学 | Ni for total hydrolysis2P/NiS @ C heterojunction photocatalyst and preparation method thereof |
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| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20141203 |
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| WD01 | Invention patent application deemed withdrawn after publication |