CN105060353B - The preparation method that the sub-nickel of a kind of orthorhombic system sulfuration is nanocrystalline - Google Patents
The preparation method that the sub-nickel of a kind of orthorhombic system sulfuration is nanocrystalline Download PDFInfo
- Publication number
- CN105060353B CN105060353B CN201510416492.7A CN201510416492A CN105060353B CN 105060353 B CN105060353 B CN 105060353B CN 201510416492 A CN201510416492 A CN 201510416492A CN 105060353 B CN105060353 B CN 105060353B
- Authority
- CN
- China
- Prior art keywords
- nickel
- preparation
- nanocrystalline
- sub
- orthorhombic system
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention discloses a kind of sub-nickel of orthorhombic system sulfuration9S8Nanocrystalline preparation method, belongs to Syntheses method and technology field.The method comprises the following steps: (1) is by biphase thing reacting by heating in closed reactor of oil reservoir that water layer that lower floor is containing inorganic nickel compound, upper strata are aliphatic mercaptan, make the aliphatic mercaptan in oil reservoir react at oil-water interfaces with the nickel ion in water layer, obtain reactant liquor；(2) above-mentioned reactant liquor is cooled to room temperature, is added thereto to precipitant, after precipitation to be precipitated, separate that to be dried to obtain the orthorhombic system sub-nickel of sulfuration nanocrystalline.The preparation method of the present invention uses two phase process to prepare the sub-nickel of orthorhombic system sulfuration9S8Nanocrystalline, the cheaper starting materials used is easy to get, apparatus and process is simple, reaction condition is gentle, simple and safe operation and reproducible, has good development and application prospect.
Description
Technical field
The invention belongs to Syntheses method field, be specifically related to a kind of sub-nickel of orthorhombic system sulfuration9S8Nanocrystalline preparation side
Method.
Background technology
Sulfide nanocrystalline has many important physicochemical properties, be widely used in optics, catalysis, magnetics, sensing,
The fields such as medical treatment, lubrication and battery.Currently for nanocrystalline most of research work all concentrate on CdSe, CdS, PbS and
The synthesis of the semiconductor nanos such as PbSe, optical characteristics and photoelectric device and biomarker aspect.The sulfide of nickel is as transition
Metal sulfide, is important inorganic functional material, has stronger microwave absorption usefulness and the strongest magnetothermal effect.The sulfur of nickel
Compound comprises multiple phase: Ni3S2、Ni3+xS、Ni4S3+x、Ni6S5、Ni7S6、Ni9S8、Ni3S4With NiS etc..At present, the sulfuration of nickel
The nanocrystalline usual employing hydro-thermal method of thing, solvent-thermal method and solvent method are prepared, and such as Qian Yitai group and Xie Yi group, utilize water
Full-boiled process prepares the sulfide nanocrystalline of the nickel of different-shape.Cu2The synthesis of S nanocrystal is more universal, and such as Korgel et al. leads to
Crossing two phase process uses collochemistry mode to synthesize monodispersed Cu2S nanocrystal, the method is easy, the Cu prepared2The nanocrystalline bodily form of S
Looks are neat.But seldom there is document report to prepare the sub-nickel (Ni of orthorhombic system sulfuration by two phase process9S8) nanocrystalline.By easy and simple to handle,
The simple two phase process of equipment requirements, uses the raw material of wide material sources to prepare the sub-nickel (Ni of orthorhombic system sulfuration9S8) nanocrystalline have very
Important theory significance and practical value.
Summary of the invention
It is an object of the invention to provide one utilizes two phase process to prepare the sub-nickel (Ni of orthorhombic system sulfuration9S8) nanocrystalline method, the party
Method need not equipment and reaction condition, the simple and safe operation of harshness, and cheaper starting materials is easy to get.
The present invention relates to a kind of sub-nickel of orthorhombic system sulfuration9S8Nanocrystalline preparation method, it comprises the following steps:
(1) by lower floor be the water layer containing inorganic nickel compound, upper strata be that the biphase thing of the oil reservoir of aliphatic mercaptan is in closed reactor
Reacting by heating, makes the aliphatic mercaptan in oil reservoir react at oil-water interfaces with the nickel ion in water layer, obtains reactant liquor；
(2) above-mentioned reactant liquor is cooled to room temperature, is added thereto to precipitant, separate after precipitation to be precipitated and be dried to obtain orthorhombic system sulfur
Change sub-nickel nanocrystalline.
The described orthorhombic system sulfuration for preparing is sub-, and nickel is nanocrystalline has non-uniform topographical, wherein said aliphatic mercaptan simultaneously as sulfur source,
Part and Reduction Body.Preferably, the precipitation of precipitation through ageing after again by being centrifugally separating to obtain target product.
In a preferred embodiment of the present invention, described aliphatic mercaptan is the one in spicy thioalcohol, lauryl mercaptan or stearylmercaptan.
In a preferred embodiment of the present invention, described inorganic nickel compound is the one in nickel sulfate, nickel nitrate and nickel acetate.
In a preferred embodiment of the present invention, in step (1), reaction temperature is 180～220 DEG C.
In a preferred embodiment of the present invention, in step (1), the response time is 5～40h.
In a preferred embodiment of the present invention, described in described biphase thing, the volume ratio of water layer and described oil reservoir is (2-20): 1.
In a preferred embodiment of the present invention, the molar concentration of described inorganic nickel compound is 0.5-1mol/L.
In a preferred embodiment of the present invention, the one during described precipitant is ethanol, isopropanol or acetone.Described precipitant
Can also is that other polar substancess.
In a preferred embodiment of the present invention, it also includes the process of the described precipitation chloroform obtained.Chloroform
Purpose be that the aliphatic mercaptan organic ligand that will be attached to precipitation surface dissolves, obtain purer target product.Washing
Product after purification is obtained by precipitant precipitation again after washing.As required, can be with the step of repeated washing-precipitation-washing, repeatedly
It is purified.
Relative to prior art, the present invention achieves following beneficial effect:
The preparation method of the present invention can be prepared by the sub-nickel of orthorhombic system sulfuration by single step reaction9S8Nanocrystalline, need not make in advance
Standby presoma, select the inorganic nickel compound of wide material sources as nickel presoma, select aliphatic mercaptan as the presoma of sulfur,
Aliphatic mercaptan is also used as part and the reducing agent of nanocrystal surface simultaneously, directly heats reaction and can be obtained by vulcanizing sub-nickel
(Ni9S8) nanocrystalline.The preparation method of the present invention uses two phase process, and the cheaper starting materials used is easy to get, apparatus and process letter
Single, reaction condition gentle, simple and safe operation and reproducible, has good development and application prospect.
Accompanying drawing explanation
Fig. 1 is the sulfuration Asia nickel (Ni obtained in embodiment 19S8) nanocrystalline X-ray powder diffraction pattern.
Fig. 2 is the sulfuration Asia nickel (Ni obtained in embodiment 19S8) nanocrystalline transmission electron microscope photo.
Detailed description of the invention
Below in conjunction with Figure of description and specific embodiment, it is described in further detail the present invention.Embodiment is only used for illustrating
The bright present invention, is not used in the restriction present invention.
Embodiment 1
In 50 milliliters of flasks, add 20 ml deionized water and 1 mM of nickel nitrate, magnetic agitation 20 minutes, move to 50
After milliliter inner liner of reaction kettle, add 1 milliliter of lauryl mercaptan.After reactor is airtight, in electric drying oven with forced convection at 190 DEG C
React 20 hours.Naturally cool to room temperature after completion of the reaction, in reactant liquor, add ethanol precipitate, through being aged and centrifugal
After separation, gained sample vacuum drying oven at 70 DEG C will be vacuum dried 6 hours, obtain the sub-nickel nanometer of orthorhombic system sulfuration
Crystalline flour end.
Fig. 1 and Fig. 2 is the sulfuration Asia nickel (Ni prepared by this example respectively9S8) nanocrystalline X-ray powder diffraction pattern and transmission electricity
Mirror photo.Fig. 1 is compareed with standard card visible product there is the sub-nickel characteristic peak of sulfuration.Product has all as seen from Figure 2
Even pattern.
Embodiment 2
In 50 milliliters of flasks, add 20 ml deionized water and 1 mM of nickel nitrate, magnetic agitation 20 minutes, move to 50
After milliliter inner liner of reaction kettle, adding 5 milliliters of lauryl mercaptans, remaining operation is all with embodiment 1.
Embodiment 3
In 50 milliliters of flasks, add 20 ml deionized water and 1 mM of nickel nitrate, magnetic agitation 20 minutes, move to 50
After milliliter inner liner of reaction kettle, adding 2 milliliters of spicy thioalcohols, react 10 hours at 200 DEG C, remaining operation is all with embodiment 1.
Embodiment 4
In 50 milliliters of flasks, add 20 ml deionized water and 0.5mmol nickel sulfate, magnetic agitation 20 minutes, move to 50
After milliliter inner liner of reaction kettle, adding 5 milliliters of stearylmercaptans, react 10 hours, remaining operation is all with embodiment 1.
Embodiment 5
In 50 milliliters of flasks, add 20 ml deionized water and 0.5mmol nickel nitrate, magnetic agitation 20 minutes, move to 50
After milliliter inner liner of reaction kettle, adding 2 milliliters of lauryl mercaptans, remaining operation is all with embodiment 1.
Claims (7)
1. the sub-nickel of orthorhombic system sulfuration9S8Nanocrystalline preparation method, it is characterised in that it comprises the following steps:
(1) by lower floor be the water layer containing inorganic nickel compound, upper strata be that the biphase thing of the oil reservoir of aliphatic mercaptan is in closed reactor
Reacting by heating, reaction temperature is 180～220 DEG C, and the response time is 5～40h, makes in the aliphatic mercaptan in oil reservoir and water layer
Nickel ion reacts at oil-water interfaces, obtains reactant liquor；
(2) above-mentioned reactant liquor is cooled to room temperature, is added thereto to precipitant, separate after precipitation to be precipitated and be dried to obtain orthorhombic system sulfur
Change sub-nickel9S8Nanocrystalline.
Preparation method the most according to claim 1, it is characterised in that described aliphatic mercaptan is spicy thioalcohol, lauryl mercaptan or ten
One in eight mercaptan.
Preparation method the most according to claim 1, it is characterised in that described inorganic nickel compound is nickel sulfate, nickel nitrate and vinegar
One in acid nickel.
Preparation method the most according to claim 1, it is characterised in that water layer and the body of described oil reservoir described in described biphase thing
Long-pending ratio is (2-20): 1.
Preparation method the most according to claim 1, it is characterised in that the molar concentration of described inorganic nickel compound is
0.5-1mol/L。
Preparation method the most according to claim 1, it is characterised in that described precipitant is in ethanol, isopropanol or acetone
Kind.
Preparation method the most according to claim 1, it is characterised in that it also includes the described precipitation chloroform that obtains
Process.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510416492.7A CN105060353B (en) | 2015-07-15 | 2015-07-15 | The preparation method that the sub-nickel of a kind of orthorhombic system sulfuration is nanocrystalline |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510416492.7A CN105060353B (en) | 2015-07-15 | 2015-07-15 | The preparation method that the sub-nickel of a kind of orthorhombic system sulfuration is nanocrystalline |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN105060353A CN105060353A (en) | 2015-11-18 |
| CN105060353B true CN105060353B (en) | 2016-08-24 |
Family
ID=54489944
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510416492.7A Active CN105060353B (en) | 2015-07-15 | 2015-07-15 | The preparation method that the sub-nickel of a kind of orthorhombic system sulfuration is nanocrystalline |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105060353B (en) |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1526648A (en) * | 2003-09-19 | 2004-09-08 | 中国科学院上海硅酸盐研究所 | A wet chemical preparation method of low-dimensional nickel sulfide nanocrystals |
| CN102198960A (en) * | 2011-05-12 | 2011-09-28 | 南京师范大学 | Method for synthesizing nickel sulfide nanorods through solid-liquid phase reaction and prepared nanorods |
-
2015
- 2015-07-15 CN CN201510416492.7A patent/CN105060353B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1526648A (en) * | 2003-09-19 | 2004-09-08 | 中国科学院上海硅酸盐研究所 | A wet chemical preparation method of low-dimensional nickel sulfide nanocrystals |
| CN102198960A (en) * | 2011-05-12 | 2011-09-28 | 南京师范大学 | Method for synthesizing nickel sulfide nanorods through solid-liquid phase reaction and prepared nanorods |
Non-Patent Citations (2)
| Title |
|---|
| Synthesis of NiS and MnS Nanocrystals from the Molecular Precursors (TMEDA)M(SC{O}C6H5)2 (M ) Ni, Mn);Lu Tian等;《Crystal Growth & Design》;20091120;第9卷(第1期);摘要 * |
| 四硫富瓦烯四硫醇盐对纳米硫化物表面的修饰;杨巍等;《无机化学学报》;20030228;第19卷(第2期);摘要 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN105060353A (en) | 2015-11-18 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Hosseinpour-Mashkani et al. | Silver and silver oxide nanoparticles: Synthesis and characterization by thermal decomposition | |
| CN106753358B (en) | A kind of double transmitting Mn doping CsPb (Cl/Br)3Perovskite is nanocrystalline and preparation method thereof | |
| CN105200246B (en) | A kind of method for detaching tungsten | |
| KR101216610B1 (en) | A process for the preparation of nano zinc oxide particles | |
| CN104439279B (en) | A kind of method realizing regulation and control nano silver wire diameter by sodium chloride consumption | |
| CN104925867B (en) | A kind of nanometer wolframic acid caesium powder body and preparation method and application | |
| CN104261491A (en) | Method for synthesizing high-purity nickel disulfide | |
| CN108557888B (en) | A kind of metal phase molybdenum disulfide nanostructure and preparation method thereof | |
| Chen et al. | Biomolecule-assisted hydrothermal synthesis of molybdenum disulfide microspheres with nanorods | |
| CN107555470A (en) | A kind of method of two-step method synthesis zinc cadmium sulphur solid-solution material | |
| CN107324357B (en) | Method for preparing ZSM-5 molecular sieve by using white mud as raw material and ZSM-5 molecular sieve | |
| CN103408055A (en) | A kind of normal temperature preparation method of spherical Cu2O porous adsorption material | |
| CN103482689B (en) | Method for preparing nano lead stannate powder by microwave hydrothermal/solvothermal process | |
| CN101214990A (en) | A kind of normal temperature synthetic method of nanometer zinc oxide | |
| CN104229900A (en) | A kind of preparation method of α-Fe2O3 cube | |
| CN109110816B (en) | A kind of synthetic method of oil-soluble molybdenum disulfide | |
| CN104787810B (en) | A kind of preparation method of cubic curing nickel | |
| CN103408056B (en) | A kind of liquid-phase precipitation method prepares the method for nano cupric oxide | |
| CN103332674A (en) | Method for hydrothermally synthesizing carbon quantum dots on basis of tartaric acid and organic amine | |
| CN103664723B (en) | The preparation method of metal dithiocarbamate solution and nano metal sulfide material | |
| CN108217728A (en) | A kind of MoS2Nano-particle morphology controllable preparation method | |
| CN105060353B (en) | The preparation method that the sub-nickel of a kind of orthorhombic system sulfuration is nanocrystalline | |
| CN103920874A (en) | Preparation method of hollow composite nano-particles | |
| CN101254939A (en) | A method for preparing zinc oxide nano hollow spheres by alkali corrosion reaction | |
| CN109133158B (en) | Preparation method of partially oxidized SnS2 flakes, products and uses thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| TR01 | Transfer of patent right | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20190724 Address after: 100070 Room 601, Building 3, 128 South Fourth Ring West Road, Fengtai District, Beijing Patentee after: PAYONEL ENVIRONMENTAL PURIFICATION ENGINEERING (BEIJING) CO., LTD. Address before: 100070 Beijing Fengtai District South Fourth Ring West Road 128 Courtyard 3, 5th floor 601-2 (Park) Patentee before: BEIJING XINYIYUAN ENVIRONMENTAL PROTECTION TECHNOLOGY CO., LTD. |