CN102838161A - Tin disulfide intercalation compound and hydrothermal synthesis method thereof - Google Patents
Tin disulfide intercalation compound and hydrothermal synthesis method thereof Download PDFInfo
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- CN102838161A CN102838161A CN2012103593809A CN201210359380A CN102838161A CN 102838161 A CN102838161 A CN 102838161A CN 2012103593809 A CN2012103593809 A CN 2012103593809A CN 201210359380 A CN201210359380 A CN 201210359380A CN 102838161 A CN102838161 A CN 102838161A
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Abstract
The invention relates to a tin disulfide intercalation compound and a hydrothermal synthesis method thereof. According to the intercalation compound, tin disulfide is taken as a main body; one or two of hexadecyl trimethyl ammonium bromide, sodium dodecyl benzene sulfonate, lauryl sodium sulfate and polyvinyl pyrrolidone is/are taken as an intercalation object(s), and the hexadecyl trimethyl ammonium bromide, the sodium dodecyl benzene sulfonate, the lauryl sodium sulfate or the polyvinyl pyrrolidone enter an interlayer of the tin disulfide, so that the intercalation compound can be obtained by using the hydrothermal synthesis method. Compared with the prior art, the hydrothermal synthesis method of the tin disulfide intercalation compound disclosed by the invention has the advantages of simple process, low production cost and the like.
Description
Technical field
The present invention relates to a kind of inorganic materials preparing technical field that belongs to, especially relate to a kind of tin disulfide intercalation compound and hydrothermal synthesis method thereof.
Background technology
The existing history that goes up a century of the discovery of intercalation compound.In 1841, C.Schafhautl immersed graphite in the mixed solution of sulfuric acid and nitric acid, found almost to reach original twice along the expansion perpendicular to graphite on the cleavage surface direction.At the beginning of 1930's, X line thing identification of phases technology is quite perfect, and the structure of the basic metal intercalation compound of graphite is confirmed by the diffraction photo.Many mineral compound like phosphoric acid salt, MOX, disulphide, layered silicate etc., also have typical laminate structure.The characteristics of these compounds be the atom on the laminate interact with the intensive covalent linkage and interlayer with power effect between the Van der Waals force equimolecular.Since Intermolecular Forces a little less than; Under certain condition; Some polar molecules can through adsorb, insert, sandwich, power gets into the interlayer of lamellar compound and does not destroy its laminate structure between mode saboteurs such as suspension, pillared, embedding; This lamellar compound is called intercalation main body (Host), and the polar molecule of entering is called intercalation object (Guest), and product is called intercalated compound (Intercalation complex).The intercalation inorganic layered compounds is one type of important solid functional materials, has wide application at numerous areas such as absorption, conduction, separation, environmental protection, biology, catalysis, thermoelectricity, transistor, Conversion of energy and storages.
Tin disulfide (SnS
2) also have a CdI
2The laminate structure of type can be used as the host lattice of " intercalation ".From beginning in 1975, initial intercalation object was mainly alkalimetal ions such as Li, Na, mainly was that research is with SnS
2As a kind of potential energy storage material, like anode material for lithium-ion batteries; The dicyclopentadienylcobalt intercalation compound receives long-term concern with its special magnetics, optics and electrology characteristic subsequently; Subsequently, propylene carbonate, diamine, and flexible high molecular materials such as PVP, MEEP, POEGO, POMOE also all be used as SnS
2The intercalation object of intercalation compound.Recent study is found to insert SnS when MEH-PPV, PFO, F8, F8BT equiconjugate compound
2Can form afterwards and have the unique optical property and the intercalation compound of photoelectric response characteristic.SnS
2The compound method of intercalation compound mainly contains through direct graft process, the light assisted electrochemical is synthetic and LiSnS
2Stripping layer composite algorithm, wherein LiSnS
2Stripping layer composite algorithm is the main method of synthetic macromolecule intercalation sulfide.These all are to form SnS earlier
2Material and then carry out intercalation, efficient is lower; Generally need simultaneously butyllithium etc. as intercalator.Therefore, the method for the intercalation compound under new, the mild conditions of development still awaits further exploitation.
Summary of the invention
The object of the invention is exactly in order to overcome the defective that above-mentioned prior art exists; Especially present stage lacks the preparing method's of economic, effective tin disulfide intercalation compound present situation; Provide a kind of when forming tin disulfide thing phase, original position forms the hydrothermal synthesis method of tin disulfide intercalation compound under the effect of intercalation objects such as cetyl trimethylammonium bromide, dodecyl sulfonated acid sodium, sodium lauryl sulphate and PVP K120.This method technology is simple, and production cost is low, and the tin disulfide intercalation compound of gained can further satisfy industrial requirement.
The object of the invention can be realized through following technical scheme:
A kind of tin disulfide intercalation compound; This intercalation compound is main body with the tin disulfide; With in cetyl trimethylammonium bromide, X 2073, sodium lauryl sulphate or the PVP K120 one or both is the intercalation object; Cetyl trimethylammonium bromide, X 2073, sodium lauryl sulphate or PVP K120 enter into the tin disulfide interlayer, enlarge the tin disulfide interlamellar spacing.
A kind of hydrothermal synthesis method of tin disulfide intercalation compound may further comprise the steps:
(1) is 1: 2～20: 4～32 to be mixed to join in the reaction kettle in molar ratio with pink salt, sulphur source and intercalation object, adds solvent then, be made into the solution that pink salt concentration is 0.005-0.1mol/L, stir or ultrasonic dissolution;
(2) with the reaction kettle sealing, controlled temperature 140-220 ℃, reaction times 1-72h, reaction naturally cools to room temperature with reaction kettle after finishing, and product is filtered or spinning, and with absolute ethanol washing for several times, vacuum is drained, and promptly obtains the tin disulfide intercalation compound.
Described pink salt is selected from one or more in stannous oxalate, stannous sulfate, tin protochloride, tin chloride, tin acetate or the stannous acetate.
Described sulphur source is for discharging the compound or the simple substance of sulfonium ion.
Described sulphur source is thiocarbamide, dithiocarbonic anhydride or thioacetamide.
Described solvent is the hydrochloric acid soln of 0～2mol/L.Described intercalation object is one or both in cetyl trimethylammonium bromide, X 2073, sodium lauryl sulphate and the PVP K120.
Compared with prior art; The present invention is generating the tin disulfide nucleus; When producing the tin disulfide single sheet; Intercalation objects such as cetyl trimethylammonium bromide, dodecyl sulfonated acid sodium, sodium lauryl sulphate and PVP K120 promptly produce to interact with the tin disulfide single sheet and form composite single layer, form the tin disulfide intercalation compound along with composite single layer under the carrying out of reaction further piles up, grows, and this method technology is simple; Production cost is low, and the tin disulfide intercalation compound of gained can further satisfy industrial requirement.
Description of drawings
Fig. 1 is the XRD spectra of embodiment 1 gained cetyl trimethylammonium bromide/tin disulfide intercalation compound.
Fig. 2 is the FESEM (a-b) and TEM (c-e) photo of embodiment 1 gained cetyl trimethylammonium bromide/tin disulfide intercalation compound.
Fig. 3 is embodiment 1 gained cetyl trimethylammonium bromide/tin disulfide intercalation compound (CTAB-SnS
2) and tin disulfide (SnS
2) ultraviolet-visible absorption spectroscopy.
Fig. 4 is the XRD spectra of embodiment 2 gained cetyl trimethylammonium bromide/tin disulfide intercalation compound.
Fig. 5 is the XRD spectra of embodiment 3 gained cetyl trimethylammonium bromide/tin disulfide intercalation compound.
Fig. 6 be embodiment 4 gained cetyl trimethylammonium bromide/tin disulfide intercalation compound XRD spectra (a) and FESEM photo (b-c).
Fig. 7 be gained cetyl trimethylammonium bromide/tin disulfide intercalation compound XRD spectra (a, embodiment 5; B, embodiment 6; C, embodiment 7; D, embodiment 8).
Fig. 8 be gained cetyl trimethylammonium bromide/tin disulfide intercalation compound the FESEM spectrogram (a, embodiment 5; B, embodiment 6; C, embodiment 7; D, embodiment 8).
Fig. 9 is the XRD spectra of embodiment 18 gained sodium lauryl sulphate/tin disulfide intercalation compound.
Figure 10 is the XRD spectra of embodiment 19 gained sodium laurylsulfonate/tin disulfide intercalation compound.
Figure 11 is the XRD spectra of embodiment 21 gained PVP K120/tin disulfide intercalation compound.
Embodiment
Below in conjunction with accompanying drawing and specific embodiment the present invention is elaborated.
The structural characterization that the present invention adopts and the method for performance test:
X-ray diffraction (XRD): structure characterization methods be to adopt the method for X ray-6000 (Shimadzu) type x-ray diffractometer (Cu target, the filtering of nickel filter plate, λ=0.15406nm, tube voltage 40kV, tube current 30mA, 15 °～65 ° of sweep limits).
Scanning electron microscope (FESEM): with resulting nanoparticle ultra-sonic dispersion in water or ethanol; Drop on the aluminium foil; After at room temperature drying naturally; Paste with conductive resin and on sample table, to place FESEM (JEOL JSM-7401F) to observe down, the picture of acquisition is scanning electron microscope (SEM) image.
Transmission electron microscope (TEM): resulting nanoparticle is dispersed in water or the ethanol; Drop on the copper mesh that is sprayed with carbon film; At room temperature dry naturally; Put into JEM-2010 type transmission electron microscope and observe shape characteristic and the self-assembled structures thereof that obtains product under the differential responses condition, the picture of acquisition is transmission electron microscope (TEM) image.
Ultraviolet-visible light (UV-Vis) spectrum: sample ligand is processed certain concentration, is reference liquid with water in quartz container, with spectrograph (Uv 2450, Shimadzu UV-Vis), and the photoabsorption situation of the compound of test gained.
1. at first take by weighing cetyl trimethylammonium bromide (CTAB), the 0.8mmolSnCl of 6.4mmol
45H
2The thioacetamide of O, 3.2mmol and 80mL Hydrogen chloride (1mol/L) are to the 250mL beaker, and at room temperature magnetic agitation is dissolved 30min, and obtaining concentration is 0.01M SnCl
4, 0.04M thioacetamide (x=4) and 0.16M CTAB solution (y=8).Gained solution is transferred in the 100mL reaction kettle, and 180 ℃ are reacted after 48 hours down
2. after reaction finished, reaction kettle naturally cooled to room temperature, and product is filtered, and with absolute ethanol washing for several times, vacuum is drained, and promptly obtains cetyl trimethylammonium bromide/tin disulfide intercalation compound.
Fig. 1 is CTAB-SnS
2The XRD spectra of intercalation compound and SnS
2The standard spectrogram of berndtite (JCPDS No.83-1705), two feature that all show hexagonal system.According to Bragg equation the XRD spectra of product is carried out diffraction angle and the spacing that indexing can obtain each characteristic diffraction peak.Spacing and lattice parameter meet following relational expression in the hexagonal system:
Bragg equation is:
2d
hklsinθ
n＝nλ(n＝0，1，2，3......)
Wherein, a, c are the unit cell parameters of hexagonal system; H, k, l are for integer is called diffraction index; Dhkl is the spacing of intercalation compound (hkl) face; N (integer) is a diffraction progression; θ n is diffraction angle; λ is incident X-rays wavelength
The unit cell parameters that can calculate intercalation compound according to above relational expression and XRD spectra is:
And the unit cell parameters of standard SnS2 berndtite (JCPDS No.83-1705) is:
Obviously, the atom that the intercalation of CTAB is difficult to change on a direction of principal axis is arranged, and its unit cell parameters does not change, and shows that the S-Sn-S layer does not deform.Corresponding with it is on the c direction of principal axis, can observe marked inflation, and this is the result of intercalation.Interlamellar spacing has expanded
on the c direction of principal axis
Can find out that from the FESEM photo (Fig. 2 a-b) of typical ct findings AB-SnS2 intercalation compound product is the flower-shaped multi-stage micro-nano structure of elliposoidal that is of a size of 2-3 μ m, this structure is to be assembled by fine and close smooth surface, nanometer sheet in irregular shape.TEM photo (Fig. 2 c) has proved that further this structure is the three-dimensional multi-stage micro-nano structure that is assembled by nanometer sheet.From Fig. 2 d can find these nanometer sheet thinner (less than 10nm), have that the nano flake of irregular profile is formed by stacking.Tile nano flakes TRTEM (Figure 2e) displayed on the two-dimensional direction spacing of the lattice fringes
This is the (100) plane of the lattice spacing
basically the same; also can be found from the graph of the lattice fringes are not nanosheets Continuous, a nano-sheet has a lot of lattice distortion amorphous region or area, which (100) diffraction peak of low intensity is the same.
Intercalation compound strengthens at the luminous absorptance tin disulfide of visible region to some extent.
Step is with embodiment 1, and difference is that the sulphur source among the embodiment 1 is become thiocarbamide.Fig. 4 shows that product is an intercalation compound.
Embodiment 3
Step is with embodiment 1, and difference is that the sulphur source among the embodiment 1 is become dithiocarbonic anhydride.Fig. 5 shows that product is an intercalation compound.
Embodiment 4
Step is with embodiment 1, and difference is that the intercalation object concentration among the embodiment 1 is become 3.2mmol (y=4).Fig. 6 shows that product is an intercalation compound.
Embodiment 5
Step is with embodiment 1, and difference is that the 80mL Hydrogen chloride (1mol/L) among the embodiment 1 is changed into 80ml deionized water (0mol/L hydrochloric acid), and the reaction times is 1 hour.Fig. 7 .a shows that product is an intercalation compound.Fig. 8 .a is the pattern of intercalation compound.
Embodiment 6
Step is with embodiment 5, and difference is to change the reaction times among the embodiment 5 into 3 hours.Fig. 7 .b shows that product is an intercalation compound.Fig. 8 .b is the pattern of intercalation compound.
Embodiment 7
Step is with embodiment 5, and difference is to change the reaction times among the embodiment 5 into 12 hours.Fig. 7 c shows that product is an intercalation compound.Fig. 8 c is the pattern of intercalation compound.
Embodiment 8
Step is with embodiment 5, and difference is to change the reaction times among the embodiment 5 into 48 hours.Fig. 7 d shows that product is an intercalation compound.Fig. 8 d is the pattern of intercalation compound.
Step is with embodiment 1, and difference is to be 0.005mol/L with pink salt concentration among the embodiment 1, and the concentration of cetyl trimethylammonium bromide becomes 12.8mmol (y=32), and the consumption in sulphur source is changed into 8rnmol (x=20), and Hydrogen chloride concentration is 2mol/L.Product is an intercalation compound.
Step is with embodiment 1, and difference is to be 0.1mol/L with pink salt concentration among the embodiment 1.The concentration of cetyl trimethylammonium bromide becomes 32mmol (y=4), and the consumption in sulphur source is changed into 16mmol (x=2), and Hydrogen chloride concentration is 2mol/L.Product is an intercalation compound.
Embodiment 11
Step is with embodiment 1, and difference is that temperature of reaction is 220 ℃.Product is an intercalation compound.
Embodiment 12
Step is with embodiment 1, and difference is that temperature of reaction is 140 ℃, and the reaction times is 72 hours.Product is an intercalation compound.
Embodiment 13
Step is with embodiment 1, and difference is that pink salt is a stannous oxalate.Product is an intercalation compound.
Embodiment 14
Step is with embodiment 1, and difference is that pink salt is a stannous sulfate.Product is an intercalation compound.
Embodiment 15
Step is with embodiment 1, and difference is that pink salt is a tin protochloride.Product is an intercalation compound.
Embodiment 16
Step is with embodiment 1, and difference is that pink salt is a tin acetate.Product is an intercalation compound.
Embodiment 17
Step is with embodiment 1, and difference is that pink salt is a stannous acetate.Product is an intercalation compound.
Embodiment 18
Step is with embodiment 1, and difference is that the intercalation object is a sodium lauryl sulphate.Fig. 9 shows that product is sodium lauryl sulphate/tin disulfide intercalation compound.
Embodiment 19
Step is with embodiment 1, and difference is that the intercalation object is a sodium laurylsulfonate.Figure 10 shows that product is sodium laurylsulfonate/tin disulfide intercalation compound.
Step is with embodiment 1, and difference is that the intercalation object is the mixture (each 3.2mmol) of sodium laurylsulfonate and sodium lauryl sulphate.Product is an intercalation compound.
Embodiment 21
Step is with embodiment 1, and difference is that the intercalation object is that ((C6H9NO) n, amount of substance is calculated as 18mmol by repeating unit to the 2g PVP K120, y=22.5).Figure 11 shows that product is the relatively poor PVP K120 of crystallinity/tin disulfide intercalation compound.
Embodiment 22
A kind of tin disulfide intercalation compound, this intercalation compound are main body with the tin disulfide, are the intercalation object with the cetyl trimethylammonium bromide, and cetyl trimethylammonium bromide enters into the tin disulfide interlayer, enlarge the tin disulfide interlamellar spacing.The hydrothermal synthesis method of tin disulfide intercalation compound may further comprise the steps:
(1) with pink salt, sulphur source and intercalation object 1: 2: 4 in molar ratio for being mixed to join in the reaction kettle; Add deionized water then as solvent, be made into the solution that pink salt concentration is 0.005mol/L, stirring and dissolving; Wherein, The pink salt that uses is stannous oxalate, and the sulphur source is a thiocarbamide, and the intercalation object is a cetyl trimethylammonium bromide;
(2) with the reaction kettle sealing, 140 ℃ of controlled temperature, reaction times 72h, reaction naturally cools to room temperature with reaction kettle after finishing, and product is filtered or spinning, and with absolute ethanol washing for several times, vacuum is drained, and promptly obtains the tin disulfide intercalation compound.
Embodiment 23
A kind of tin disulfide intercalation compound; This intercalation compound is main body with the tin disulfide; With X 2073 and sodium lauryl sulphate is the intercalation object, and X 2073 and sodium lauryl sulphate enter into the tin disulfide interlayer, enlarges the tin disulfide interlamellar spacing.The hydrothermal synthesis method of tin disulfide intercalation compound may further comprise the steps:
(1) with pink salt, sulphur source and intercalation object 1: 20: 32 in molar ratio for being mixed to join in the reaction kettle; Add solvent then, be made into the solution that pink salt concentration is 0.1mol/L, ultrasonic dissolution; Wherein, The pink salt that uses is tin protochloride and tin chloride, and the sulphur source is a thioacetamide, and the intercalation object is X 2073 and sodium lauryl sulphate;
(2) with the reaction kettle sealing, 220 ℃ of controlled temperature, reaction times 1h, reaction naturally cools to room temperature with reaction kettle after finishing, and product is filtered or spinning, and with absolute ethanol washing for several times, vacuum is drained, and promptly obtains the tin disulfide intercalation compound.
Claims (7)
1. tin disulfide intercalation compound; It is characterized in that; This intercalation compound is main body with the tin disulfide; With in cetyl trimethylammonium bromide, X 2073, sodium lauryl sulphate or the PVP K120 one or both is the intercalation object, and cetyl trimethylammonium bromide, X 2073, sodium lauryl sulphate or PVP K120 enter into the tin disulfide interlayer, enlarges the tin disulfide interlamellar spacing.
2. the hydrothermal synthesis method of a tin disulfide intercalation compound as claimed in claim 1 is characterized in that, this method may further comprise the steps;
(1) is 1: 2～20: 4～32 to be mixed to join in the reaction kettle in molar ratio with pink salt, sulphur source and intercalation object, adds solvent then, be made into the solution that pink salt concentration is 0.005-0.1mol/L, stir or ultrasonic dissolution;
(2) with the reaction kettle sealing, controlled temperature 140-220 ℃, reaction times 1-72h, reaction naturally cools to room temperature with reaction kettle after finishing, and product is filtered or spinning, and with absolute ethanol washing for several times, vacuum is drained, and promptly obtains the tin disulfide intercalation compound.
3. according to the hydrothermal synthesis method of tin disulfide intercalation compound as claimed in claim 2, it is characterized in that described pink salt is selected from one or more in stannous oxalate, stannous sulfate, tin protochloride, tin chloride, tin acetate or the stannous acetate.
4. according to the hydrothermal synthesis method of tin disulfide intercalation compound as claimed in claim 2, it is characterized in that described sulphur source is for discharging the compound or the simple substance of sulfonium ion.
5. according to hydrothermal synthesis method, it is characterized in that described sulphur source is thiocarbamide, dithiocarbonic anhydride or thioacetamide like claim 2 or 4 described tin disulfide intercalation compounds.
6. according to the hydrothermal synthesis method of tin disulfide intercalation compound as claimed in claim 2, it is characterized in that described solvent is the hydrochloric acid soln of 0～2mol/L.
7. according to the hydrothermal synthesis method of tin disulfide intercalation compound as claimed in claim 2; It is characterized in that described intercalation object is one or both in cetyl trimethylammonium bromide, X 2073, sodium lauryl sulphate and the PVP K120.
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| CN106587138A (en) * | 2015-10-19 | 2017-04-26 | 淮阴工学院 | Method for preparing morphology controllable tin sulfide nano material |
| CN106611837A (en) * | 2015-10-27 | 2017-05-03 | 上海交通大学 | Cobalt-intercalated molybdenum sulfide secondary battery material and preparation method and application thereof |
| CN107032345A (en) * | 2017-05-12 | 2017-08-11 | 湖南大学 | A kind of preparation method of compound between graphite layers |
| CN108249476A (en) * | 2018-01-17 | 2018-07-06 | 济南大学 | A kind of synthetic method and products obtained therefrom of SnS2/Mn3O4 three-dimensional multistages structure |
| CN111268720A (en) * | 2020-01-13 | 2020-06-12 | 信阳师范学院 | Preparation method of large interlayer spacing tin disulfide nanoflower sodium ion battery negative electrode material |
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| CN103373742A (en) * | 2013-07-05 | 2013-10-30 | 上海交通大学 | Method for hydrothermal synthesis of SnS2 nano-materials |
| CN103373742B (en) * | 2013-07-05 | 2015-10-14 | 上海交通大学 | Hydrothermal Synthesis SnS 2the method of nano material |
| CN106587138A (en) * | 2015-10-19 | 2017-04-26 | 淮阴工学院 | Method for preparing morphology controllable tin sulfide nano material |
| CN106611837A (en) * | 2015-10-27 | 2017-05-03 | 上海交通大学 | Cobalt-intercalated molybdenum sulfide secondary battery material and preparation method and application thereof |
| CN107032345A (en) * | 2017-05-12 | 2017-08-11 | 湖南大学 | A kind of preparation method of compound between graphite layers |
| CN107032345B (en) * | 2017-05-12 | 2019-05-24 | 湖南大学 | A kind of preparation method of compound between graphite layers |
| CN108249476A (en) * | 2018-01-17 | 2018-07-06 | 济南大学 | A kind of synthetic method and products obtained therefrom of SnS2/Mn3O4 three-dimensional multistages structure |
| CN108249476B (en) * | 2018-01-17 | 2019-10-11 | 济南大学 | A kind of synthetic method and products obtained therefrom of SnS2/Mn3O4 three-dimensional multistage structure |
| CN111268720A (en) * | 2020-01-13 | 2020-06-12 | 信阳师范学院 | Preparation method of large interlayer spacing tin disulfide nanoflower sodium ion battery negative electrode material |
| CN111268720B (en) * | 2020-01-13 | 2022-07-01 | 信阳师范学院 | Preparation method of large interlayer spacing tin disulfide nanoflower sodium ion battery negative electrode material |
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