CN106564962B - A kind of method that protein matter reduction prepares class graphene molybdenum disulfide-ferriferrous oxide composite material - Google Patents
A kind of method that protein matter reduction prepares class graphene molybdenum disulfide-ferriferrous oxide composite material Download PDFInfo
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Abstract
The method for preparing class graphene molybdenum disulfide ferriferrous oxide composite material is reduced the present invention provides a kind of protein matter, molybdenum disulfide powder is added in intercalation solution and carries out intercalation, filtering, drying, obtain intercalation molybdenum disulfide powder after the completion of reaction；Intercalation molybdenum disulfide powder made from step 1 and protein matter and water are mixed and stirred for uniformly, dry, grinding obtains precursor powder；It is added to the water after ferric nitrate is mixed with citric acid, carries out chelatropic reaction, obtain yellow sol solution；Precursor powder is added in into yellow sol solution, mixed gel is obtained after being stirred, dry, grinding obtains dry gel powder；Dry gel powder carries out reduction reaction under a shielding gas, postcooling that the reaction was complete, takes out reaction product.The present invention realizes the stripping of molybdenum disulfide and the generation of ferroso-ferric oxide simultaneously, and a step completes the recombination process of class graphene molybdenum disulfide and ferroso-ferric oxide.
Description
Technical field
The invention belongs to New Two Dimensional Material Fields, are related to class graphene molybdenum disulfide composite material, and in particular to a kind of
The method that protein matter reduction prepares class graphene molybdenum disulfide-ferriferrous oxide composite material.
Background technology
Class graphene molybdenum disulfide (the Graphene-like MoS being made of few layer of molybdenum disulfide2) it is that one kind has class
Like the New Two Dimensional of graphene-structured and performance (2D) lamellar compound, formed in recent years with its unique physics, chemical property
For emerging research hotspot.Class graphene molybdenum disulfide has " sandwich by what the multilayer molybdenum disulfide of hexagonal crystal system formed
It is sandwich " the two dimensional crystal material of layer structure, individual layer molybdenum disulfide is made of three layers of atomic layer, and intermediate one layer is molybdenum atom layer,
Upper and lower two layers is sulphur atom layer, and molybdenum atom layer forms class " sandwich " structure, molybdenum atom and sulphur folded by two layers of sulphur atom layer
Atom forms two-dimensional atomic crystal with Covalent bonding together；Multilayer molybdenum disulfide is made of several individual layer molybdenum disulfide, is not surpassed generally
Five layers are crossed, for interlayer there are weak Van der Waals force, interlamellar spacing is about 0.65nm.
As a kind of important two-dimensional layer nano material, few layer molybdenum disulfide is with its unique " sandwich " stratiform
Structure is widely used in various fields such as lubricant, catalysis, energy stores, composite materials.Compared to zero band gap of graphene,
Class graphene molybdenum disulfide possesses brighter prospect in field of photoelectric devices there are regulatable band gap；Compared to silicon material
The three-dimensional bulk structure of material, class graphene molybdenum disulfide have the two-dimensional layered structure of nanoscale, can be used to manufacture and partly lead
Body or the higher electronic chip of specification smaller, efficiency, will be used widely in fields such as follow-on nano-electric devices.
Although platelike molybdenumdisulfide has good greasy property and photoelectric properties, it has in all many performances
It treats further to be promoted, molybdenum disulfide is used in combination with other organic or inorganic particles, be to be promoted using their synergistic effect
One of method of molybdenum disulfide performance.Patent CN201410369695 disclose a kind of molybdenum disulfide-titanium dioxide compound and
Its preparation method, exists with molybdenum disulfide using titanium dioxide and lubrication is cooperateed with to be acted on concerted catalysis, and two are synthesized by chemical method
Molybdenum sulfide-titanium dioxide compound is one of effective way for the lubrication and catalytic performance for improving molybdenum disulfide and titanium dioxide；
Patent of invention CN201510149438 discloses a kind of preparation method for the graphene composite film for adulterating individual layer curing molybdenum sheet,
By graphene and the compound electric conductivity for improving composite material of molybdenum disulfide nano sheet, enhancing electrochemical electrode is reacted and urged
Change the transmission of electronics in reaction process, so as to improve the chemical property of composite material and catalytic performance；Patent of invention
CN201510349912 discloses a kind of molybdenum disulfide-carbon composite and preparation method thereof, using cheap titanium dioxide
Silicon particle and glucose are prepared for being applied to molybdenum disulfide lithium cell negative pole material curing molybdenum sheet as template and base material
Layer-carbon hollow ball nanocomposite, this structural composite material are conducive to keep the stability of electrode, and can shorten lithium
The transmission range of ion is conducive to the promotion of high rate performance.
Although molybdenum disulfide composite material disclosed above is in greasy property and photoelectric properties to molybdenum disulfide stratiform
The performance of material has very big promotion, but effectively solves to do there is no proposition for the performance boost of magnetic steering and adsorbing domain
Method.
By compound with magnetic medium, such as and Fe3O4It is functionalized compound, obtains functionalized molybdenum disulfide stratiform material,
Its saturation magnetization can effectively be increased, and make it have magnetic conductance tropism energy, biocompatibility and strong adsorptivity, can be used
In fields such as living things catalysis, drug targeting, environmental renovation and sea water desalinations, class graphene molybdenum disulfide is greatly expanded
Application range.
Patent of invention CN201210524859 discloses a kind of synthesis MoS2-Fe3O4The preparation method of nanocomposite,
With Fe3O4Nano particle is raw material, distributes it in deionized water and adds in sodium molybdate, sodium chloride, sodium sulfocyanate and surface are lived
Property agent CTAB, 6-10h is reacted in stainless steel cauldron, MoS is obtained after cleaning-drying2The Fe of cladding3O4Nano particle.The party
Although MoS has been made using hydro-thermal method in method2-Fe3O4Nanocomposite, but its preparation flow is complicated, and energy consumption is big, is not suitable for work
Industry metaplasia is produced, and its product structure is MoS2The Fe of cladding3O4Nano particle, and it is usual in adsorbing domain and photocatalysis field
Need the stratiform MoS of large area2Composite material, with Fe3O4Fe is needed after nano-particles reinforcement3O4Nano particle is uniformly attached to it
It on lamella, and is functionalized with it, obtains modified stratiform MoS2-Fe3O4Nanocomposite.In addition, MoS2The layer of stratified material
Number is fewer, and band gap is bigger, and electron transfer efficiency is higher, and photoelectric properties are better.Therefore, exploration is a kind of prepares class graphene two
The simple and easy method of molybdenum sulfide-ferriferrous oxide nano composite material is very necessary.
The content of the invention
Based on problems of the prior art, it is an object of the present invention to provide a kind of reduction of protein matter to prepare
The method of class graphene molybdenum disulfide-ferriferrous oxide composite material can obtain the class stone with nanoscale, superior performance
It is compound to solve existing class graphene molybdenum disulfide-ferroso-ferric oxide for black alkene molybdenum disulfide-ferriferrous oxide nano composite material
Material preparation flow is complicated, and energy consumption is big, and not environmentally and unsuitable industrialized production and granular composite material particle are adsorbing
The technical issues of with photocatalysis aspect poor performance.
In order to solve the above-mentioned technical problem, the application, which adopts the following technical scheme that, is achieved：
A kind of method that protein matter reduction prepares class graphene molybdenum disulfide-ferriferrous oxide composite material, the party
Method comprises the following steps：
Molybdenum disulfide powder is added in intercalation solution and carries out intercalation by step 1, filtering, baking after the completion of reaction
It is dry, obtain intercalation molybdenum disulfide powder；
The mixed solution that the intercalation solution is potassium chlorate, sodium nitrate, the concentrated sulfuric acid and hydrogen peroxide form；
The molybdenum disulfide powder and potassium chlorate, sodium nitrate, the concentrated sulfuric acid of mass concentration 98% and mass concentration 30%
Hydrogen peroxide between proportion relation be 1g：(1~4) g：(0.5~2) g：(9~40) mL：(4~20) mL；
Intercalation molybdenum disulfide powder made from step 1 and protein matter and water are mixed and stirred for uniformly by step 2,
Dry, grinding, obtains precursor powder；
Proportion relation between the intercalation molybdenum disulfide powder and protein matter and water is 2g：(0.25~1.25)
g：(5~30) g；
Step 3 is added to the water after ferric nitrate is mixed with citric acid, carries out chelatropic reaction, obtains sol solution；
Proportion relation between the ferric nitrate, citric acid and deionized water is 1g：(0.8~1.2) g:(1~3) g；
Step 4 adds in precursor powder into sol solution, and mixed gel is obtained after being stirred, dry, grinds
To dry gel powder；
Proportion relation between the sol solution and precursor powder is：100g：(1.7~5.5) g；
Step 5, dry gel powder carry out reduction reaction under a shielding gas, postcooling that the reaction was complete, take out reaction production
Object obtains class graphene molybdenum disulfide-ferriferrous oxide composite material after grinding.
The present invention also has following distinguishing feature：
Specifically, the protein matter is tyrosine, tryptophan, phenylalanine or threonine.
Preferably, the molybdenum disulfide powder and potassium chlorate, sodium nitrate, the concentrated sulfuric acid of mass concentration 98% and quality are dense
Proportion relation between the hydrogen peroxide of degree 30% is 1g：2g：1g：23mL：7mL.
Preferably, the proportion relation between the intercalation molybdenum disulfide powder and protein matter and water is 2g：0.5g：
15g。
Specifically, in step 1, the process of the intercalation is：Molybdenum disulfide powder is added in mixed solution,
10~30 DEG C of 1~3h of reaction are heated to, then at 30~70 DEG C and stir 20~50min, it is stirred to react 10 at 75~100 DEG C~
Then 30min filters, is dry, obtaining intercalation molybdenum disulfide powder.
Specifically, in step 2, after intercalation molybdenum disulfide powder, protein matter and the water are mixed evenly,
At a temperature of 50~100 DEG C in drying box by 6~dry for 24 hours, grind, obtain precursor powder.
Specifically, in step 3, the detailed process of chelatropic reaction is：It is added to the water after ferric nitrate is mixed with citric acid,
The pH of ammonium hydroxide adjusting reaction system is added in 6.5~7.5,4~6h of chelatropic reaction is stirred at 45~80 DEG C, it is molten to obtain colloidal sol
Liquid.
Specifically, in step 4, precursor powder is added in into sol solution, 2~3.5h is stirred at 45~80 DEG C and is obtained
To mixed gel, xerogel is obtained after dry 7~15h at 90~130 DEG C, xerogel is ground to 200 mesh sieves and done
Gel powder.
Specifically, in step 5, the process of the reduction reaction is：The dry gel powder of gained in step 4 is packed into
Boat is burnt, is put into tube furnace, protective atmosphere is continually fed into and carries out reduction reaction, taken out after cooling to room temperature with the furnace after the completion of reaction
Reduzate is to get to class graphene molybdenum disulfide-bismuth molybdate composite material；
When the protein matter is tyrosine, the temperature of reduction reaction is 280~400 DEG C, soaking time for 40~
90min；When the protein matter is tryptophan, the temperature of reduction reaction is 240~320 DEG C, soaking time for 30~
80min；When the protein matter is phenylalanine, the temperature of reduction reaction is 250~320 DEG C, soaking time for 50~
120min；When the protein matter is threonine, the temperature of reduction reaction is 200~300 DEG C, soaking time for 40~
120min。
Preferably, the protective atmosphere is nitrogen or argon gas.
Compared with prior art, the present invention beneficial has the technical effect that：
(I) present invention is mixed to form presoma using protide organic carbon source with molybdenum disulfide so that organic carbon source is inserted into
Molybdenum disulfide powder interlayer increases its interfloor distance, weakens molybdenum disulfide interlayer van der Waals interaction, binding protein organic carbon
Source heating carbonization promotes to realize the reduction and stripping of molybdenum disulfide.
(II) present invention is reduced by sol-gel method and the heating of protide organic carbon, while realizes molybdenum disulfide
The generation with ferroso-ferric oxide is removed, and a step completes the recombination process of class graphene molybdenum disulfide and ferroso-ferric oxide.
(III) product prepared by the present invention is the class graphene molybdenum disulfide with high carrier mobility and four oxidations three
The compound nano material of iron nano-particle, and Fe3O4Nano particle is uniformly attached on individual layer molybdenum disulfide lamella, is had preferable
The fields such as magnetic conductance tropism energy, drug targeting, environmental renovation and sea water desalination, greatly expand molybdenum disulfide applies model
It encloses.
(IV) class graphene molybdenum disulfide-ferriferrous oxide nano composite material prepared by the present invention, it is easy to operate, it is not required to
Want complicated and cumbersome preparation facilities, preparation efficiency are high, yield is big, environmental protection and suitable industrialized production.
Description of the drawings
Fig. 1 is the Raman collection of illustrative plates of class graphene molybdenum disulfide-ferriferrous oxide nano composite material in embodiment 1.
Fig. 2 is the TEM figures of class graphene molybdenum disulfide-ferriferrous oxide nano composite material in embodiment 1.
Fig. 3 is the XRD diagram of class graphene molybdenum disulfide-ferriferrous oxide nano composite material in embodiment 1.
Fig. 4 is the Raman collection of illustrative plates of molybdenum disulfide-ferriferrous oxide nano composite material in comparative example 1.
Fig. 5 is the TEM figures of molybdenum disulfide-ferriferrous oxide nano composite material in comparative example 1.
The particular content of the present invention is described in more detail with reference to embodiments.
Specific embodiment
It should be noted that heretofore described class graphene molybdenum disulfide is the molybdenum disulfide of few layer structure, it is described
The structure that few layer structure is 1~5 layer.The molecular formula of ferric nitrate is Fe (NO3)3·9H2O。
Above-mentioned technical proposal is deferred to, specific embodiments of the present invention are given below, it is necessary to which explanation is the present invention not office
It is limited to specific examples below, all equivalents done on the basis of technical scheme each fall within the protection model of the present invention
It encloses.The present invention is described in further details with reference to embodiment.
Embodiment 1：
The present embodiment provides a kind of protein matter reduction and prepares class graphene molybdenum disulfide-ferriferrous oxide composite material
Method, this method comprises the following steps：
Molybdenum disulfide powder is ground to the sieving of 200 mesh, 10g screenings molybdenum disulfide powders is taken to be added to slotting by step 1
In layer solution, the composition of intercalation solution be potassium chlorate be 20g, sodium nitrate 10g, the concentrated sulfuric acid of mass concentration 98% are 230mL
Hydrogen peroxide with mass concentration 30% is 70mL；
Then heating water bath at 30 DEG C and stirs 30min, carries out intercalation, be then heated to 75 to 15 DEG C of reaction 2h
DEG C 30min is stirred to react, acquired solution after reaction is filtered and dries filter cake, be ground to the sieving of 200 mesh, obtain two sulphur of intercalation
Change molybdenum powder.
Step 2 takes 0.5g tyrosine to add in 15g deionized waters, treats that tyrosine is stirring evenly and then adding into 2.0g intercalations two
Vulcanize molybdenum powder, stir evenly, dried at a temperature of 60 in drying box DEG C by 8h, be ground to the sieving of 200 mesh, obtain forerunner
Body powder.
Step 3 takes 120g ferric nitrates to be added in after being mixed with 96g citric acids in 120g deionized waters, adds in ammonium hydroxide and adjusts pH
It is worth for 6.8, yellow sol solution is obtained after stirring chelating 6h at 65 DEG C.
Step 4 takes 100g sol solutions and adds in 2.3g precursor powders wherein, continues the stirring 3h at 65 DEG C and obtains
To mixed gel, mixed gel is obtained into xerogel after dry 8h at 100 DEG C, and is ground to 200 mesh and sieved and done
Gel powder.
Dry gel powder is fitted into burning boat and is placed in tube furnace, is passed through argon gas, be warming up to 330 DEG C, reaction by step 5
Taking-up product is ground to get compound to class graphene molybdenum disulfide-ferroso-ferric oxide after cooling to room temperature after 60min with the furnace
Material.
Raman collection of illustrative plates such as Fig. 1 of class graphene molybdenum disulfide-ferroso-ferric oxide nano composite material prepared by the present embodiment
Shown, XRD diagram is as shown in Fig. 2, high-resolution TEM figures are as shown in Figure 3.
E in Raman collection of illustrative plates in Fig. 12g 1With Ag 1Value is respectively 384.3 and 408.4, displacement difference 24.1, with reference to Raman spectral difference
Related article (Li H, Zhang Q, Yap C C R, the et al.From Bulk to of relation between value and the molybdenum disulfide number of plies
Monolayer MoS2:Evolution of Raman Scattering[J].Advanced Functional
Materials,2012,22(7):It 1385-1390.) understands, displacement difference is less than 25, and the number of plies of the product is 1~5 layer, belongs to few
Layer structure molybdenum disulfide shows that molybdenum disulfide is the class graphene molybdenum disulfide of few layer in composite material prepared by the present embodiment.
XRD data, which may indicate that in product, in Fig. 2 ferroso-ferric oxide generation.Fig. 3 middle high-resolution TEM figures are shown as the class stone of few layer
Black alkene molybdenum disulfide-ferriferrous oxide nano composite material.Comprehensive attached drawing can show that the sample prepared by the present embodiment is class
Graphene molybdenum disulfide-ferriferrous oxide nano composite material.
Embodiment 2：
The present embodiment provides a kind of protein matter reduction and prepares class graphene molybdenum disulfide-ferriferrous oxide composite material
Method, this method comprises the following steps：
Molybdenum disulfide powder is ground to the sieving of 200 mesh, 10g screenings molybdenum disulfide powders is taken to be added to slotting by step 1
In layer solution, the composition of intercalation solution be potassium chlorate be 40g, sodium nitrate 5g, the concentrated sulfuric acid of mass concentration 98% be 300mL and
The hydrogen peroxide of mass concentration 30% is 60mL.
Then heating water bath at 10 DEG C and stirs 30min, carries out intercalation, be then heated to 95 to 10 DEG C of reaction 2h
DEG C 25min is stirred to react, acquired solution after reaction is filtered and dries filter cake, be ground to the sieving of 200 mesh, obtain two sulphur of intercalation
Change molybdenum powder.
Step 2 takes 1.1g tyrosine to add in 12.5g deionized waters, treats that tyrosine is stirring evenly and then adding into 2.0g intercalations
Molybdenum disulfide powder stirs evenly, and is dried at a temperature of 70 in drying box DEG C by 7.5h, is ground to the sieving of 200 mesh, obtains
Precursor powder.
Step 3 takes 120g ferric nitrates to be added in after being mixed with 108g citric acids in 120g deionized waters, adds in ammonium hydroxide and adjusts
PH value is 7.2, and yellow sol solution is obtained after stirring chelating 4h at 55 DEG C.
Step 4 takes 100g sol solutions and adds in 2.8g precursor powders wherein, continues to stir 2.5h at 55 DEG C
Mixed gel is obtained, mixed gel is obtained into xerogel after dry 15h at 90 DEG C, and is ground to 200 mesh and sieves to obtain
Dry gel powder.
Dry gel powder is fitted into burning boat and is placed in tube furnace, is passed through argon gas, be warming up to 300 DEG C, reaction by step 5
Taking-up product is ground to get compound to class graphene molybdenum disulfide-ferroso-ferric oxide after cooling to room temperature after 80min with the furnace
Material.
The characterization result and embodiment of the present embodiment products therefrom class graphene molybdenum disulfide-ferriferrous oxide composite material
1 is essentially identical.
Embodiment 3：
The present embodiment provides a kind of protein matter reduction and prepares class graphene molybdenum disulfide-ferriferrous oxide composite material
Method, this method comprises the following steps：
Molybdenum disulfide powder is ground to the sieving of 200 mesh, 10g screenings molybdenum disulfide powders is taken to be added to slotting by step 1
In layer solution, the composition of intercalation solution be potassium chlorate be 10g, sodium nitrate 8g, the concentrated sulfuric acid of mass concentration 98% be 400mL and
The hydrogen peroxide of mass concentration 30% is 45mL.
Then heating water bath at 45 DEG C and stirs 50min, carries out intercalation, be then heated to 98 to 30 DEG C of reaction 1h
DEG C 15min is stirred to react, acquired solution after reaction is filtered and dries filter cake, be ground to the sieving of 200 mesh, obtain two sulphur of intercalation
Change molybdenum powder.
Step 2 takes 1.1g tyrosine to add in 25g deionized waters, treats that tyrosine is stirring evenly and then adding into 2.0g intercalations two
Vulcanize molybdenum powder, stir evenly, dried at a temperature of 50 in drying box DEG C by 8h, be ground to the sieving of 200 mesh, obtain forerunner
Body powder.
Step 3 takes 120g ferric nitrates to be added in after being mixed with 144g citric acids in 200g deionized waters, adds in ammonium hydroxide and adjusts
PH value is 6.7, and yellow sol solution is obtained after stirring chelating 6h at 45 DEG C.
Step 4 takes 100g sol solutions and adds in 3.5g precursor powders wherein, continues the stirring 2h at 45 DEG C and obtains
To mixed gel, mixed gel is obtained into xerogel after dry 12h at 110 DEG C, and is ground to 200 mesh and sieved and done
Gel powder.
Dry gel powder is fitted into burning boat and is placed in tube furnace, is passed through argon gas, be warming up to 400 DEG C, reaction by step 5
Taking-up product is ground to get compound to class graphene molybdenum disulfide-ferroso-ferric oxide after cooling to room temperature after 40min with the furnace
Material.
The characterization result and embodiment of the present embodiment products therefrom class graphene molybdenum disulfide-ferriferrous oxide composite material
1 is essentially identical.
Embodiment 4：
The present embodiment provides a kind of protein matter reduction and prepares class graphene molybdenum disulfide-ferriferrous oxide composite material
Method, this method comprises the following steps：
Molybdenum disulfide powder is ground to the sieving of 200 mesh, 10g screenings molybdenum disulfide powders is taken to be added to slotting by step 1
In layer solution, the composition of intercalation solution be potassium chlorate be 15g, sodium nitrate 20g, the concentrated sulfuric acid of mass concentration 98% are 210mL
Hydrogen peroxide with mass concentration 30% is 100mL.
Then heating water bath at 35 DEG C and stirs 20min, carries out intercalation, be then heated to 12 DEG C of reaction 2.5h
80 DEG C are stirred to react 30min, and acquired solution after reaction is filtered and dries filter cake, are ground to the sieving of 200 mesh, obtain intercalation two
Vulcanize molybdenum powder.
Step 2 takes 0.9g tyrosine to add in 5g deionized waters, treats that tyrosine is stirring evenly and then adding into 2.0g intercalations two
Vulcanize molybdenum powder, stir evenly, dried at a temperature of 90 in drying box DEG C by 7h, be ground to the sieving of 200 mesh, obtain forerunner
Body powder.
Step 3 takes 120g ferric nitrates to be added in after being mixed with 100g citric acids in 150g deionized waters, adds in ammonium hydroxide and adjusts
PH value is 6.6, and yellow sol solution is obtained after stirring chelating 5.5h at 80 DEG C.
Step 4 takes 100g sol solutions and adds in 5.5g precursor powders wherein, continues the stirring 2h at 80 DEG C and obtains
To mixed gel, mixed gel is obtained into xerogel after dry 7h at 90 DEG C, and is ground to 200 mesh and sieves to obtain dry coagulate
Rubber powder end.
Dry gel powder is fitted into burning boat and is placed in tube furnace, is passed through nitrogen, be warming up to 280 DEG C, reaction by step 5
Taking-up product is ground to get compound to class graphene molybdenum disulfide-ferroso-ferric oxide after cooling to room temperature after 90min with the furnace
Material.
The characterization result and embodiment of the present embodiment products therefrom class graphene molybdenum disulfide-ferriferrous oxide composite material
1 is essentially identical.
Embodiment 5：
The present embodiment provides a kind of protein matter reduction and prepares class graphene molybdenum disulfide-ferriferrous oxide composite material
Method, this method comprises the following steps：
Molybdenum disulfide powder is ground to the sieving of 200 mesh, 10g screenings molybdenum disulfide powders is taken to be added to slotting by step 1
In layer solution, the composition of intercalation solution be potassium chlorate be 35g, sodium nitrate 18g, the concentrated sulfuric acid of mass concentration 98% be 90mL and
The hydrogen peroxide of mass concentration 30% is 150mL.
Then heating water bath at 50 DEG C and stirs 20min, carries out intercalation, be then heated to 100 to 25 DEG C of reaction 3h
DEG C 10min is stirred to react, acquired solution after reaction is filtered and dries filter cake, be ground to the sieving of 200 mesh, obtain two sulphur of intercalation
Change molybdenum powder.
Step 2 takes 1g tryptophans to add in 28g deionized waters, treats that tryptophan is stirring evenly and then adding into two sulphur of 2.0g intercalations
Change molybdenum powder, stir evenly, dried at a temperature of 100 in drying box DEG C by 18h, be ground to the sieving of 200 mesh, obtain forerunner
Body powder.
Step 3 takes 120g ferric nitrates to be added in after being mixed with 132g citric acids in 250g deionized waters, adds in ammonium hydroxide and adjusts
PH value is 7.2, and yellow sol solution is obtained after stirring chelating 6h at 80 DEG C.
Step 4 takes 100g sol solutions and adds in 3.7g precursor powders wherein, continues to stir 2.5h at 80 DEG C
Mixed gel is obtained, mixed gel is obtained into xerogel after dry 15h at 130 DEG C, and is ground to 200 mesh and sieves to obtain
Dry gel powder.
Dry gel powder is fitted into burning boat and is placed in tube furnace, is passed through argon gas, be warming up to 240 DEG C, reaction by step 5
Taking-up product is ground to get compound to class graphene molybdenum disulfide-ferroso-ferric oxide after cooling to room temperature after 80min with the furnace
Material.
The characterization result and embodiment of the present embodiment products therefrom class graphene molybdenum disulfide-ferriferrous oxide composite material
1 is essentially identical.
Embodiment 6：
The present embodiment provides a kind of protein matter reduction and prepares class graphene molybdenum disulfide-ferriferrous oxide composite material
Method, this method comprises the following steps：
Molybdenum disulfide powder is ground to the sieving of 200 mesh, 10g screenings molybdenum disulfide powders is taken to be added to slotting by step 1
In layer solution, the composition of intercalation solution be potassium chlorate be 25g, sodium nitrate 15g, the concentrated sulfuric acid of mass concentration 98% are 150mL
Hydrogen peroxide with mass concentration 30% is 120mL.
Then heating water bath at 32 DEG C and stirs 25min, carries out intercalation, be then heated to 18 DEG C of reaction 2.5h
78 DEG C are stirred to react 20min, and acquired solution after reaction is filtered and dries filter cake, are ground to the sieving of 200 mesh, obtain intercalation two
Vulcanize molybdenum powder.
Step 2 takes 1.1g tryptophans to add in 29g deionized waters, treats that tryptophan is stirring evenly and then adding into 2.0g intercalations two
Vulcanize molybdenum powder, stir evenly, by drying for 24 hours at a temperature of 80 in drying box DEG C, the sieving of 200 mesh is ground to, before obtaining
Drive body powder.
Step 3 takes 120g ferric nitrates to be added in after being mixed with 144g citric acids in 360g deionized waters, adds in ammonium hydroxide and adjusts
PH value is 6.8, and yellow sol solution is obtained after stirring chelating 6h at 80 DEG C.
Step 4 takes 100g sol solutions and adds in 3.1g precursor powders wherein, continues the stirring 3h at 80 DEG C and obtains
To mixed gel, mixed gel is obtained into xerogel after dry 15h at 110 DEG C, and is ground to 200 mesh and sieved and done
Gel powder.
Dry gel powder is fitted into burning boat and is placed in tube furnace, is passed through argon gas, be warming up to 320 DEG C, reaction by step 5
Taking-up product is ground to get compound to class graphene molybdenum disulfide-ferroso-ferric oxide after cooling to room temperature after 30min with the furnace
Material.
The characterization result and embodiment of the present embodiment products therefrom class graphene molybdenum disulfide-ferriferrous oxide composite material
1 is essentially identical.
Embodiment 7：
The present embodiment provides a kind of protein matter reduction and prepares class graphene molybdenum disulfide-ferriferrous oxide composite material
Method, this method comprises the following steps：
Molybdenum disulfide powder is ground to the sieving of 200 mesh, 10g screenings molybdenum disulfide powders is taken to be added to slotting by step 1
In layer solution, the composition of intercalation solution be potassium chlorate be 30g, sodium nitrate 12g, the concentrated sulfuric acid of mass concentration 98% are 255mL
Hydrogen peroxide with mass concentration 30% is 65mL.
Then heating water bath at 42 DEG C and stirs 45min, carries out intercalation, be then heated to 20 DEG C of reaction 1.5h
88 DEG C are stirred to react 12min, and acquired solution after reaction is filtered and dries filter cake, are ground to the sieving of 200 mesh, obtain intercalation two
Vulcanize molybdenum powder.
Step 2 takes 0.65g tryptophans to add in 20g deionized waters, treats that tryptophan is stirring evenly and then adding into 2.0g intercalations
Molybdenum disulfide powder stirs evenly, and is dried at a temperature of 75 in drying box DEG C by 20h, is ground to the sieving of 200 mesh, obtains
Precursor powder.
Step 3 takes 120g ferric nitrates to be added in after being mixed with 115g citric acids in 150g deionized waters, adds in ammonium hydroxide and adjusts
PH value is 7.0, and yellow sol solution is obtained after stirring chelating 4h at 65 DEG C.
Step 4 takes 100g sol solutions and adds in 5.5g precursor powders wherein, continues the stirring 2h at 65 DEG C and obtains
To mixed gel, mixed gel is obtained into xerogel after dry 8h at 120 DEG C, and is ground to 200 mesh and sieved and done
Gel powder.
Dry gel powder is fitted into burning boat and is placed in tube furnace, is passed through argon gas, be warming up to 280 DEG C, reaction by step 5
Taking-up product is ground to get compound to class graphene molybdenum disulfide-ferroso-ferric oxide after cooling to room temperature after 60min with the furnace
Material.
The characterization result and embodiment of the present embodiment products therefrom class graphene molybdenum disulfide-ferriferrous oxide composite material
1 is essentially identical.
Embodiment 8：
The present embodiment provides a kind of protein matter reduction and prepares class graphene molybdenum disulfide-ferriferrous oxide composite material
Method, this method comprises the following steps：
Molybdenum disulfide powder is ground to the sieving of 200 mesh, 10g screenings molybdenum disulfide powders is taken to be added to slotting by step 1
In layer solution, the composition of intercalation solution be potassium chlorate be 20g, sodium nitrate 10g, the concentrated sulfuric acid of mass concentration 98% are 225mL
Hydrogen peroxide with mass concentration 30% is 75mL.
Then heating water bath at 35 DEG C and stirs 20min, carries out intercalation, be then heated to 15 DEG C of reaction 2.5h
83 DEG C are stirred to react 18min, and acquired solution after reaction is filtered and dries filter cake, are ground to the sieving of 200 mesh, obtain intercalation two
Vulcanize molybdenum powder.
Step 2 takes 0.45g tryptophans to add in 16g deionized waters, treats that tryptophan is stirring evenly and then adding into 2.0g intercalations
Molybdenum disulfide powder stirs evenly, and is dried at a temperature of 80 in drying box DEG C by 16h, is ground to the sieving of 200 mesh, obtains
Precursor powder.
Step 3 takes 120g ferric nitrates to be added in after being mixed with 120g citric acids in 260g deionized waters, adds in ammonium hydroxide and adjusts
PH value is 7.2, and yellow sol solution is obtained after stirring chelating 4h at 55 DEG C.
Step 4 takes 100g sol solutions and adds in 2.7g precursor powders wherein, continues to stir 3.5h at 55 DEG C
Mixed gel is obtained, mixed gel is obtained into xerogel after dry 12h at 120 DEG C, and is ground to 200 mesh and sieves to obtain
Dry gel powder.
Dry gel powder is fitted into burning boat and is placed in tube furnace, is passed through nitrogen, be warming up to 300 DEG C, reaction by step 5
Taking-up product is ground to get compound to class graphene molybdenum disulfide-ferroso-ferric oxide after cooling to room temperature after 80min with the furnace
Material.
The characterization result and embodiment of the present embodiment products therefrom class graphene molybdenum disulfide-ferriferrous oxide composite material
1 is essentially identical.
Embodiment 9：
The present embodiment provides a kind of protein matter reduction and prepares class graphene molybdenum disulfide-ferriferrous oxide composite material
Method, this method comprises the following steps：
Molybdenum disulfide powder is ground to the sieving of 200 mesh, 10g screenings molybdenum disulfide powders is taken to be added to slotting by step 1
In layer solution, the composition of intercalation solution be potassium chlorate be 40g, sodium nitrate 5g, the concentrated sulfuric acid of mass concentration 98% be 300mL and
The hydrogen peroxide of mass concentration 30% is 60mL.
Then heating water bath at 38 DEG C and stirs 25min, carries out intercalation, be then heated to 86 to 12 DEG C of reaction 2h
DEG C 11min is stirred to react, acquired solution after reaction is filtered and dries filter cake, be ground to the sieving of 200 mesh, obtain two sulphur of intercalation
Change molybdenum powder.
Step 2 takes 0.95g phenylalanines to add in 26g deionized waters, treats that phenylalanine is stirring evenly and then adding into 2.0g
Intercalation molybdenum disulfide powder, stirs evenly, and is dried at a temperature of 85 in drying box DEG C by 13h, is ground to the sieving of 200 mesh,
Obtain precursor powder.
Step 3 takes 120g ferric nitrates to be added in after being mixed with 102g citric acids in 120g deionized waters, adds in ammonium hydroxide and adjusts
PH value is 6.5, and yellow sol solution is obtained after stirring chelating 4h at 55 DEG C.
Step 4 takes 100g sol solutions and adds in 3.9g precursor powders wherein, continues the stirring 2h at 55 DEG C and obtains
To mixed gel, mixed gel is obtained into xerogel after dry 8h at 90 DEG C, and is ground to 200 mesh and sieves to obtain dry coagulate
Rubber powder end.
Dry gel powder is fitted into burning boat and is placed in tube furnace, is passed through argon gas, be warming up to 320 DEG C, reaction by step 5
Taking-up product is ground to get compound to class graphene molybdenum disulfide-ferroso-ferric oxide after cooling to room temperature after 50min with the furnace
Material.
The characterization result and embodiment of the present embodiment products therefrom class graphene molybdenum disulfide-ferriferrous oxide composite material
1 is essentially identical.
Embodiment 10：
The present embodiment provides a kind of protein matter reduction and prepares class graphene molybdenum disulfide-ferriferrous oxide composite material
Method, this method comprises the following steps：
Molybdenum disulfide powder is ground to the sieving of 200 mesh, 10g screenings molybdenum disulfide powders is taken to be added to slotting by step 1
In layer solution, the composition of intercalation solution be potassium chlorate be 10g, sodium nitrate 8g, the concentrated sulfuric acid of mass concentration 98% be 400mL and
The hydrogen peroxide of mass concentration 30% is 45mL.
Then heating water bath at 70 DEG C and stirs 30min, carries out intercalation, be then heated to 25 DEG C of reaction 1.5h
90 DEG C are stirred to react 22min, and acquired solution after reaction is filtered and dries filter cake, are ground to the sieving of 200 mesh, obtain intercalation two
Vulcanize molybdenum powder.
Step 2 takes 0.9g phenylalanines to add in 5g deionized waters, treats that phenylalanine is stirring evenly and then adding into 2.0g and inserts
Layer molybdenum disulfide powder, stirs evenly, and is dried at a temperature of 55 in drying box DEG C by 10h, is ground to the sieving of 200 mesh, obtains
To precursor powder.
Step 3 takes 120g ferric nitrates to be added in after being mixed with 98g citric acids in 120g deionized waters, adds in ammonium hydroxide and adjusts pH
It is worth for 7.0, yellow sol solution is obtained after stirring chelating 5h at 75 DEG C.
Step 4 takes 100g sol solutions and adds in 1.75g precursor powders wherein, continues to stir 2.5h at 75 DEG C
Mixed gel is obtained, mixed gel is obtained into xerogel after dry 10h at 130 DEG C, and is ground to 200 mesh and sieves to obtain
Dry gel powder.
Dry gel powder is fitted into burning boat and is placed in tube furnace, is passed through argon gas, be warming up to 250 DEG C, reaction by step 5
Taking-up product is ground to get multiple to class graphene molybdenum disulfide-ferroso-ferric oxide after cooling to room temperature after 120min with the furnace
Condensation material.
The characterization result and embodiment of the present embodiment products therefrom class graphene molybdenum disulfide-ferriferrous oxide composite material
1 is essentially identical.
Embodiment 11：
The present embodiment provides a kind of protein matter reduction and prepares class graphene molybdenum disulfide-ferriferrous oxide composite material
Method, this method comprises the following steps：
Molybdenum disulfide powder is ground to the sieving of 200 mesh, 10g screenings molybdenum disulfide powders is taken to be added to slotting by step 1
In layer solution, the composition of intercalation solution be potassium chlorate be 15g, sodium nitrate 20g, the concentrated sulfuric acid of mass concentration 98% are 200mL
Hydrogen peroxide with mass concentration 30% is 100mL.
Then heating water bath at 60 DEG C and stirs 36min, carries out intercalation, be then heated to 96 to 20 DEG C of reaction 2h
DEG C 10min is stirred to react, acquired solution after reaction is filtered and dries filter cake, be ground to the sieving of 200 mesh, obtain two sulphur of intercalation
Change molybdenum powder.
Step 2 takes 1g phenylalanines to add in 30g deionized waters, treats that phenylalanine is stirring evenly and then adding into 2.0g intercalations
Molybdenum disulfide powder stirs evenly, and is dried at a temperature of 75 in drying box DEG C by 9h, the sieving of 200 mesh is ground to, before obtaining
Drive body powder.
Step 3 takes 120g ferric nitrates to be added in after being mixed with 130g citric acids in 230g deionized waters, adds in ammonium hydroxide and adjusts
PH value is 6.8, and yellow sol solution is obtained after stirring chelating 6h at 55 DEG C.
Step 4 takes 100g sol solutions and adds in 3.3g precursor powders wherein, continues the stirring 2h at 55 DEG C and obtains
To mixed gel, mixed gel is obtained into xerogel after dry 12h at 120 DEG C, and is ground to 200 mesh and sieved and done
Gel powder.
Dry gel powder is fitted into burning boat and is placed in tube furnace, is passed through argon gas, be warming up to 280 DEG C, reaction by step 5
Taking-up product is ground to get compound to class graphene molybdenum disulfide-ferroso-ferric oxide after cooling to room temperature after 80min with the furnace
Material.
The characterization result and embodiment of the present embodiment products therefrom class graphene molybdenum disulfide-ferriferrous oxide composite material
1 is essentially identical.
Embodiment 12：
The present embodiment provides a kind of protein matter reduction and prepares class graphene molybdenum disulfide-ferriferrous oxide composite material
Method, this method comprises the following steps：
Molybdenum disulfide powder is ground to the sieving of 200 mesh, 10g screenings molybdenum disulfide powders is taken to be added to slotting by step 1
In layer solution, the composition of intercalation solution be potassium chlorate be 35g, sodium nitrate 18g, the concentrated sulfuric acid of mass concentration 98% be 90mL and
The hydrogen peroxide of mass concentration 30% is 150mL.
Then heating water bath at 52 DEG C and stirs 42min, carries out intercalation, be then heated to 10 DEG C of reaction 2.5h
100 DEG C are stirred to react 10min, and acquired solution after reaction is filtered and dries filter cake, are ground to the sieving of 200 mesh, obtain intercalation
Molybdenum disulfide powder.
Step 2 takes 0.25g phenylalanines to add in 27g deionized waters, treats that phenylalanine is stirring evenly and then adding into 2.0g
Intercalation molybdenum disulfide powder, stirs evenly, and is dried at a temperature of 60 in drying box DEG C by 8h, is ground to the sieving of 200 mesh, obtains
To precursor powder.
Step 3 takes 120g ferric nitrates to be added in after being mixed with 108g citric acids in 160g deionized waters, adds in ammonium hydroxide and adjusts
PH value is 7.2, and yellow sol solution is obtained after stirring chelating 4.5h at 55 DEG C.
Step 4 takes 100g sol solutions and adds in 2.2g precursor powders wherein, continues the stirring 2h at 55 DEG C and obtains
To mixed gel, mixed gel is obtained into xerogel after dry 13h at 90 DEG C, and is ground to 200 mesh and sieved and done
Gel powder.
Dry gel powder is fitted into burning boat and is placed in tube furnace, is passed through nitrogen, be warming up to 300 DEG C, reaction by step 5
Taking-up product is ground to get compound to class graphene molybdenum disulfide-ferroso-ferric oxide after cooling to room temperature after 70min with the furnace
Material.
The characterization result and embodiment of the present embodiment products therefrom class graphene molybdenum disulfide-ferriferrous oxide composite material
1 is essentially identical.
Embodiment 13：
The present embodiment provides a kind of protein matter reduction and prepares class graphene molybdenum disulfide-ferriferrous oxide composite material
Method, this method comprises the following steps：
Step 1 is identical with the step of embodiment 1 one.
Step 2 takes 1.2g threonines to add in 21g deionized waters, treats that threonine is stirring evenly and then adding into 2.0g intercalations two
Vulcanize molybdenum powder, stir evenly, dried at a temperature of 75 in drying box DEG C by 18h, the sieving of 200 mesh is ground to, before obtaining
Drive body powder.
Step 3 takes 120g ferric nitrates to be added in after being mixed with 125g citric acids in 300g deionized waters, adds in ammonium hydroxide and adjusts
PH value is 7.0, and yellow sol solution is obtained after stirring chelating 5.5h at 60 DEG C.
Step 4 takes 100g sol solutions and adds in 1.7g precursor powders wherein, continues to stir 2.5h at 60 DEG C
Mixed gel is obtained, mixed gel is obtained into xerogel after dry 15h at 130 DEG C, and is ground to 200 mesh and sieves to obtain
Dry gel powder.
Dry gel powder is fitted into burning boat and is placed in tube furnace, is passed through argon gas, be warming up to 300 DEG C, reaction by step 5
Taking-up product is ground to get compound to class graphene molybdenum disulfide-ferroso-ferric oxide after cooling to room temperature after 40min with the furnace
Material.
The characterization result and embodiment of the present embodiment products therefrom class graphene molybdenum disulfide-ferriferrous oxide composite material
1 is essentially identical.
Embodiment 14：
The present embodiment provides a kind of protein matter reduction and prepares class graphene molybdenum disulfide-ferriferrous oxide composite material
Method, this method comprises the following steps：
Step 1 is identical with the step of embodiment 1 one.
Step 2 takes 0.27g threonines to add in 6.5g deionized waters, treats that threonine is stirring evenly and then adding into 2.0g intercalations
Molybdenum disulfide powder stirs evenly, and by drying for 24 hours at a temperature of 60 in drying box DEG C, is ground to the sieving of 200 mesh, obtains
Precursor powder.
Step 3 takes 120g ferric nitrates to be added in after being mixed with 100g citric acids in 280g deionized waters, adds in ammonium hydroxide and adjusts
PH value is 7.5, and yellow sol solution is obtained after stirring chelating 6h at 55 DEG C.
Step 4 takes 100g sol solutions and adds in 4.1g precursor powders wherein, continues to stir 3.5h at 55 DEG C
Mixed gel is obtained, mixed gel is obtained into xerogel after dry 15h at 120 DEG C, and is ground to 200 mesh and sieves to obtain
Dry gel powder.
Dry gel powder is fitted into burning boat and is placed in tube furnace, is passed through argon gas, be warming up to 200 DEG C, reaction by step 5
Taking-up product is ground to get multiple to class graphene molybdenum disulfide-ferroso-ferric oxide after cooling to room temperature after 120min with the furnace
Condensation material.
The characterization result and embodiment of the present embodiment products therefrom class graphene molybdenum disulfide-ferriferrous oxide composite material
1 is essentially identical.
Embodiment 15：
The present embodiment provides a kind of protein matter reduction and prepares class graphene molybdenum disulfide-ferriferrous oxide composite material
Method, this method comprises the following steps：
Step 1 is identical with the step of embodiment 1 one.
Step 2 takes 0.6g threonines to add in 21g deionized waters, treats that threonine is stirring evenly and then adding into 2.0g intercalations two
Vulcanize molybdenum powder, stir evenly, dried at a temperature of 80 in drying box DEG C by 9h, be ground to the sieving of 200 mesh, obtain forerunner
Body powder.
The step of step 3, the present embodiment three, is identical with the step of embodiment 1 three.
The step of step 4, the present embodiment four, is identical with the step of embodiment 1 four.
Dry gel powder is fitted into burning boat and is placed in tube furnace, is passed through argon gas, be warming up to 250 DEG C, reaction by step 5
Taking-up product is ground to get compound to class graphene molybdenum disulfide-ferroso-ferric oxide after cooling to room temperature after 70min with the furnace
Material.
The characterization result and embodiment of the present embodiment products therefrom class graphene molybdenum disulfide-ferriferrous oxide composite material
1 is essentially identical.
Embodiment 16：
The present embodiment provides a kind of protein matter reduction and prepares class graphene molybdenum disulfide-ferriferrous oxide composite material
Method, this method comprises the following steps：
Step 1 is identical with the step of embodiment 1 one.
Step 2 takes 1.25g threonines to add in 23g deionized waters, treats that threonine is stirring evenly and then adding into 2.0g intercalations
Molybdenum disulfide powder stirs evenly, and is dried at a temperature of 80 in drying box DEG C by 9h, the sieving of 200 mesh is ground to, before obtaining
Drive body powder.
The step of step 3, the present embodiment three, is identical with the step of embodiment 1 three.
The step of step 4, the present embodiment four, is identical with the step of embodiment 1 four.
Dry gel powder is fitted into burning boat and is placed in tube furnace, is passed through argon gas, be warming up to 280 DEG C, reaction by step 5
Taking-up product is ground to get compound to class graphene molybdenum disulfide-ferroso-ferric oxide after cooling to room temperature after 50min with the furnace
Material.
The characterization result and embodiment of the present embodiment products therefrom class graphene molybdenum disulfide-ferriferrous oxide composite material
1 is essentially identical.
Comparative example 1：
This comparative example provides a kind of method for preparing molybdenum disulfide-ferriferrous oxide composite material, and this method includes following
Step：
Molybdenum disulfide powder is ground to the sieving of 200 mesh, takes 10g screenings molybdenum disulfide powders, be added by step 1
Mass concentration is 10%, in the ethanol solution containing 100g polyphenylene sulfides, and heating water bath is to 30 DEG C and stirs 12h, is mixed
Liquid.5gKMnO is added in above-mentioned mixed liquor4Powder, heating water bath is to 50 DEG C and stirs 18h, filters and dries filter cake, grinds
The sieving of 200 mesh is milled to, obtains intercalation molybdenum disulfide powder.
Step 2 is identical with the step of embodiment 1 two.
Step 3 is identical with the step of embodiment 1 three.
Step 4 is identical with the step of embodiment 1 four.
Step 5 is identical with the step of embodiment 1 five.
Raman spectrum analyses and TEM points are carried out to molybdenum disulfide made from this comparative example-ferriferrous oxide composite material
Analysis.The Raman spectrum of composite material are as shown in figure 4, its E2g 1With Ag 1Value is respectively 375.7 and 402.5, displacement difference 26.8, position
It moves difference and is more than 25, show that the molybdenum disulfide in the composite material belongs to block structure molybdenum disulfide.The TEM image of composite material is such as
Shown in Fig. 5, illustrate that this product molybdenum disulfide block is accumulated, multilayered structure, and the compound uneven group of presentation of ferroso-ferric oxide is presented
Poly- phenomenon, so the composite material is not belonging to class graphene molybdenum disulfide-ferriferrous oxide nano composite material.
Comparative example 2：
This comparative example provides a kind of method for preparing molybdenum disulfide-ferriferrous oxide composite material, and this method includes following
Step：
Step 1, it is identical with other processes in the step of embodiment 1 one, it differs only in：The composition of intercalation solution
The concentrated sulfuric acid for potassium permanganate 20g, sodium nitrate 10g, mass concentration 98% is 230mL.
Step 2 is identical with the step of embodiment 1 two.
Step 3 is identical with the step of embodiment 1 three.
Step 4 is identical with the step of embodiment 1 four.
Step 5 is identical with the step of embodiment 1 five.
There is molybdenum disulfide block as comparative example 1 in molybdenum disulfide-ferriferrous oxide composite material made from this comparative example
Body is accumulated, and the appearance without finding graphene-structured, is not belonging to class graphene molybdenum disulfide nano-composite material.
Comparative example 3：
This comparative example provides a kind of method for preparing molybdenum disulfide-ferriferrous oxide composite material, and this method includes following
Step：
Step 1 is identical with the step of embodiment 1 one.
Step 2 is identical with the step of embodiment 1 two.
Step 3 is identical with the step of embodiment 1 three.
Step 4 is identical with the step of embodiment 1 four.
Dry gel powder is fitted into burning boat and is placed in tube furnace, is passed through argon gas, be warming up to 500 DEG C, react 5min by step 5
After cool to the furnace after room temperature and take out product and be ground to get to molybdenum disulfide-ferriferrous oxide composite material.
Comparative example 4：
This comparative example provides a kind of method for preparing molybdenum disulfide-ferriferrous oxide composite material, and this method includes following
Step：
Step 1 is identical with the step of embodiment 1 one.
Step 2 is identical with the step of embodiment 1 two.
Step 3 is identical with the step of embodiment 1 three.
Step 4 is identical with the step of embodiment 1 four.
Dry gel powder is fitted into burning boat and is placed in tube furnace, is passed through argon gas, be warming up to 250 DEG C, reaction by step 5
It is cooled to the furnace after 40min after room temperature and takes out product and be ground to get to molybdenum disulfide-ferriferrous oxide composite material.
There is molybdenum disulfide block as comparative example 1 in molybdenum disulfide-ferriferrous oxide composite material made from this comparative example
Body is accumulated, and the appearance without finding graphene-structured, is not belonging to class graphene molybdenum disulfide nano-composite material.
Comparative example 5：
This comparative example provides a kind of method for preparing molybdenum disulfide-ferriferrous oxide composite material, and this method includes following
Step：
Step 1 is identical with the step of embodiment 1 one.
Step 2 is identical with the step of embodiment 1 two.
Step 3 is identical with the step of embodiment 1 three.
Step 4 is identical with the step of embodiment 1 four.
Dry gel powder is fitted into burning boat and is placed in tube furnace, is passed through argon gas, be warming up to 1300 DEG C, reaction by step 5
It is cooled to the furnace after 15min after room temperature and takes out product and be ground to get to molybdenum disulfide-ferriferrous oxide composite material.
There is molybdenum disulfide block as comparative example 1 in molybdenum disulfide-ferriferrous oxide composite material made from this comparative example
Body is accumulated, and the appearance without finding graphene-structured, is not belonging to class graphene molybdenum disulfide nano-composite material.
Claims (4)
1. a kind of method that protein matter reduction prepares class graphene molybdenum disulfide-ferriferrous oxide composite material, feature
It is, this method comprises the following steps：
Molybdenum disulfide powder is added in intercalation solution and carries out intercalation by step 1, be heated to 10~30 DEG C reaction 1~
Then 3h at 30~70 DEG C and stirs 20~50min, is stirred to react 10~30min at 75~100 DEG C, then filters, is dry,
Obtain intercalation molybdenum disulfide powder；
The mixed solution that the intercalation solution is potassium chlorate, sodium nitrate, the concentrated sulfuric acid and hydrogen peroxide form；
The molybdenum disulfide powder is double with potassium chlorate, sodium nitrate, the concentrated sulfuric acid of mass concentration 98% and mass concentration 30%
Proportion relation between oxygen water is 1g：(1~4) g：(0.5~2) g：(9~40) mL：(4~20) mL；
Intercalation molybdenum disulfide powder made from step 1 and protein matter and water are mixed and stirred for uniformly, dry by step 2
At a temperature of 50~100 DEG C in dry case by 6~dry for 24 hours, grind, obtain precursor powder；
Proportion relation between the intercalation molybdenum disulfide powder and protein matter and water is 2g：(0.25~1.25) g：(5
~30) g；
The protein matter is tyrosine, tryptophan, phenylalanine or threonine；
Step 3 is added to the water after ferric nitrate is mixed with citric acid, carries out chelatropic reaction, must add in ammonium hydroxide and adjust reaction system
PH 6.5~7.5, at 45~80 DEG C stir 4~6h of chelatropic reaction, obtain sol solution；
Proportion relation between the ferric nitrate, citric acid and deionized water is 1g：(0.8~1.2) g:(1~3) g；
Step 4 adds in precursor powder into sol solution, and 2~3.5h is stirred at 45~80 DEG C and obtains mixed gel,
Xerogel is obtained after dry 7~15h at 90~130 DEG C, xerogel is ground to 200 mesh sieves to obtain dry gel powder；
Proportion relation between the sol solution and precursor powder is：100g：(1.7~5.5) g；
Step 5, by step 4 gained dry gel powder be packed into burn boat, be put into tube furnace, be continually fed into protective atmosphere into
Row reduction reaction cools to the furnace after room temperature after the completion of reaction and takes out reduzate to get to-four oxygen of class graphene molybdenum disulfide
Change three iron composite materials；
When the protein matter is tyrosine, the temperature of reduction reaction is 280~400 DEG C, soaking time for 40~
90min；When the protein matter is tryptophan, the temperature of reduction reaction is 240~320 DEG C, soaking time for 30~
80min；When the protein matter is phenylalanine, the temperature of reduction reaction is 250~320 DEG C, soaking time for 50~
120min；When the protein matter is threonine, the temperature of reduction reaction is 200~300 DEG C, soaking time for 40~
120min。
2. the method as described in claim 1, which is characterized in that the molybdenum disulfide powder and potassium chlorate, sodium nitrate, quality
Proportion relation between the concentrated sulfuric acid of concentration 98% and the hydrogen peroxide of mass concentration 30% is 1g：2g：1g：23mL：7mL.
3. the method as described in claim 1, which is characterized in that the intercalation molybdenum disulfide powder and protein matter and water
Between proportion relation be 2g：0.5g：15g.
4. the method as described in claims 1 to 3 any claim, which is characterized in that the protective atmosphere for nitrogen or
Argon gas.
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