CN105800597B - A kind of preparation method of mechanical stripping high conductivity composite graphite alkene - Google Patents
A kind of preparation method of mechanical stripping high conductivity composite graphite alkene Download PDFInfo
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- CN105800597B CN105800597B CN201610106146.3A CN201610106146A CN105800597B CN 105800597 B CN105800597 B CN 105800597B CN 201610106146 A CN201610106146 A CN 201610106146A CN 105800597 B CN105800597 B CN 105800597B
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B26/00—Obtaining alkali, alkaline earth metals or magnesium
- C22B26/10—Obtaining alkali metals
- C22B26/12—Obtaining lithium
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B26/00—Obtaining alkali, alkaline earth metals or magnesium
- C22B26/20—Obtaining alkaline earth metals or magnesium
- C22B26/22—Obtaining magnesium
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B5/00—General methods of reducing to metals
- C22B5/02—Dry methods smelting of sulfides or formation of mattes
- C22B5/10—Dry methods smelting of sulfides or formation of mattes by solid carbonaceous reducing agents
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2204/00—Structure or properties of graphene
- C01B2204/20—Graphene characterized by its properties
- C01B2204/22—Electronic properties
Abstract
The invention discloses a kind of preparation method of mechanical stripping high conductivity composite graphite alkene, using graphite as raw material, metal ion is first penetrated into graphite layers, metal salts of organic acids is obtained by making metal halide react with organic acid or acylate solution to the method that composite graphite heats, decompose metal salts of organic acids and obtain metal oxide, then there is reduction characteristic using carbon, it is reduced metal oxide original position, metal nanoparticle is obtained, high conductivity composite graphite alkene is obtained with using mechanical stripping again afterwards.This method directly uses graphite as raw material, metal is penetrated into graphite layers with ionic condition, the pi bond electrophilic of graphite layers make use of to act on, overcome the problem of direct pyrolytic metal halide causes graphite layers metallic skewness, and avoid the use of high activity alkali metal, whole technical process is safe and reliable, of low cost, and environmental protection, be adapted to large-scale production.
Description
Technical field
The present invention relates to technical field of nanometer material preparation, more particularly to a kind of mechanical stripping high conductivity composite graphite alkene
Preparation method.
Background technology
Graphene has the advantages that intrinsic mobility is high, specific surface area is big, Young's modulus is high and fracture strength is big, be lithium from
The ideal chose of conducting host materials in sub- battery, ultracapacitor.Graphene is the good conductor of electronics, can be electrode material
Build conductive network；The specific surface area of its superelevation can dispersive electrode material, prevent the reunion of nano particle.But current graphene
Also there are impedance it is higher the problem of, strongly limit its application in association area.Conventional method is by graphene and gold
Belong to it is compound can using the good electric conductivity of metal material come crane span structure graphene film the defects of, so that graphene be substantially improved
The conductive characteristic of film.
China Patent Publication No. 101051542 discloses a kind of preparation method of graphite base high conductive composite powder material,
It is characterized by comprising following steps：1）It is prepared by presoma：Metal chloride is inserted into expanded graphite layer and is prepared into metal chlorine
Compound-expanded graphite interlayer compound；2）Wash drying：With distilled water or alcohol solvent by metal chloride-expanded graphite layer
Between residual chlorine compound washes clean in compounds precursors, obtain the presoma of clean dry；3）Roasting：By clean dry
When roasting 2-4 is small under presoma and high temperature；4）Quenching：Put into immediately after product of roasting is taken out rapid in distilled water at room temperature
It is cold；5）Post processing：Quenched product is filtered, is dry, then crushes, obtains product.The composite powder material that this method obtains has
Cost is low, conductivity is high, has the characteristics of good compatibility with organic matter.But as introduced this area skill in Instructions Page 2
Chloride of the art personnel in the presoma for finding to be prepared using molten-salt growth method during implementing the program is distributed in " farmland shape ", into
And the metal oxide that water is reacted with chloride is also distributed in " farmland shape ", it follows that utilizing metal chlorine using molten-salt growth method
There is insert and reunites seriously in compound when preparing graphite-based high conductivity composite powder material as graphite layers insertion body, reduction
It is not easy the problem of thorough.
In the prior art, China Patent Publication No. 102807845A discloses a kind of thin graphene interlayer and includes metal
The preparation method of the high heat conduction heat sink material of grain, step A, uses concentration to be mixed for the hydrogen peroxide of 30%-60% in graphite, then
The oleum containing 20% sulfur trioxide or 96% concentrated sulfuric acid and phosphorus pentoxide are added, prepares sulfuric acid intercalated graphite,
Wash and dry；Step B, microwave, the thin graphene expanded, ultrasonic cleavage are dry；Step C, step A and step
The one or many circulations of rapid B, make 2-50 layers of the graphene number of plies prepared, 2-300 microns of lamella size, carbon-to-oxygen ratio
20-100 ；Step D, intercalation metal chloride or metal simple-substance；Step E, contains metal chloride by what is prepared in step D
The thin graphene of intercalation, using hydrogen reducing.Layer and layer of the invention that be stored in thin graphene by metallic particles original position
Between, the thermal conductivity of Z-direction is improved, environmental pollution is small, and cost is low, is adapted to industrialized mass production.But this method uses
Microwave means obtain expanded graphite, it is impossible to which, applied to the large-scale production of electrode material, operating process is complicated, and environment is also resulted in
Electromagnetic pollution.
China Patent Publication No. 104694989A discloses a kind of preparation method of graphene-based metallic composite, first
Working electrode in using graphene aerogel as three-electrode system, using the method for electro-deposition, obtains graphene-based metal and answers
Pre-product is closed, then, obtained graphene-based metal composite pre-product is again by being thermally treated resulting in graphene-based Metals composite
Material.Due to the method using electro-deposition so that the preparation method of graphene-based metallic composite provided by the invention is not related to
Any high energy consumption high pollution operation, environment friendly are strong.But this method obtains the resistance still very a height of 10 of composite graphite alkene
~100 Ω, and using precious metals pt as electrode, and raw material is graphene aerogel, it is costly.
As it can be seen that there is no also one kind graphite layers insert is uniformly dispersed in the prior art, and safe operation process is reliable,
It is of low cost, it is adapted to the technological means of large-scale production to prepare graphene and metallic composite.
The content of the invention
Metal ion in view of the deficiencies of the prior art, is directly first penetrated into graphite by the present invention using graphite as raw material
Interlayer, organic acid is obtained by making metal halide react with organic acid or acylate to the method that composite graphite heats
Metal salt, decomposes metal salts of organic acids and obtains metal oxide, then have the characteristics that reduction characteristic using carbon, make gold
Belong to oxide in-situ to be reduced, obtain metal nanoparticle, it is compound using mechanical stripping to be obtained with high conductivity again afterwards
Graphene.This method directly uses graphite cost to be greatly reduced, is suitable for serialization industrial manufacture process as raw material, compatible
The technique of mechanical stripping graphene, is adapted to the company on the existing basis in part directly to go into operation.
The present invention provides a kind of preparation method of mechanical stripping high conductivity composite graphite alkene, and the described method includes following step
Suddenly：
A. electrolyte solution is provided, the electrolyte solution is the electricity that electrolyte metal halogen is dissolved in solvent orange 2 A formation
Electrolyte solution；
B. graphite material is provided as raw material, the raw material is launched in the electrolyte solution, the raw material is in electricity
The concentration of electrolyte solution is 10 ~ 200 mg/L, stands 1 ~ 5 day, makes metal ion in electrolyte solution and the solvent orange 2 A common
The graphite material interlayer is penetrated into, forms intercalated graphite, intercalated graphite is taken out in separation；
C. under conditions of protective gas is passed through, the intercalated graphite is warming up to 700~900 DEG C, reaction 0.5~
1h, after the metal halide is reacted with solvent orange 2 A, decomposes and obtains metal oxide and gas, increases graphite layers distance, cooling
After obtain metal oxide intercalated graphite；
D. under conditions of protective gas is passed through, the metal oxide intercalated graphite is warming up to 900~1500 DEG C,
0.5~1h is reacted, metal oxide is obtained metal intercalation graphite after cooling, is then carried out by the graphite in-situ reducing
Mechanical stripping obtains metallic graphite carbon alkene composite material.
Preferably, the halogen is lithium halide, magnesium halide, calcium halide, iron halide, copper halide, aluminum halide, nickel halogenide, halogen
Change at least one of zinc, silver halide, the concentration of the halogen in a solvent is 30 ~ 700mg/L.
Preferably, the graphite material is compact crystal shape graphite, in crystalline flake graphite, expanded graphite or expansible graphite
It is one or more of.
Preferably, the solvent orange 2 A is organic acid or the aqueous solution of acylate, and concentration is 10 ~ 100 mg/L, described organic
Acid or salt are 1- ethyl-3-methylimidazoles tetrafluoro boric acid, five acetyl fluoride imines of 1- ethyl-3-methylimidazoles, 1- ethyl -3- first
Two cyaniding nitrogen of base imidazoles, 1- ethyl -3,5- methylimidazole trifluoros methylsulfonimide, 1,3- diethyl -4-methylimidazole trifluoro
One or more in methylsulfonimide or 1,3- diethyl -5- methylimidazole trifluoro methylsulfonyls.
Preferably, one kind during the mechanical stripping is peeled off for air-flow stripping, mechanical shock stripping or screw extruding.
Preferably, the resistivity of the metallic graphite carbon alkene composite material is 10-7~10-8 Ω·cm。
Said one or multiple technical solutions in the embodiment of the present application, at least have following one or more technology effects
Fruit：
1st, the program is sent out under the high temperature conditions mainly by the use of organic acid or acylate and metal halide as reactant
Raw reaction, obtains metal salts of organic acids, and metal salts of organic acids is obtaining metal oxide and gas by pyrolytic, raw
Into gas expand graphite layers distance, improve metal oxide dispersion uniformity, metal oxide is also after being more advantageous to
The metal nanoparticle that original obtains is evenly distributed in graphene surface.
2nd, in the program using organic acid or acylate solution as solvent and reactant make use of organic acid or salt without
The characteristics of strong oxidizing property, organic acid can dissociate into graphite layers and metal ion slow reaction, avoid to the strong of graphite
Strong oxidation.
3rd, the program obtains nano-metal particle using graphite reduction metal oxide in situ, reduces making for other raw materials
With, cost is reduced, it is environmentally friendly, suitable to mass produce.
Embodiment
By embodiment, the present invention is described in further detail, but this should not be interpreted as to the model of the present invention
Enclose and be only limitted to following example.Without departing from the idea of the above method of the present invention, according to ordinary skill knowledge
The various replacements or change made with customary means, should be included in the scope of the present invention.
Embodiment one
500g expanded graphites are launched and are dissolved in the 1- ethyl-3-methylimidazole tetrafluoro boric acids that concentration is 10mg/L into LiF
Formed in concentration be 30 mg/L electrolyte solution in, stir evenly, expanded graphite in electrolyte solution concentration be 20
Mg/L, after standing 1 day, the metal-lithium ion in electrolyte solution penetrates into swollen jointly with 1- ethyl-3-methylimidazoles tetrafluoro boric acid
Swollen graphite layers, form intercalated graphite, then, take out the expanded graphite of intercalation, 700 DEG C are warming up under the conditions of Ar gas is passed through,
Reacted by 0.5h, LiF and 1- ethyl-3-methylimidazole tetrafluoro boric acid, obtain LiBF4, and resolve at high temperature
Lithia and gas CO2、N2And HF, the generation of gas add graphite layers distance, graphite expands, and oxygen is obtained after cooling
Change lithium intercalated graphite.Next, under conditions of Ar atmosphere protections, lithia intercalated graphite is warming up to 900 DEG C, is passed through
0.5h, the lithias of graphite layers are obtained metal Li intercalated graphites, are then shelled with screw extruding by graphite in-situ reducing after cooling
From metallic graphite carbon alkene composite material is obtained, metallic graphite carbon alkene composite powder is obtained.The metallic graphite carbon obtained in embodiment one
The resistivity of alkene composite material is 8.2 × 10-8Ω·cm。
Embodiment two
500g expanded graphites are launched and are dissolved in the 1- ethyl-3-methylimidazole tetrafluoro boric acids that concentration is 10mg/L into LiF
Formed in concentration be 500 mg/L electrolyte solution in, stir evenly, expanded graphite in electrolyte solution concentration be 200
Mg/L, after standing 3 days, the metal-lithium ion in electrolyte solution penetrates into swollen jointly with 1- ethyl-3-methylimidazoles tetrafluoro boric acid
Swollen graphite layers, form intercalated graphite, then, take out the expanded graphite of intercalation, 800 DEG C are warming up under the conditions of Ar gas is passed through,
Reacted by 0.5h, LiF and 1- ethyl-3-methylimidazole tetrafluoro boric acid, obtain LiBF4, and resolve at high temperature
Lithia and gas CO2、N2And HF, the generation of gas add graphite layers distance, graphite expands, and oxygen is obtained after cooling
Change lithium intercalated graphite.Next, under conditions of Ar atmosphere protections, lithia intercalated graphite is warming up to 900 DEG C, is passed through
0.5h, the lithias of graphite layers are obtained metal Li intercalated graphites, are then shelled with screw extruding by graphite in-situ reducing after cooling
From metallic graphite carbon alkene composite material is obtained, metallic graphite carbon alkene composite powder is obtained.The metallic graphite carbon obtained in embodiment two
The resistivity of alkene composite material is 9.1 × 10-8Ω·cm。
Embodiment three
500g expanded graphites are launched into MgF2It is dissolved in the five fluorine second of 1- ethyl-3-methylimidazoles that concentration is 100mg/L
Concentration is in the electrolyte solution of 30 mg/L formed in imide solution, is stirred evenly, expanded graphite is in electrolyte solution
Concentration is 20 mg/L, after standing 1 day, the metal ions M g in electrolyte solution2+With five acetyl fluoride of 1- ethyl-3-methylimidazoles
Imide liquor penetrates into expanded graphite interlayer jointly, forms intercalated graphite, then, takes out intercalated graphite and is risen under the conditions of Ar gas is passed through
Temperature is to 800 DEG C, by 0.5h, MgF2With five acetyl fluoride imine reaction of 1- ethyl-3-methylimidazoles, five acetyl fluoride imines are obtained
Magnesium, resolves into magnesia and gas, gas CO under the high temperature conditions2、N2Generation with HF adds graphite layers distance, graphite
Expand, magnesia intercalated graphite is obtained after cooling.Next, under conditions of Ar atmosphere protections, by magnesia intercalation stone
Ink is warming up to 1000 DEG C, and by 0.5h, magnesia obtains metal Mg intercalated graphites by the carbon in-situ reducing in graphite after cooling,
Then peeled off to obtain metallic graphite carbon alkene composite material with mechanical shock, obtain metallic graphite carbon alkene composite powder.Embodiment three
The resistivity of the metallic graphite carbon alkene composite material of middle acquisition is 1.5 × 10-7Ω·cm。
Example IV
500g crystalline flake graphites are launched into FeCl3It is dissolved in 1, the 3- diethyl -5- methylimidazoles three that concentration is 10mg/L
In electrolyte solution formed in fluorine methylsulfonyl, stirring evenly, expanded graphite concentration in electrolyte solution is 20 mg/L,
After standing 1 day, the metal cations Fe in electrolyte solution3+Penetrated into jointly with 1,3- diethyl -5- methylimidazole trifluoro methylsulfonyls
Expanded graphite interlayer, forms intercalated graphite, then, takes out intercalated graphite and 900 DEG C are warming up under the conditions of Ar gas is passed through, pass through
0.8h, Fe3+Reacted with 1,3- diethyl -5- methylimidazole trifluoros methylsulfonyl, obtain trifluoromethanesulfonic acid iron, and pyrolytic Cheng Jin
Belong to Fe2O3With gas CO2、N2And HF, gas CO2、N2Generation with HF adds graphite layers distance, and graphite expands, cold
But Fe is obtained afterwards2O3Intercalated graphite.Next, under conditions of Ar atmosphere protections, by Fe2O3Intercalated graphite is warming up to 1200 DEG C,
By 0.8h, Fe2O3By the carbon in-situ reducing in graphite, metal Fe intercalated graphites are obtained after cooling, are then shelled with screw extruding
From metallic graphite carbon alkene composite material is obtained, the resistivity of the metallic graphite carbon alkene composite material obtained in example IV is 2.6 × 10-7
Ω·cm。
Embodiment five
500g crystalline flake graphites are launched into AlCl3It is dissolved in 1, the 3- diethyl -5- methylimidazoles three that concentration is 10mg/L
In electrolyte solution formed in fluorine methylsulfonyl, stirring evenly, expanded graphite concentration in electrolyte solution is 20 mg/L,
After standing 1 day, the metal ion Al in electrolyte solution3+Penetrated into jointly with 1,3- diethyl -5- methylimidazole trifluoro methylsulfonyls
Expanded graphite interlayer, forms intercalated graphite, then, takes out intercalated graphite and 900 DEG C are warming up under the conditions of Ar gas is passed through, pass through
0.5h, Al3+Reacted with 1,3- diethyl -5- methylimidazole trifluoros methylsulfonyl, obtain trifluoromethanesulfonic acid iron, and pyrolytic Cheng Jin
Belong to Al2O3With gas CO2、N2And HF, gas CO2、N2Generation with HF adds graphite layers distance, and graphite expands, cold
But Al is obtained afterwards2O3Intercalated graphite.Next, under conditions of Ar atmosphere protections, metal oxide intercalated graphite is warming up to
900 DEG C, by 0.5h, Al2O3By the carbon in-situ reducing in graphite, metal Al intercalated graphites are obtained after cooling, then use screw rod
Extruding stripping obtains metallic graphite carbon alkene composite material, and the resistivity of the metallic graphite carbon alkene composite material obtained in embodiment five is
4.5×10-7Ω·cm。
Embodiment six
500g crystalline flake graphites are launched into CuCl2It is dissolved in 1, the 3- diethyl -5- methylimidazoles three that concentration is 10mg/L
In electrolyte solution formed in fluorine methylsulfonyl, stirring evenly, expanded graphite concentration in electrolyte solution is 20 mg/L,
After standing 5 days, the metal ion Cu in electrolyte solution2+Penetrated into jointly with 1,3- diethyl -5- methylimidazole trifluoro methylsulfonyls
Expanded graphite interlayer, forms intercalated graphite, then, takes out intercalated graphite and 900 DEG C are warming up under the conditions of Ar gas is passed through, pass through
0.5h, Cu2+Reacted with 1,3- diethyl -5- methylimidazole trifluoros methylsulfonyl, obtain trifluoromethanesulfonic acid iron, and pyrolytic Cheng Jin
Belong to CuO and gas CO2、N2And HF, gas CO2、N2Generation with HF adds graphite layers distance, and graphite expands, cooling
After obtain CuO intercalated graphites.Next, under conditions of Ar atmosphere protections, metal oxide intercalated graphite is warming up to 1500
DEG C, by 0.5h, CuO is obtained Ni metal intercalated graphite, is then used screw extruding by the carbon in-situ reducing in graphite after cooling
Stripping obtains metallic graphite carbon alkene composite material, the resistivity of the metallic graphite carbon alkene composite material obtained in embodiment six for 7.5 ×
10-8Ω·cm。
Although preferred embodiments of the present invention have been described, but those skilled in the art once know basic creation
Property concept, then can make these embodiments other change and modification.So appended claims be intended to be construed to include it is excellent
Select embodiment and fall into all change and modification of the scope of the invention.
Obviously, various changes and modifications can be made to the invention without departing from essence of the invention by those skilled in the art
God and scope.In this way, if these modifications and changes of the present invention belongs to the scope of the claims in the present invention and its equivalent technologies
Within, then the present invention is also intended to comprising including these modification and variations.
Claims (4)
1. a kind of preparation method of mechanical stripping high conductivity composite graphite alkene, it is characterised in that the described method includes following step
Suddenly：
A. electrolyte solution is provided, the electrolyte solution is the electrolyte that electrolyte metal halogen is dissolved in solvent orange 2 A formation
Solution, the solvent orange 2 A are organic acid or the aqueous solution of acylate；
The metal halide is lithium halide, magnesium halide, calcium halide, iron halide, copper halide, aluminum halide, nickel halogenide, zinc halide, halogen
Change at least one of silver, the concentration of the metal halide in a solvent is 30 ~ 700mg/L；
The concentration of the solvent orange 2 A is 10 ~ 100mg/L, and the organic acid or acylate are 1- ethyl-3-methylimidazole tetrafluoro boron
Acid, five acetyl fluoride imines of 1- ethyl-3-methylimidazoles, two cyaniding nitrogen of 1- ethyl-3-methylimidazoles, 1- ethyl -3,5- dimethyl
Imidazoles trifluoro methylsulfonimide, 1,3- diethyl -4-methylimidazole trifluoro methylsulfonimide or 1,3- diethyl -5- methylimidazoles
One or more in trifluoro methylsulfonyl；
B. graphite material is provided as raw material, the raw material is launched in the electrolyte solution, the raw material is in electrolyte
The concentration of solution is 10 ~ 200mg/L, stands 1 ~ 5 day, the metal ion in electrolyte solution is penetrated into jointly with the solvent orange 2 A
The graphite material interlayer, forms intercalated graphite, and intercalated graphite is taken out in separation；
C. under conditions of protective gas is passed through, the intercalated graphite is warming up to 700~900 DEG C, 0.5~1h is reacted, makes institute
Metal halide is stated with after solvent orange 2 A reaction, decomposing and obtaining metal oxide and gas, increase graphite layers distance, obtained after cooling
Metal oxide intercalated graphite；
D. under conditions of protective gas is passed through, the metal oxide intercalated graphite is warming up to 900~1500 DEG C, reaction
0.5~1h, makes metal oxide obtain metal intercalation graphite after cooling by the graphite in-situ reducing, then carries out mechanical stripping
From obtaining metallic graphite carbon alkene composite material.
A kind of 2. preparation method of mechanical stripping high conductivity composite graphite alkene according to claim 1, it is characterised in that
The graphite material is compact crystal shape graphite, the one or more in crystalline flake graphite, expanded graphite or expansible graphite.
A kind of 3. preparation method of mechanical stripping high conductivity composite graphite alkene according to claim 1, it is characterised in that
The mechanical stripping is one kind during air-flow stripping, mechanical shock stripping or screw extruding are peeled off.
A kind of 4. preparation method of mechanical stripping high conductivity composite graphite alkene according to claim 1, it is characterised in that
The resistivity of the metallic graphite carbon alkene composite material is 10-7 ~10-8 Ω·cm。
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| CN108249428B (en) * | 2018-01-23 | 2020-02-07 | 福州大学 | Method for preparing single-layer graphene based on electrolyte solvent hot-insertion lithium stripping |
| CN110117807B (en) * | 2019-03-09 | 2021-04-27 | 深圳市中科墨磷科技有限公司 | Preparation method of two-dimensional material-transition metal heterojunction sheet |
| CN114853004A (en) * | 2022-04-25 | 2022-08-05 | 蜂巢能源科技股份有限公司 | Negative electrode material and preparation method and application thereof |
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| CN102807845B (en) * | 2012-08-17 | 2014-12-03 | 叶全惠 | Preparation method for high heat conduction and radiation material by intercalating metal particles between layers of thin-layer graphene |
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Effective date of registration: 20221115 Address after: Room 802-2, Building 1, No. 118, 3rd Street, Cuiqian North Road, Xiangzhou District, Zhuhai City, Guangdong Province, 519000 Patentee after: Zhongju High tech Materials Co.,Ltd. Address before: 610091, Sichuan, Chengdu province Qingyang dragon industrial port, East Sea 4 Patentee before: CHENDU NEW KELI CHEMICAL SCIENCE Co.,Ltd. CHINA |