CN108545726A - A kind of preparation method of High-performance heat conduction material - Google Patents
A kind of preparation method of High-performance heat conduction material Download PDFInfo
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- CN108545726A CN108545726A CN201810397803.3A CN201810397803A CN108545726A CN 108545726 A CN108545726 A CN 108545726A CN 201810397803 A CN201810397803 A CN 201810397803A CN 108545726 A CN108545726 A CN 108545726A
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- graphite
- heat conduction
- conduction material
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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
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/184—Preparation
- C01B32/19—Preparation by exfoliation
Abstract
The invention discloses a kind of preparation methods of High-performance heat conduction material, including Heat Conduction Material, the Heat Conduction Material is made of graphite, the concentrated sulfuric acid, hydrogen peroxide, potassium nitrate, oxidant, deionized water, hydrogenperoxide steam generator, phosphoric acid, hydrogen chloride, potassium permanganate, including following operating procedure.The preparation method of the High-performance heat conduction material, pass through the effect of the concentrated sulfuric acid and hydrogen peroxide, acid solution can be obtained after stirring, graphite is put into acid solution, it can accelerate the reaction of graphite, solution can penetrate into the interlayer of graphite after acidification, convenient for the oxidation of graphite, utilize the effect of oxidant, accelerate the oxidation reaction of graphite powder in water, utilize the effect of deionized water, graphite powder after acidification can be rinsed, utilize the effect of phosphoric acid, it can reduce when generating Heat Conduction Material, generate a large amount of toxic gas, toxic gas is prevented to be dispersed into air, influence the health of surrounding population and ecological environment.
Description
Technical field
The present invention relates to new material technology field, specially a kind of preparation method of High-performance heat conduction material.
Background technology
Heat Conduction Material is a kind of infant industry material, these materials are to be designed in recent years for the heat transfer requirement of equipment
, it has excellent performance, reliably, they are suitble to various environment and requirement, there is appropriate countermeasure to the heat conduction problem being likely to occur, right
Equipment it is highly integrated and extra small it is ultra-thin provide strong help, which has more and more been applied to perhaps
In multi-product, the reliability of product is improved.
Graphene have excellent optics, electricity, mechanical characteristic, materialogy, micro-nano technology, the energy, biomedicine and
Drug delivery etc. is with important application prospects, it is considered to be a kind of future revolutionary material uses micromechanics stripping method
Graphene is isolated in success from graphite.
Existing most Heat Conduction Material when some toxic gases such as the concentrated sulfuric acid are added, will produce in the production process
A large amount of toxic gas such as dinitrogen tetroxide, chlorine dioxide etc., when generating toxic gas, can cause prestige to the environment of surrounding
The side of body, a large amount of toxic gas are dispersed into air, influence the health of surrounding population.
Invention content
(1) the technical issues of solving
In view of the deficiencies of the prior art, the present invention provides a kind of preparation method of High-performance heat conduction material, has heat conduction
Effect is good, generates the advantages that toxic gas is few, solves most Heat Conduction Material, in the production process, the concentrated sulfuric acid is being added
Deng some toxic gases when, will produce a large amount of toxic gas such as dinitrogen tetroxide, chlorine dioxide etc., generate toxic gas
When, it can threaten to the environment of surrounding, a large amount of toxic gas is dispersed into air, influences asking for the health of surrounding population
Topic.
(2) technical solution
To realize above-mentioned good heat conduction effect, generating the few purpose of toxic gas, the present invention provides the following technical solutions：It is a kind of
The preparation method of High-performance heat conduction material, including Heat Conduction Material, the Heat Conduction Material are by graphite, the concentrated sulfuric acid, hydrogen peroxide, nitric acid
Potassium, oxidant, deionized water, hydrogenperoxide steam generator, phosphoric acid, hydrogen chloride, potassium permanganate composition, including following operating procedure：
The first step：The selection and placement of experimental facilities and heating device
A good chemical laboratory of environment is selected, a beaker is selected in laboratory, is placed in the bottom of beaker
The heating device to match with experiment demand needs the raw material used to put neatly, prevents in reality when being then ready for experiment
During testing, the chaotic effect for influencing experiment occurs；
Second step：Find the ratio of the raw material and reaction that prepare
The concentrated sulfuric acid and hydrogen peroxide are put into polymeric kettle, acid solution is obtained after being stirred, graphite is put into
In the acid solution arrived, acid molecule is made to be intercalation into the interlayer of graphite, obtains compound between graphite layers, can swollen graphite, then may be used
Swollen graphite is heated rapidly to 900 DEG C under the protection of argon gas, the acid molecule in graphite interlayer rapidly decompose enterprise planning in vapor and
Carbon dioxide expands synusia, obtains expanded graphite, and graphite synusia can expand tens times in vertical direction；
Third walks the reaction of Heat Conduction Material
Graphite powder is made with expanded graphite, prepares graphite powder, the potassium permanganate of the concentrated sulfuric acid and phosphoric acid sum, by graphite powder, dense
Sulfuric acid and phosphoric acid are put into beaker, and suitable ice water is then poured into beaker, after magnetic agitation, in the Gao Meng that 6g is added
Sour potassium stirs 1 hour in ice water, the ice water in beaker is then heated to 50 degrees Celsius, and water is then added into beaker, when
Water heating in beaker, is stirred 15 minutes, beaker carries out insulation reaction；
4th step Heat Conduction Material is made
The product in beaker is poured into ice water, suitable hydrogen peroxide is added while stirring, until solution becomes golden yellow
Then color is put into product in centrifuge and is stirred 30 minutes, filters impurity therein, chlorination is then added into liquid
Hydrogen pours into product and is rinsed into neutrality in deionized water, and obtained powder is dispersed back into water ultrasonic 8 hours, filtering
Suspension is obtained after complete black residue, it is then dry for 24 hours to get to graphite oxide in 80 degrees Celsius of environment.
Preferably, rotating speed of the centrifuge in whipping process is 7200 turns, the PH that deionized water rinsing is added
Value about seven.
Preferably, the deal of the graphite powder is 2g, and the deal of the concentrated sulfuric acid is nine parts, and the deal of the phosphoric acid is one
The deal of part potassium permanganate is 50g.
Preferably, the water in the beaker should be heated to 90-100 degrees Celsius, and the beaker should be protected in good environment
Warm twenty four hours.
Preferably, the graphite oxide aqueous solution for being added four milliliters, is stirred by ultrasonic 3h, you can obtain uniform and stable dispersion
Graphene oxide colloid in water, then generates Heat Conduction Material.
Preferably, the deal that the potassium permanganate is once added is 6g, and the number that the potassium permanganate is added is three times.
(3) advantageous effect
Compared with prior art, the present invention provides a kind of preparation methods of High-performance heat conduction material, have following beneficial
Effect：
1, the preparation method of the High-performance heat conduction material can be obtained by the effect of the concentrated sulfuric acid and hydrogen peroxide after stirring
To acid solution, graphite is put into acid solution, the reaction of graphite can be accelerated, solution can penetrate into the interlayer of graphite after acidification,
Accelerate the oxidation reaction of graphite powder in water using the effect of oxidant convenient for the oxidation of graphite, utilize the work of deionized water
With the graphite powder after acidification can be rinsed, using the effect of phosphoric acid, can be reduced when generating Heat Conduction Material, generated a large amount of
Toxic gas prevents toxic gas to be dispersed into air, influences the health of surrounding population and ecological environment.
2, the preparation method of the High-performance heat conduction material passes through the effect of hydrogen chloride so that Heat Conduction Material is soluble easily in water, profit
With the effect of graphite, the heat conductivility of Heat Conduction Material can be increased, traditional Heat Conduction Material can be substituted, improve Heat Conduction Material
Applicability and practicability.
Specific implementation mode
Based on the embodiments of the present invention, those of ordinary skill in the art are obtained without making creative work
The every other embodiment obtained, shall fall within the protection scope of the present invention.
The present invention provides a kind of technical solution：A kind of preparation method of High-performance heat conduction material, including Heat Conduction Material, heat conduction
Material is by graphite, the concentrated sulfuric acid, hydrogen peroxide, potassium nitrate, oxidant, deionized water, hydrogenperoxide steam generator, phosphoric acid, hydrogen chloride, height
Potassium manganate forms, including following operating procedure：
The first step：The selection and placement of experimental facilities and heating device
A good chemical laboratory of environment is selected, a beaker is selected in laboratory, is placed in the bottom of beaker
The heating device to match with experiment demand needs the raw material used to put neatly, prevents in reality when being then ready for experiment
During testing, the chaotic effect for influencing experiment occurs；
Second step：Find the ratio of the raw material and reaction that prepare
The concentrated sulfuric acid and hydrogen peroxide are put into polymeric kettle, acid solution is obtained after being stirred, graphite is put into
In the acid solution arrived, acid molecule is made to be intercalation into the interlayer of graphite, obtains compound between graphite layers, can swollen graphite, then may be used
Swollen graphite is heated rapidly to 900 DEG C under the protection of argon gas, the acid molecule in graphite interlayer rapidly decompose enterprise planning in vapor and
Carbon dioxide expands synusia, obtains expanded graphite, and graphite synusia can expand tens times in vertical direction；
Third walks the reaction of Heat Conduction Material
Graphite powder is made with expanded graphite, prepares graphite powder, the potassium permanganate of the concentrated sulfuric acid and phosphoric acid sum, by graphite powder, dense
Sulfuric acid and phosphoric acid are put into beaker, and suitable ice water is then poured into beaker, after magnetic agitation, in the Gao Meng that 6g is added
Sour potassium stirs 1 hour in ice water, the ice water in beaker is then heated to 50 degrees Celsius, and water is then added into beaker, when
Water heating in beaker, is stirred 15 minutes, beaker carries out insulation reaction；
4th step Heat Conduction Material is made
The product in beaker is poured into ice water, suitable hydrogen peroxide is added while stirring, can be obtained after stirring
Graphite is put into acid solution by acid solution, can accelerate the reaction of graphite, solution can penetrate into the interlayer of graphite after acidification, just
Then product is put into centrifuge and is stirred 30 minutes until solution becomes golden yellow in the oxidation of graphite, filtering is wherein
Impurity, hydrogen chloride is then added into liquid, product is poured into and is rinsed into neutrality in deionized water, again obtained powder
Ultrasonic 8 hours are distributed in water, suspension is obtained after having filtered black residue, it is then dry in 80 degrees Celsius of environment
For 24 hours to get to graphite oxide, rotating speed of the centrifuge in whipping process is 7200 turns, and the pH value of deionized water rinsing is added about
It is seven, the graphite powder after acidification can be rinsed, using the effect of phosphoric acid, can be reduced when generating Heat Conduction Material, is generated a large amount of
Toxic gas, prevent toxic gas to be dispersed into air, influence the health of surrounding population and ecological environment, the deal of graphite powder
For 2g, the deal of the concentrated sulfuric acid is nine parts, and the deal of phosphoric acid is that the deal of a potassium permanganate is 50g, and the water in beaker should heat
To 90-100 degrees Celsius, beaker should keep the temperature twenty four hours in good environment, and four milliliters of graphite oxide aqueous solution is added,
3h is stirred by ultrasonic, you can obtain the uniform and stable graphene oxide colloid being dispersed in water, then generate Heat Conduction Material, permanganic acid
The deal that potassium is once added is 6g, and the number that potassium permanganate is added is three times, to accelerate the oxidation reaction of graphite powder in water so that
Heat Conduction Material is soluble easily in water, using the effect of graphite, can increase the heat conductivility of Heat Conduction Material, can substitute traditional heat conduction
Material improves the applicability and practicability of Heat Conduction Material.
Embodiment 1
A kind of preparation method of High-performance heat conduction material, including Heat Conduction Material, the Heat Conduction Material are by graphite, dense sulphur
Acid, hydrogen peroxide, potassium nitrate, oxidant, deionized water, hydrogenperoxide steam generator, phosphoric acid, hydrogen chloride, potassium permanganate composition, including with
Lower operating procedure：
The first step：The selection and placement of experimental facilities and heating device
A good chemical laboratory of environment is selected, a beaker is selected in laboratory, is placed in the bottom of beaker
The heating device to match with experiment demand needs the raw material used to put neatly, prevents in reality when being then ready for experiment
During testing, the chaotic effect for influencing experiment occurs；
Second step：Find the ratio of the raw material and reaction that prepare
The concentrated sulfuric acid and hydrogen peroxide are put into polymeric kettle, acid solution is obtained after being stirred, graphite is put into
In the acid solution arrived, acid molecule is made to be intercalation into the interlayer of graphite, obtains compound between graphite layers, can swollen graphite, then may be used
Swollen graphite is heated rapidly to 900 DEG C under the protection of argon gas, the acid molecule in graphite interlayer rapidly decompose enterprise planning in vapor and
Carbon dioxide expands synusia, obtains expanded graphite, and graphite synusia can expand tens times in vertical direction；
Third walks the reaction of Heat Conduction Material
Graphite powder is made with expanded graphite, prepares graphite powder, the potassium permanganate of the concentrated sulfuric acid and phosphoric acid sum, by graphite powder, dense
Sulfuric acid and phosphoric acid are put into beaker, and suitable ice water is then poured into beaker, after magnetic agitation, in the Gao Meng that 7g is added
Sour potassium stirs 30 minutes in ice water, the ice water in beaker is then heated to 50 degrees Celsius, and water is then added into beaker, when
Water heating in beaker, is stirred 15 minutes, beaker carries out insulation reaction；
4th step Heat Conduction Material is made
The product in beaker is poured into ice water, suitable hydrogen peroxide is added while stirring, can be obtained after stirring
Graphite is put into acid solution by acid solution, can accelerate the reaction of graphite, solution can penetrate into the interlayer of graphite after acidification, just
Then product is put into centrifuge and is stirred 30 minutes until solution becomes golden yellow in the oxidation of graphite, filtering is wherein
Impurity, hydrogen chloride is then added into liquid, product is poured into and is rinsed into neutrality in deionized water, again obtained powder
Ultrasonic 8 hours are distributed in water, suspension is obtained after having filtered black residue, it is then dry in 80 degrees Celsius of environment
For 24 hours to get to graphite oxide.
Embodiment 2
A kind of preparation method of High-performance heat conduction material, including Heat Conduction Material, the Heat Conduction Material are by graphite, dense sulphur
Acid, hydrogen peroxide, potassium nitrate, oxidant, deionized water, hydrogenperoxide steam generator, phosphoric acid, hydrogen chloride, potassium permanganate composition, including with
Lower operating procedure：
The first step：The selection and placement of experimental facilities and heating device
A good chemical laboratory of environment is selected, a beaker is selected in laboratory, is placed in the bottom of beaker
The heating device to match with experiment demand needs the raw material used to put neatly, prevents in reality when being then ready for experiment
During testing, the chaotic effect for influencing experiment occurs；
Second step：Find the ratio of the raw material and reaction that prepare
The concentrated sulfuric acid and hydrogen peroxide are put into polymeric kettle, acid solution is obtained after being stirred, graphite is put into
In the acid solution arrived, acid molecule is made to be intercalation into the interlayer of graphite, obtains compound between graphite layers, can swollen graphite, then may be used
Swollen graphite is heated rapidly to 900 DEG C under the protection of argon gas, the acid molecule in graphite interlayer rapidly decompose enterprise planning in vapor and
Carbon dioxide expands synusia, obtains expanded graphite, and graphite synusia can expand tens times in vertical direction；
Third walks the reaction of Heat Conduction Material
Graphite powder is made with expanded graphite, prepares graphite powder, the potassium permanganate of the concentrated sulfuric acid and phosphoric acid sum, by graphite powder, dense
Sulfuric acid and phosphoric acid are put into beaker, and suitable ice water is then poured into beaker, after magnetic agitation, in the Gao Meng that 6g is added
Sour potassium stirs 1 hour in ice water, the ice water in beaker is then heated to 50 degrees Celsius, and water is then added into beaker, when
Water heating in beaker, is stirred 15 minutes, beaker carries out insulation reaction；
4th step Heat Conduction Material is made
The product in beaker is poured into ice water, suitable hydrogen peroxide is added while stirring, can be obtained after stirring
Graphite is put into acid solution by acid solution, can accelerate the reaction of graphite, solution can penetrate into the interlayer of graphite after acidification, just
Then product is put into centrifuge and is stirred 30 minutes until solution becomes golden yellow in the oxidation of graphite, filtering is wherein
Impurity, hydrogen chloride is then added into liquid, product is poured into and is rinsed into neutrality in deionized water, again obtained powder
Ultrasonic 7 hours are distributed in water, suspension is obtained after having filtered black residue, it is then dry in 80 degrees Celsius of environment
13 hours to get to graphite oxide.
In conclusion should can obtain acid solution after stirring by the effect of the concentrated sulfuric acid and hydrogen peroxide, graphite is put into
In acid solution, the reaction of graphite can be accelerated, solution can penetrate into the interlayer of graphite after acidification, be convenient for the oxidation of graphite, utilize
The effect of oxidant, accelerating the oxidation reaction of graphite powder in water can be by the graphite powder after acidification using the effect of deionized water
Rinsing, using the effect of phosphoric acid, can reduce when generating Heat Conduction Material, generate a large amount of toxic gas, prevent toxic gas
It is dispersed into air, influences the health of surrounding population and ecological environment；Pass through the effect of hydrogen chloride so that Heat Conduction Material is soluble in
Water can increase the heat conductivility of Heat Conduction Material using the effect of graphite, can substitute traditional Heat Conduction Material, improve and lead
The applicability and practicability of hot material；Solve most Heat Conduction Material, in the production process, be added concentrated sulfuric acid etc. some
When toxic gas, a large amount of toxic gas such as dinitrogen tetroxide, chlorine dioxide etc. is will produce, when generating toxic gas, meeting
It threatens to the environment of surrounding, a large amount of toxic gas is dispersed into air, influences the problem of the health of surrounding population.
It should be noted that herein, relational terms such as first and second and the like are used merely to a reality
Body or operation are distinguished with another entity or operation, are deposited without necessarily requiring or implying between these entities or operation
In any actual relationship or order or sequence.Moreover, the terms "include", "comprise" or its any other variant are intended to
Non-exclusive inclusion, so that the process, method, article or equipment including a series of elements is not only wanted including those
Element, but also include other elements that are not explicitly listed, or further include for this process, method, article or equipment
Intrinsic element.
It although an embodiment of the present invention has been shown and described, for the ordinary skill in the art, can be with
Understanding without departing from the principles and spirit of the present invention can carry out these embodiments a variety of variations, modification, replace
And modification, the scope of the present invention is defined by the appended.
Claims (6)
1. a kind of preparation method of High-performance heat conduction material, including Heat Conduction Material, it is characterised in that：The Heat Conduction Material is by stone
Ink, the concentrated sulfuric acid, hydrogen peroxide, potassium nitrate, oxidant, deionized water, hydrogenperoxide steam generator, phosphoric acid, hydrogen chloride, potassium permanganate group
At, including following operating procedure：
The first step：The selection and placement of experimental facilities and heating device
Select a good chemical laboratory of environment, a beaker selected in laboratory, the bottom of beaker place with it is real
The heating device that the demand of testing matches needs the raw material used to put neatly, prevents from testing when being then ready for experiment
The chaotic effect for influencing experiment occurs for Cheng Zhong；
Second step：Find the ratio of the raw material and reaction that prepare
The concentrated sulfuric acid and hydrogen peroxide are put into polymeric kettle, acid solution is obtained after being stirred, graphite is put into
In acid solution, acid molecule is made to be intercalation into the interlayer of graphite, obtains compound between graphite layers, can swollen graphite, then can swollen stone
Ink is heated rapidly to 900 DEG C under the protection of argon gas, and it is in vapor and dioxy that the acid molecule in graphite interlayer, which rapidly decomposes enterprise planning,
Change carbon, synusia is expanded, expanded graphite is obtained, graphite synusia can expand tens times in vertical direction；
Third walks the reaction of Heat Conduction Material
Graphite powder is made with expanded graphite, prepares graphite powder, the potassium permanganate of the concentrated sulfuric acid and phosphoric acid sum, by graphite powder, the concentrated sulfuric acid
It is put into beaker with phosphoric acid, suitable ice water is then poured into beaker, after magnetic agitation, in the permanganic acid that 6g is added
Potassium stirs 1 hour in ice water, the ice water in beaker is then heated to 50 degrees Celsius, and water is then added into beaker, works as burning
Water heating in cup, is stirred 15 minutes, beaker carries out insulation reaction；
4th step Heat Conduction Material is made
The product in beaker is poured into ice water, suitable hydrogen peroxide is added while stirring, until solution becomes golden yellow,
Then product is put into centrifuge and is stirred 30 minutes, filtered impurity therein, hydrogen chloride is then added into liquid,
Product, which pours into, is rinsed into neutrality in deionized water, obtained powder is dispersed back into water ultrasonic 8 hours, has filtered black
Suspension is obtained after residue, it is then dry for 24 hours to get to graphite oxide in 80 degrees Celsius of environment.
2. a kind of preparation method of High-performance heat conduction material according to claim 1, it is characterised in that：The centrifuge exists
Rotating speed in whipping process is 7200 turns, and the pH value that deionized water rinsing is added is about seven.
3. a kind of preparation method of High-performance heat conduction material according to claim 1, it is characterised in that：The graphite powder
Deal is 2g, and the deal of the concentrated sulfuric acid is nine parts, and the deal of the phosphoric acid is that the deal of a potassium permanganate is 50g.
4. a kind of preparation method of High-performance heat conduction material according to claim 1, it is characterised in that：In the beaker
Water should be heated to 90-100 degrees Celsius, and the beaker should keep the temperature twenty four hours in good environment.
5. a kind of preparation method of High-performance heat conduction material according to claim 1, it is characterised in that：It is described that four millis are added
3h is stirred by ultrasonic, you can obtains the uniform and stable graphene oxide colloid being dispersed in water, then in the graphite oxide aqueous solution risen
Generate Heat Conduction Material.
6. a kind of preparation method of High-performance heat conduction material according to claim 1, it is characterised in that：The potassium permanganate
The deal being once added is 6g, and the number that the potassium permanganate is added is three times.
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| CN201810397803.3A CN108545726A (en) | 2018-04-28 | 2018-04-28 | A kind of preparation method of High-performance heat conduction material |
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Citations (3)
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| CN102897757A (en) * | 2012-10-16 | 2013-01-30 | 清华大学 | Preparation method for single-layered graphene oxide |
| US20150158729A1 (en) * | 2013-12-11 | 2015-06-11 | Enerage Inc. | Method for Manufacturing Nano-Graphene Sheets |
| CN105293476A (en) * | 2015-11-16 | 2016-02-03 | 复旦大学 | Preparation method of large-size graphene oxide or graphene |
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2018
- 2018-04-28 CN CN201810397803.3A patent/CN108545726A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102897757A (en) * | 2012-10-16 | 2013-01-30 | 清华大学 | Preparation method for single-layered graphene oxide |
| US20150158729A1 (en) * | 2013-12-11 | 2015-06-11 | Enerage Inc. | Method for Manufacturing Nano-Graphene Sheets |
| CN105293476A (en) * | 2015-11-16 | 2016-02-03 | 复旦大学 | Preparation method of large-size graphene oxide or graphene |
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| 张永康: "石墨烯的制备及其摩擦学性能研究", 《中国优秀硕士学位论文全文数据库•工程科技I辑》 * |
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Effective date of registration: 20191226 Address after: 404500 Xinjian village, Maoba Township, Yunyang County, Chongqing Applicant after: Du Haimei Address before: 241000 C1, room four, youth Pioneer Park, Wuhu road advertising industrial park, Jiujiang District, Wuhu, Anhui, Beijing Applicant before: Wuhu Sheng innovation Mstar Technology Ltd |
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Application publication date: 20180918 |