CN106117603A - A kind of preparation method of sulfenyl product carbon complex conductive fillers - Google Patents
A kind of preparation method of sulfenyl product carbon complex conductive fillers Download PDFInfo
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- CN106117603A CN106117603A CN201610469431.1A CN201610469431A CN106117603A CN 106117603 A CN106117603 A CN 106117603A CN 201610469431 A CN201610469431 A CN 201610469431A CN 106117603 A CN106117603 A CN 106117603A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/04—Carbon
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/06—Sulfur
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/08—Ingredients agglomerated by treatment with a binding agent
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/12—Adsorbed ingredients, e.g. ingredients on carriers
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/44—Carbon
- C09C1/48—Carbon black
- C09C1/56—Treatment of carbon black ; Purification
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/20—Conductive material dispersed in non-conductive organic material
- H01B1/24—Conductive material dispersed in non-conductive organic material the conductive material comprising carbon-silicon compounds, carbon or silicon
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/001—Conductive additives
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Abstract
The invention discloses the preparation method of a kind of sulfenyl product carbon complex conductive fillers, belong to conductive filler preparing technical field.The present invention is in the basic conditions, utilize microwave exposure, gumshiraz initial hydrolysis is made to prepare gumshiraz slurry standby, the methane-generating pit supernatant process petrochemical industry product carbon that recycling is acid, dissolve ash therein, white carbon black is made to obtain purification, mix with standby gumshiraz slurry, add culture propagation, make mixture have loose structure, then improved the uniformity of filler by screw extruding, add Sublimed Sulfur to be combined, making gumshiraz adhesive carbonization through calcining, remaining carbon is as skeleton, and in fixing filler, sulfur and white carbon black prepare complex conductive fillers.The invention has the beneficial effects as follows: preparation process of the present invention is simple, effectively solve because its particle diameter is thin, the bigger problem of dust in the course of processing;Preparation cost is less than additive method more than 26.3%, and products obtained therefrom good processability, electric conductivity improves 29.3~31.2%.
Description
Technical field
The present invention relates to the preparation method of a kind of sulfenyl product carbon complex conductive fillers, belong to conductive filler technology of preparing
Field.
Background technology
Along with electronic technology quickly grows, computer, radio communication are extensively applied and intensive configuration, make space fill
Scolded the electromagnetic wave of different wave length and frequency, the normal use of these Electromagnetic Interference electronic product, become the atmospheric pollution that continues,
A kind of new polluter after water pollution, sound pollution, electromagnetic pollution.Through medical evidence, electromagnetic radiation can produce 3 to organism
Plant effect: heat effect, non-thermal effect, accumulation benefit, these effects organ each to human body, tissue, system all produce in various degree
Harm, therefore cable semi-conductive shielding material arises at the historic moment.Semi-conductive shielding material is typically filled out by matrix resin, conduction
Material, cross-linking agent, antioxidant, processing aid and in right amount other additives make.Crosslinked polyetylene insulated cable semiconductive screen
Covering its dc resistivity of material shielding layers requirement is 103Below Ω cm, make to become as the high polymer of insulant partly leading
Electric material, it is necessary to be added thereto to conductive materials, such as metal dust, graphite, white carbon black etc..Integrated cost and effect, add conduction
White carbon black is the most suitable.More common conductive black is acetylene carbon black, but acetylene carbon black is due to its fine size, and dust is relatively big, processing
Poor performance, causes its cost high, and electric conductivity reduces.The conduction working out a kind of electric conductivity the most on this basis high is filled out
Material, has good development prospect and social benefit in association areas such as cables.
Summary of the invention
The technical problem to be solved: prepare semi-conductive shielding material as conductive filler for acetylene carbon black,
Due to its fine size, in the course of processing, dust is relatively big, poor processability, causes its cost high, and the drawback that electric conductivity reduces carries
Supply one in the basic conditions, utilized microwave exposure, made gumshiraz initial hydrolysis prepare gumshiraz slurry, recycling acidity
Methane-generating pit supernatant processes petrochemical industry product carbon, dissolves ash therein, makes white carbon black obtain purification, mixes with gumshiraz slurry,
Add culture propagation, make mixture have loose structure, then the uniformity by screw extruding raising filler, add Sublimed Sulfur multiple
Closing, make gumshiraz adhesive carbonization through calcining, remaining carbon is as skeleton, and in fixing filler, sulfur and white carbon black prepare composite conducting and fill out
Material, to reach to improve the purpose of its electric conductivity and processing characteristics.Preparation process of the present invention is simple, effectively solve because its particle diameter is thin,
The bigger problem of dust in the course of processing, products obtained therefrom good processability, electric conductivity is high.
For solving above-mentioned technical problem, the present invention uses the technical scheme as described below to be:
(1) gather 100~150g former gumshiraz, be placed in the beaker filling 1~2L deionized water immersion 10~20min, manually
After removing silt and bark, drain away the water, proceeded in 75~85 DEG C of baking ovens, dried 12~16h, then by dry Fructus Persicae
Natural gum is put in Universalpulverizer, grinding and sieving, collect 20~60 mesh gumshiraz powder, then be placed on fill 200~
300mL mass concentration be 4~8% sodium hydroxide solution beaker in, soak 4~6h, subsequently beaker is proceeded to microwave applicator
In, with 600~800W Power Processing 20~40min, stand, treat that it naturally cools to room temperature, obtain gumshiraz slurry, standby;
(2) collect 200~300g petrochemical industry product carbons, add in the beaker filling 1~2L methane-generating pit supernatant, then beaker is put
Testing the speed in constant temperature blender with magnetic force in digital display, be heated to 40~45 DEG C, set speed of agitator as 300~500r/min, constant temperature stirs
Mixing reaction 2~4h, sucking filtration removes filtrate, is washed with deionized soot filter cake 3~5 times, then is proceeded to 95~105 DEG C of baking ovens
In, it is dried to constant weight, pulverizes, obtain pretreatment product carbon powder;
(3) 70~90g above-mentioned gained pretreatment product carbon powder, 16~20g wheaten starches, 2~4g yeast powders are weighed successively
With 3~5g citric acids, add in the fermentation tank filling 60~80g step (1) gained gumshiraz slurries, be subsequently heated to 40~45
DEG C, start agitator, with 600~800r/min rotating speed stirring reactions 6~8h;
(4) after question response terminates, adding 15~20g Sublimed Sulfur powder, continue stirring reaction 1~2h, discharging, by gained discharging thing
Proceeding in screw extruder, controlling pressure is 6~10MPa, and discharging thing is squeezed into a diameter of 5~10mm bar, then by institute
Obtain bar and proceed in Muffle furnace, be passed through argon shield with 3~5mL/min speed, then raise temperature to 320~350 DEG C, at calcining
After reason 30~50min, cool to room temperature with the furnace, then proceeded to, in mortar, pulverize, obtain sulfenyl product carbon composite guide
Electricity filler.
The principle of the present invention: in the basic conditions, utilizes microwave exposure, makes gumshiraz initial hydrolysis prepare peach tree rubber cement
Material, the binding agent as filler is standby, the methane-generating pit supernatant process petrochemical industry product carbon that recycling is acid, dissolves ash therein
Point, make white carbon black obtain purification, mix with standby gumshiraz slurry, add culture propagation and produce, make mixture have loose structure,
Improved the uniformity of filler again by screw extruding, add Sublimed Sulfur composite strengthening filler electric conductivity, make gumshiraz glue through calcining
Glutinous agent carbonization, remaining carbon is as skeleton, and in fixing filler, sulfur and white carbon black prepare complex conductive fillers.
The application process of the present invention: the sulfenyl product carbon complex conductive fillers present invention prepared adds to semiconductive screen
Covering material and prepare in raw material, addition is raw material gross mass 25~30%, prepares semi-conductive shielding material.This conductive filler is processed
Performance is good, and electric conductivity improves 29.3~31.2%, product electrical conductivity be 1.5 × 10-1~3.2 × 10S/cm, at 23 DEG C
Specific insulation≤98.5 Ω cm, is worthy to be popularized and uses.
The present invention is compared with additive method, and Advantageous Effects is:
(1) preparation process of the present invention is simple, effectively solves because its particle diameter is thin, the bigger problem of dust in the course of processing;
(2) preparation cost be less than additive method more than 26.3%, products obtained therefrom good processability, electric conductivity improve 29.3~
31.2%。
Detailed description of the invention
First gather 100~150g former gumshiraz, be placed in the beaker filling 1~2L deionized water immersion 10~20min,
After artificial removing silt and bark, drain away the water, proceeded in 75~85 DEG C of baking ovens, dried 12~16h, then will be dried
Gumshiraz put in Universalpulverizer, grinding and sieving, collect 20~60 mesh gumshiraz powder, then be placed on and fill 200
~300mL mass concentration be 4~8% sodium hydroxide solution beaker in, soak 4~6h, subsequently beaker is proceeded to microwave applicator
In, with 600~800W Power Processing 20~40min, stand, treat that it naturally cools to room temperature, obtain gumshiraz slurry, standby;So
Rear collection 200~300g petrochemical industry product carbon, adds in the beaker filling 1~2L methane-generating pit supernatant, then beaker is placed in number
Aobvious testing the speed in constant temperature blender with magnetic force, be heated to 40~45 DEG C, sets speed of agitator as 300~500r/min, constant temperature stirring is instead
Answering 2~4h, sucking filtration removes filtrate, is washed with deionized soot filter cake 3~5 times, then is proceeded in 95~105 DEG C of baking ovens,
It is dried to constant weight, pulverizes, obtain pretreatment product carbon powder;Weigh 70~90g above-mentioned gained pretreatment the most successively secondary
Produce hydrocarbon black powder, 16~20g wheaten starches, 2~4g yeast powders and 3~5g citric acids, add and fill 60~80g gained gumshiraz
In the fermentation tank of slurry, be subsequently heated to 40~45 DEG C, start agitator, with 600~800r/min rotating speeds stirring reaction 6~
8h;After last question response terminates, adding 15~20g Sublimed Sulfur powder, continue stirring reaction 1~2h, discharging, by gained discharging thing
Proceeding in screw extruder, controlling pressure is 6~10MPa, and discharging thing is squeezed into a diameter of 5~10mm bar, then by institute
Obtain bar and proceed in Muffle furnace, be passed through argon shield with 3~5mL/min speed, then raise temperature to 320~350 DEG C, at calcining
After reason 30~50min, cool to room temperature with the furnace, then proceeded to, in mortar, pulverize, obtain sulfenyl product carbon composite guide
Electricity filler.
Example 1
First gather the former gumshiraz of 100g, be placed in the beaker filling 1L deionized water immersion 10min, artificial removing silt and tree
Pi Hou, drains away the water, and is proceeded in 75 DEG C of baking ovens, dried 12h, drier gumshiraz is put into Universalpulverizer
In, grinding and sieving, collect 20 mesh gumshiraz powder, then be placed on that to fill 200mL mass concentration be 4% sodium hydroxide solution
Beaker in, soak 4h, subsequently beaker proceeded in microwave applicator, with 600W Power Processing 20min, stand, treat that it is natural
It is cooled to room temperature, obtains gumshiraz slurry, standby;Then collect 200g petrochemical industry product carbon, add and fill 1L methane-generating pit supernatant
Beaker in, then beaker be placed in digital display test the speed in constant temperature blender with magnetic force, be heated to 40 DEG C, set speed of agitator as 300r/
Min, constant temperature stirring reaction 2h, sucking filtration removes filtrate, is washed with deionized soot filter cake 3 times, then is proceeded to 95 DEG C of baking ovens
In, it is dried to constant weight, pulverizes, obtain pretreatment product carbon powder;Weigh 70g above-mentioned gained pretreatment by-product the most successively
Hydrocarbon black powder, 16g wheaten starch, 2g yeast powder and 3g citric acid, add in the fermentation tank filling 60g gained gumshiraz slurry,
It is subsequently heated to 40 DEG C, starts agitator, with 600r/min rotating speed stirring reaction 6h;After last question response terminates, add 15g liter
China's sulfur powder, continues stirring reaction 1h, discharging, proceeds in screw extruder by gained discharging thing, and control pressure is 6MPa, will go out
Material thing is squeezed into a diameter of 5mm bar, then proceeds in Muffle furnace by gained bar, is passed through argon with 3mL/min speed and protects
Protect, then raise temperature to 320 DEG C, after calcination processing 30min, cool to room temperature with the furnace, then proceeded to, in mortar, pulverize,
Obtain sulfenyl product carbon complex conductive fillers.
The sulfenyl product carbon complex conductive fillers interpolation present invention prepared is prepared in raw material to semi-conductive shielding material,
Addition is raw material gross mass 25%, prepares semi-conductive shielding material.This conductive filler good processability, electric conductivity improves
29.3%, product electrical conductivity be 1.5 × 10-1S/cm, is 98.5 Ω cm 23 DEG C of lower volume resistivity, be worthy to be popularized with
Use.
Example 2
First gather the former gumshiraz of 125g, be placed in the beaker filling 2L deionized water immersion 15min, artificial removing silt and tree
Pi Hou, drains away the water, and is proceeded in 80 DEG C of baking ovens, dried 14h, drier gumshiraz is put into Universalpulverizer
In, grinding and sieving, collect 40 mesh gumshiraz powder, then be placed on that to fill 250mL mass concentration be 6% sodium hydroxide solution
Beaker in, soak 5h, subsequently beaker proceeded in microwave applicator, with 700W Power Processing 30min, stand, treat that it is natural
It is cooled to room temperature, obtains gumshiraz slurry, standby;Then collect 250g petrochemical industry product carbon, add and fill 2L methane-generating pit supernatant
Beaker in, then beaker be placed in digital display test the speed in constant temperature blender with magnetic force, be heated to 43 DEG C, set speed of agitator as 400r/
Min, constant temperature stirring reaction 3h, sucking filtration removes filtrate, is washed with deionized soot filter cake 4 times, then is proceeded to 100 DEG C of baking ovens
In, it is dried to constant weight, pulverizes, obtain pretreatment product carbon powder;Weigh 80g above-mentioned gained pretreatment by-product the most successively
Hydrocarbon black powder, 18g wheaten starch, 3g yeast powder and 4g citric acid, add in the fermentation tank filling 70g gained gumshiraz slurry,
It is subsequently heated to 43 DEG C, starts agitator, with 700r/min rotating speed stirring reaction 7h;After last question response terminates, add 18g liter
China's sulfur powder, continues stirring reaction 2h, discharging, proceeds in screw extruder by gained discharging thing, and control pressure is 8MPa, will go out
Material thing is squeezed into a diameter of 8mm bar, then proceeds in Muffle furnace by gained bar, is passed through argon with 4mL/min speed and protects
Protect, then raise temperature to 335 DEG C, after calcination processing 40min, cool to room temperature with the furnace, then proceeded to, in mortar, pulverize,
Obtain sulfenyl product carbon complex conductive fillers.
The sulfenyl product carbon complex conductive fillers interpolation present invention prepared is prepared in raw material to semi-conductive shielding material,
Addition is raw material gross mass 28%, prepares semi-conductive shielding material.This conductive filler good processability, electric conductivity improves
30.4%, product electrical conductivity be 1.2 × 10S/cm, be 101.5 Ω cm 23 DEG C of lower volume resistivity, be worthy to be popularized with
Use.
Example 3
First gather the former gumshiraz of 150g, be placed in the beaker filling 2L deionized water immersion 20min, artificial removing silt and tree
Pi Hou, drains away the water, and is proceeded in 85 DEG C of baking ovens, dried 16h, drier gumshiraz is put into Universalpulverizer
In, grinding and sieving, collect 60 mesh gumshiraz powder, then be placed on that to fill 300mL mass concentration be 8% sodium hydroxide solution
Beaker in, soak 6h, subsequently beaker proceeded in microwave applicator, with 800W Power Processing 40min, stand, treat that it is natural
It is cooled to room temperature, obtains gumshiraz slurry, standby;Then collect 300g petrochemical industry product carbon, add and fill 2L methane-generating pit supernatant
Beaker in, then beaker be placed in digital display test the speed in constant temperature blender with magnetic force, be heated to 45 DEG C, set speed of agitator as 500r/
Min, constant temperature stirring reaction 4h, sucking filtration removes filtrate, is washed with deionized soot filter cake 5 times, then is proceeded to 105 DEG C of baking ovens
In, it is dried to constant weight, pulverizes, obtain pretreatment product carbon powder;Weigh 90g above-mentioned gained pretreatment by-product the most successively
Hydrocarbon black powder, 20g wheaten starch, 4g yeast powder and 5g citric acid, add in the fermentation tank filling 80g gained gumshiraz slurry,
It is subsequently heated to 45 DEG C, starts agitator, with 800r/min rotating speed stirring reaction 8h;After last question response terminates, add 20g liter
China's sulfur powder, continues stirring reaction 2h, discharging, proceeds in screw extruder by gained discharging thing, and control pressure is 10MPa, will
Discharging thing is squeezed into a diameter of 10mm bar, then proceeds in Muffle furnace by gained bar, is passed through argon with 5mL/min speed
Protection, then raises temperature to 350 DEG C, after calcination processing 50min, cools to room temperature with the furnace, then proceeded to, in mortar, grind to form
Powder, obtains sulfenyl product carbon complex conductive fillers.
The sulfenyl product carbon complex conductive fillers interpolation present invention prepared is prepared in raw material to semi-conductive shielding material,
Addition is raw material gross mass 30%, prepares semi-conductive shielding material.This conductive filler good processability, electric conductivity improves
31.2%, product electrical conductivity be 3.2 × 10S/cm, be 103.2 Ω cm 23 DEG C of lower volume resistivity, be worthy to be popularized with
Use.
Claims (1)
1. the preparation method of a sulfenyl product carbon complex conductive fillers, it is characterised in that concrete preparation process is:
(1) gather 100~150g former gumshiraz, be placed in the beaker filling 1~2L deionized water immersion 10~20min, manually
After removing silt and bark, drain away the water, proceeded in 75~85 DEG C of baking ovens, dried 12~16h, then by dry Fructus Persicae
Natural gum is put in Universalpulverizer, grinding and sieving, collect 20~60 mesh gumshiraz powder, then be placed on fill 200~
300mL mass concentration be 4~8% sodium hydroxide solution beaker in, soak 4~6h, subsequently beaker is proceeded to microwave applicator
In, with 600~800W Power Processing 20~40min, stand, treat that it naturally cools to room temperature, obtain gumshiraz slurry, standby;
(2) collect 200~300g petrochemical industry product carbons, add in the beaker filling 1~2L methane-generating pit supernatant, then beaker is put
Testing the speed in constant temperature blender with magnetic force in digital display, be heated to 40~45 DEG C, set speed of agitator as 300~500r/min, constant temperature stirs
Mixing reaction 2~4h, sucking filtration removes filtrate, is washed with deionized soot filter cake 3~5 times, then is proceeded to 95~105 DEG C of baking ovens
In, it is dried to constant weight, pulverizes, obtain pretreatment product carbon powder;
(3) 70~90g above-mentioned gained pretreatment product carbon powder, 16~20g wheaten starches, 2~4g yeast powders are weighed successively
With 3~5g citric acids, add in the fermentation tank filling 60~80g step (1) gained gumshiraz slurries, be subsequently heated to 40~45
DEG C, start agitator, with 600~800r/min rotating speed stirring reactions 6~8h;
(4) after question response terminates, adding 15~20g Sublimed Sulfur powder, continue stirring reaction 1~2h, discharging, by gained discharging thing
Proceeding in screw extruder, controlling pressure is 6~10MPa, and discharging thing is squeezed into a diameter of 5~10mm bar, then by institute
Obtain bar and proceed in Muffle furnace, be passed through argon shield with 3~5mL/min speed, then raise temperature to 320~350 DEG C, at calcining
After reason 30~50min, cool to room temperature with the furnace, then proceeded to, in mortar, pulverize, obtain sulfenyl product carbon composite guide
Electricity filler.
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Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
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CN104779379A (en) * | 2014-12-31 | 2015-07-15 | 山东玉皇新能源科技有限公司 | Novel sulfur and carbon composite material for lithium secondary battery, and preparation method thereof |
CN104904044A (en) * | 2012-12-05 | 2015-09-09 | 中国科学院化学研究所 | Sulfur-carbon composite material, application of sulfur-carbon composite material in lithium-sulfur battery and method for producing the composite material |
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2016
- 2016-06-25 CN CN201610469431.1A patent/CN106117603A/en active Pending
Patent Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
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CN104904044A (en) * | 2012-12-05 | 2015-09-09 | 中国科学院化学研究所 | Sulfur-carbon composite material, application of sulfur-carbon composite material in lithium-sulfur battery and method for producing the composite material |
CN104779379A (en) * | 2014-12-31 | 2015-07-15 | 山东玉皇新能源科技有限公司 | Novel sulfur and carbon composite material for lithium secondary battery, and preparation method thereof |
Non-Patent Citations (1)
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孙建生等译: "《电力电缆工程(原书第3版)》", 30 November 2014, 机械工业出版社 * |
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