CN110002436A - A kind of high purity graphite alkene conducting particles and its process for producing - Google Patents
A kind of high purity graphite alkene conducting particles and its process for producing Download PDFInfo
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- CN110002436A CN110002436A CN201910351816.1A CN201910351816A CN110002436A CN 110002436 A CN110002436 A CN 110002436A CN 201910351816 A CN201910351816 A CN 201910351816A CN 110002436 A CN110002436 A CN 110002436A
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- 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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Abstract
The present invention relates to the preparation technical fields of chemical material, the invention discloses a kind of high purity graphite alkene conducting particles and its process for producing, include the steps that the selection and weighing and the mixing of raw material, heating, drying and washing of raw material, this kind of graphene-based conducting particles, the graphene-based conducting particles of graphene-based conducting particles preparation method preparation are with high purity, and operating procedure is detailed, difficulty is small, and the cost of preparation is low.
Description
Technical field
The present invention relates to the preparation technical field of chemical material more particularly to a kind of high purity graphite alkene conducting particles and its
Process for producing.
Background technique
It is graphene-based to be used as a kind of novel conductive wire material, it is used in terms of battery electrode material, good conductivity, it is existing
It is pure when thering is a kind of high purity graphite alkenyl conducting particles in the market and a kind of high purity graphite alkenyl conducting particles to prepare
Not high, and complex steps and fuzzy are spent, the difficulty of operation is larger, therefore is unfavorable for promoting.
Summary of the invention
The invention proposes a kind of high purity graphite alkene conducting particles and its process for producing, to solve above-mentioned background skill
The problem of being proposed in art.
The invention proposes a kind of high purity graphite alkene conducting particles, raw material matches as follows in parts by weight: graphite powder
60-70 parts, 30-35 parts of potassium peroxydisulfate, 20-30 parts of phosphorus pentoxide, 60-80% concentration 20-30 parts of the concentrated sulfuric acid, potassium permanganate
20-25 parts, 30-40 parts of deionized water, 15-20 parts of hydrochloric acid, 30-40 parts of hydrogen peroxide solution, 1-3 parts of sodium borohydride, surface-active
1-3 parts of agent and 3-5 parts of conductive black.
A kind of high purity graphite alkenyl conducting particles process for producing, steps are as follows:
M1, the 60-80% that one third is added in graphite powder, potassium peroxydisulfate and phosphorus pentoxide according to the weight ratio are dense
In the concentrated sulfuric acid of degree, and after stirring 3-5 minutes, table is added between 60-70 degrees Celsius in the concentrated sulfuric acid temperature of 60-80% concentration
Face activating agent and conductive black, are again stirring for, after stirring, after 3-5 hours cooling, and washing to neutrality, and it is dry；
M2, the sample after drying is put into 2/3rds concentrated sulfuric acid of 60-80% concentration, and the temperature control of the concentrated sulfuric acid
System adds potassium permanganate, the temperature of mixture is maintained at 0-20 degrees Celsius within 0-10 degrees Celsius；
M3, the vessel for holding mixture are placed in 36-40 degrees Celsius of oil bath, 3-5 hours are kept the temperature, in the mistake of heat preservation
Cheng Zhong is slowly added to 1/5th deionized water into vessel；
M4, be added 1/5th deionized water 8-12 minute after, by remaining deionized water and hydrogen peroxide solution
Mixing, mixed solution is all poured into the vessel for filling mixture, is filtered while hot；
M5, the mixture in M4 is washed using dilute hydrochloric acid solution, by being put into 500ML three-necked bottle for acquisition, water
Bath heating, temperature are controlled at 90-100 degrees Celsius, and sodium borohydride is added, until there is flocculent deposit appearance, are stopped heating, are carried out
It is dry, obtain a kind of high purity graphite alkenyl conducting particles powder；
M6, to high purity graphite alkenyl conducting particles powder obtained in M5 and resin-oatmeal, infrared enhancing powder, conductive black
Powder, the auxiliary agents such as coupling agent, surfactant, dispersing agent, antioxidant are mixed, ultrasonic disperse；It is squeezed out, is granulated by extruder again
Machine is granulated, and finally obtains a kind of high purity graphite alkenyl conducting particles.
A kind of high purity graphite alkene conducting particles, raw material match as follows in parts by weight: 30-35 parts of graphite powder, over cure
Sour potassium 15-20 parts, 10-15 parts of phosphorus pentoxide, 1-3 parts of sodium borohydride, 15-20 parts of deionized water, 20-25 parts of hydrogen peroxide solution
And 10-15 parts of the concentrated sulfuric acid of 30-40% concentration.
A kind of high purity graphite alkenyl conducting particles process for producing, steps are as follows:
H1, the 30-40% that one third is added in graphite powder, potassium peroxydisulfate and phosphorus pentoxide according to the weight ratio are dense
In the concentrated sulfuric acid of degree, and the concentrated sulfuric acid temperature of 30-40% concentration, between 60-70 degrees Celsius, after stirring 3-5 minutes, stirring is tied
Shu Hou, after 3-5 hours cooling, washing to neutrality, and it is dry；
H2, M2, the sample after drying is put into 2/3rds concentrated sulfuric acid of 30-40% concentration, and the temperature of the concentrated sulfuric acid
Degree control is within 0-10 degrees Celsius；
H3, the vessel for holding mixture are placed in 36-40 degrees Celsius of oil bath, 3-5 hours are kept the temperature, in the mistake of heat preservation
Cheng Zhong is slowly added to 1/5th deionized water into vessel；
H4, be added 1/5th deionized water 8-12 minute after, by remaining deionized water and hydrogen peroxide solution
Mixing, mixed solution is all poured into the vessel for filling mixture, is filtered while hot；
H5, the mixed solution obtained in H4 is put into 500ML three-necked bottle, heating water bath, temperature control is taken the photograph in 90-100
Sodium borohydride is added in family name's degree, until there is flocculent deposit appearance, stops heating, is dried, obtains a kind of high purity graphite alkene
Base conducting particles powder；
H6, to high purity graphite alkenyl conducting particles powder obtained in H5 and resin-oatmeal, infrared enhancing powder, conductive black
Powder, the auxiliary agents such as coupling agent, surfactant, dispersing agent, antioxidant are mixed, ultrasonic disperse；It is squeezed out, is granulated by extruder again
Machine is granulated, and finally obtains a kind of high purity graphite alkenyl conducting particles.
Preferably, which should carry out in dustless laboratory, and the temperature control in laboratory
At 20-24 degrees Celsius.
Preferably, during preparation, raw material is poured into the concentrated sulfuric acid in solution, needs to be poured slowly into, avoids raw material
It splashes after being contacted with the concentrated sulfuric acid.
Preferably, when carrying out H5 or M5 step, after occurring flocculent deposit in three-necked bottle, mixture is poured out, is utilized
Sieve is filtered, and after filtering, is being dried.
A kind of high purity graphite alkene conducting particles proposed by the present invention and its process for producing, beneficial effect are, are somebody's turn to do
The graphene-based conducting particles of kind, the graphene-based conducting particles of graphene-based conducting particles preparation method preparation are with high purity, and grasp
It is detailed to make step, difficulty is small.
Specific embodiment
It is next combined with specific embodiments below that the present invention will be further described.
Embodiment 1
A kind of high purity graphite alkene conducting particles, raw material match as follows in parts by weight: 60 parts of graphite powder, potassium peroxydisulfate
30 parts, 20 parts of phosphorus pentoxide, 20 parts of 20 parts of the concentrated sulfuric acid, the potassium permanganate of 60% concentration, 30 parts of deionized water, 15 parts of hydrochloric acid,
30 parts of hydrogen peroxide solution, 1 part of sodium borohydride, 1 part of surfactant and 3 parts of conductive black.
A kind of high purity graphite alkenyl conducting particles process for producing, steps are as follows:
M1,60% concentration that graphite powder, potassium peroxydisulfate and phosphorus pentoxide are added to one third according to the weight ratio
The concentrated sulfuric acid in, and the concentrated sulfuric acid temperature of 60% concentration is between 60 degrees Celsius, after stirring 3 minutes, be added surfactant with
And conductive black, it is again stirring for, after stirring, after 4 hours cooling, washing to neutrality, and it is dry；
M2, the sample after drying is put into 2/3rds concentrated sulfuric acid of 60% concentration, and the temperature control of the concentrated sulfuric acid
Within 4 degrees Celsius, potassium permanganate is added, the temperature of mixture is maintained at 10 degrees Celsius；
M3, the vessel for holding mixture are placed in 38 degrees Celsius of oil bath, keep the temperature 4 hours, during heat preservation,
/ 5th deionized water is slowly added into vessel；
M4, after 9 minutes of deionized water of 1/5th are added, remaining deionized water is mixed with hydrogen peroxide solution
It closes, mixed solution is all poured into the vessel for filling mixture, is filtered while hot；
M5, the mixture in M4 is washed using dilute hydrochloric acid solution, by being put into 500ML three-necked bottle for acquisition, water
Bath heating, temperature are controlled at 93 degrees Celsius, and sodium borohydride is added, until there is flocculent deposit appearance, are stopped heating, are done
It is dry, obtain a kind of high purity graphite alkenyl conducting particles powder；
M6, to high purity graphite alkenyl conducting particles powder obtained in M5 and resin-oatmeal, infrared enhancing powder, conductive black
Powder, the auxiliary agents such as coupling agent, surfactant, dispersing agent, antioxidant are mixed, ultrasonic disperse；It is squeezed out, is granulated by extruder again
Machine is granulated, and finally obtains a kind of high purity graphite alkenyl conducting particles.
A kind of high purity graphite alkene conducting particles, raw material match as follows in parts by weight: 30 parts of graphite powder, potassium peroxydisulfate
16 parts, 12 parts of phosphorus pentoxide, 1 part of sodium borohydride, 17 parts of deionized water, 22 parts of hydrogen peroxide solution and 30% concentration dense sulphur
12 parts of acid.
A kind of high purity graphite alkenyl conducting particles process for producing, steps are as follows:
H1,30% concentration that graphite powder, potassium peroxydisulfate and phosphorus pentoxide are added to one third according to the weight ratio
The concentrated sulfuric acid in, and the concentrated sulfuric acid temperature of 30% concentration is between 62 degrees Celsius, cooling after stirring after stirring 4 minutes
After 3.5 hours, washing to neutrality, and it is dry；
H2, M2, the sample after drying is put into 2/3rds concentrated sulfuric acid of 30% concentration, and the temperature control of the concentrated sulfuric acid
System is at 7 degrees Celsius；
H3, the vessel for holding mixture are placed in 37 degrees Celsius of oil bath, keep the temperature 4 hours, during heat preservation,
/ 5th deionized water is slowly added into vessel；
H4, after 11 minutes of deionized water of 1/5th are added, remaining deionized water is mixed with hydrogen peroxide solution
It closes, mixed solution is all poured into the vessel for filling mixture, is filtered while hot；
H5, the mixed solution obtained in H4 being put into 500ML three-necked bottle, heating water bath, temperature is controlled at 97 degrees Celsius,
Sodium borohydride is added, until there is flocculent deposit appearance, stops heating, is dried, obtains a kind of high purity graphite alkenyl and leads
Charged particle powder；
H6, to high purity graphite alkenyl conducting particles powder obtained in H5 and resin-oatmeal, infrared enhancing powder, conductive black
Powder, the auxiliary agents such as coupling agent, surfactant, dispersing agent, antioxidant are mixed, ultrasonic disperse；It is squeezed out, is granulated by extruder again
Machine is granulated, and finally obtains a kind of high purity graphite alkenyl conducting particles.
The process for producing process should carry out in dustless laboratory, and the temperature control in laboratory is Celsius 22
Degree.
During preparation, raw material is poured into the concentrated sulfuric acid in solution, needs to be poured slowly into, avoids raw material and the concentrated sulfuric acid
It splashes after contact.
When carrying out H5 or M5 step, after occurring flocculent deposit in three-necked bottle, mixture is poured out, is carried out using sieve
Filtering, after filtering, is being dried.
As there is high oxidative reagent as potassium permanganate, the concentrated sulfuric acid and hydrogen peroxide in raw material, to need to operate
Personnel wear the preparation that relevant use for laboratory anticorrosion clothing is tested, and before entering laboratory, several operators
Mutually check whether clothing is worn neatly.
Embodiment 2
A kind of high purity graphite alkene conducting particles, raw material match as follows in parts by weight: 65 parts of graphite powder, potassium peroxydisulfate
33 parts, 25 parts of phosphorus pentoxide, 22 parts of 23 parts of the concentrated sulfuric acid, the potassium permanganate of 70% concentration, 36 parts of deionized water, 17 parts of hydrochloric acid,
37 parts of hydrogen peroxide solution, 2 parts of sodium borohydride, 2 parts of surfactant and 4 parts of conductive black.
A kind of high purity graphite alkenyl conducting particles process for producing, steps are as follows:
M1,70% concentration that graphite powder, potassium peroxydisulfate and phosphorus pentoxide are added to one third according to the weight ratio
The concentrated sulfuric acid in, and the concentrated sulfuric acid temperature of 70% concentration is between 65 degrees Celsius, after stirring 4 minutes, be added surfactant with
And conductive black, it is again stirring for, after stirring, after 4 hours cooling, washing to neutrality, and it is dry；
M2, the sample after drying is put into 2/3rds concentrated sulfuric acid of 70% concentration, and the temperature control of the concentrated sulfuric acid
Within 4 degrees Celsius, potassium permanganate is added, the temperature of mixture is maintained at 16 degrees Celsius；
M3, the vessel for holding mixture are placed in 38 degrees Celsius of oil bath, 3.5 hours are kept the temperature, in the process of heat preservation
In, 1/5th deionized water is slowly added into vessel；
M4, after 9 minutes of deionized water of 1/5th are added, remaining deionized water is mixed with hydrogen peroxide solution
It closes, mixed solution is all poured into the vessel for filling mixture, is filtered while hot；
M5, the mixture in M4 is washed using dilute hydrochloric acid solution, by being put into 500ML three-necked bottle for acquisition, water
Bath heating, temperature are controlled at 94 degrees Celsius, and sodium borohydride is added, until there is flocculent deposit appearance, are stopped heating, are done
It is dry, obtain a kind of high purity graphite alkenyl conducting particles powder；
M6, to high purity graphite alkenyl conducting particles powder obtained in M5 and resin-oatmeal, infrared enhancing powder, conductive black
Powder, the auxiliary agents such as coupling agent, surfactant, dispersing agent, antioxidant are mixed, ultrasonic disperse；It is squeezed out, is granulated by extruder again
Machine is granulated, and finally obtains a kind of high purity graphite alkenyl conducting particles.
A kind of high purity graphite alkene conducting particles, raw material match as follows in parts by weight: 32 parts of graphite powder, potassium peroxydisulfate
18 parts, 13 parts of phosphorus pentoxide, 2 parts of sodium borohydride, 18 parts of deionized water, 23 parts of hydrogen peroxide solution and 35% concentration dense sulphur
14 parts of acid.
A kind of high purity graphite alkenyl conducting particles process for producing, steps are as follows:
H1,35% concentration that graphite powder, potassium peroxydisulfate and phosphorus pentoxide are added to one third according to the weight ratio
The concentrated sulfuric acid in, and the concentrated sulfuric acid temperature of 35% concentration is between 66 degrees Celsius, cooling after stirring after stirring 4.5 minutes
After 4 hours, washing to neutrality, and it is dry；
H2, M2, the sample after drying is put into 2/3rds concentrated sulfuric acid of 35% concentration, and the temperature control of the concentrated sulfuric acid
System is at 8 degrees Celsius；
H3, the vessel for holding mixture are placed in 38 degrees Celsius of oil bath, keep the temperature 4 hours, during heat preservation,
/ 5th deionized water is slowly added into vessel；
H4, after 11 minutes of deionized water of 1/5th are added, remaining deionized water is mixed with hydrogen peroxide solution
It closes, mixed solution is all poured into the vessel for filling mixture, is filtered while hot；
H5, the mixed solution obtained in H4 being put into 500ML three-necked bottle, heating water bath, temperature is controlled at 96 degrees Celsius,
Sodium borohydride is added, until there is flocculent deposit appearance, stops heating, is dried, obtains a kind of high purity graphite alkenyl and leads
Charged particle powder；
H6, to high purity graphite alkenyl conducting particles powder obtained in H5 and resin-oatmeal, infrared enhancing powder, conductive black
Powder, the auxiliary agents such as coupling agent, surfactant, dispersing agent, antioxidant are mixed, ultrasonic disperse；It is squeezed out, is granulated by extruder again
Machine is granulated, and finally obtains a kind of high purity graphite alkenyl conducting particles.
Preferably, which should carry out in dustless laboratory, and the temperature control in laboratory
At 22 degrees Celsius.
Preferably, during preparation, raw material is poured into the concentrated sulfuric acid in solution, needs to be poured slowly into, avoids raw material
It splashes after being contacted with the concentrated sulfuric acid.
Preferably, when carrying out H5 or M5 step, after occurring flocculent deposit in three-necked bottle, mixture is poured out, is utilized
Sieve is filtered, and after filtering, is being dried.
Embodiment 3
A kind of high purity graphite alkene conducting particles, raw material match as follows in parts by weight: 68 parts of graphite powder, potassium peroxydisulfate
34 parts, 28 parts of phosphorus pentoxide, 24 parts of 22 parts of the concentrated sulfuric acid, the potassium permanganate of 80% concentration, 33 parts of deionized water, 18 parts of hydrochloric acid,
40 parts of hydrogen peroxide solution, 2.5 parts of sodium borohydride, 3 parts of surfactant and 3 parts of conductive black.
A kind of high purity graphite alkenyl conducting particles process for producing, steps are as follows:
M1,80% concentration that graphite powder, potassium peroxydisulfate and phosphorus pentoxide are added to one third according to the weight ratio
The concentrated sulfuric acid in, and the concentrated sulfuric acid temperature of 80% concentration is between 68 degrees Celsius, and after stirring 4.5 minutes, surfactant is added
And conductive black, it is again stirring for, after stirring, after 5 hours cooling, washing to neutrality, and it is dry；
M2, the sample after drying is put into 2/3rds concentrated sulfuric acid of 80% concentration, and the temperature control of the concentrated sulfuric acid
Within 9 degrees Celsius, potassium permanganate is added, the temperature of mixture is maintained at 17 degrees Celsius；
M3, the vessel for holding mixture are placed in 39 degrees Celsius of oil bath, keep the temperature 5 hours, during heat preservation,
/ 5th deionized water is slowly added into vessel；
M4, after 11 minutes of deionized water of 1/5th are added, remaining deionized water is mixed with hydrogen peroxide solution
It closes, mixed solution is all poured into the vessel for filling mixture, is filtered while hot；
M5, the mixture in M4 is washed using dilute hydrochloric acid solution, by being put into 500ML three-necked bottle for acquisition, water
Bath heating, temperature are controlled at 98 degrees Celsius, and sodium borohydride is added, until there is flocculent deposit appearance, are stopped heating, are done
It is dry, obtain a kind of high purity graphite alkenyl conducting particles powder；
M6, to high purity graphite alkenyl conducting particles powder obtained in M5 and resin-oatmeal, infrared enhancing powder, conductive black
Powder, the auxiliary agents such as coupling agent, surfactant, dispersing agent, antioxidant are mixed, ultrasonic disperse；It is squeezed out, is granulated by extruder again
Machine is granulated, and finally obtains a kind of high purity graphite alkenyl conducting particles.
A kind of high purity graphite alkene conducting particles, raw material match as follows in parts by weight: 34 parts of graphite powder, potassium peroxydisulfate
18 parts, 14 parts of phosphorus pentoxide, 3 parts of sodium borohydride, 20 parts of deionized water, 23 parts of hydrogen peroxide solution and 40% concentration dense sulphur
14 parts of acid.
A kind of high purity graphite alkenyl conducting particles process for producing, steps are as follows:
H1,40% concentration that graphite powder, potassium peroxydisulfate and phosphorus pentoxide are added to one third according to the weight ratio
The concentrated sulfuric acid in, and the concentrated sulfuric acid temperature of 40% concentration is between 70 degrees Celsius, after stirring 4 minutes, after stirring, cooling 5
After hour, washing to neutrality, and it is dry；
H2, M2, the sample after drying is put into 2/3rds concentrated sulfuric acid of 40% concentration, and the temperature control of the concentrated sulfuric acid
System is at 10 degrees Celsius；
H3, the vessel for holding mixture are placed in 38 degrees Celsius of oil bath, keep the temperature 4 hours, during heat preservation,
/ 5th deionized water is slowly added into vessel；
H4, be added 1/5th deionized water after ten minutes, remaining deionized water is mixed with hydrogen peroxide solution
It closes, mixed solution is all poured into the vessel for filling mixture, is filtered while hot；
H5, the mixed solution obtained in H4 being put into 500ML three-necked bottle, heating water bath, temperature is controlled at 98 degrees Celsius,
Sodium borohydride is added, until there is flocculent deposit appearance, stops heating, is dried, obtains a kind of high purity graphite alkenyl and leads
Charged particle powder；
H6, to high purity graphite alkenyl conducting particles powder obtained in H5 and resin-oatmeal, infrared enhancing powder, conductive black
Powder, the auxiliary agents such as coupling agent, surfactant, dispersing agent, antioxidant are mixed, ultrasonic disperse；It is squeezed out, is granulated by extruder again
Machine is granulated, and finally obtains a kind of high purity graphite alkenyl conducting particles.
Preferably, which should carry out in dustless laboratory, and the temperature control in laboratory
At 24 degrees Celsius.
Preferably, during preparation, raw material is poured into the concentrated sulfuric acid in solution, needs to be poured slowly into, avoids raw material
It splashes after being contacted with the concentrated sulfuric acid.
Preferably, when carrying out H5 or M5 step, after occurring flocculent deposit in three-necked bottle, mixture is poured out, is utilized
Sieve is filtered, and after filtering, is being dried.
The foregoing is only a preferred embodiment of the present invention, but scope of protection of the present invention is not limited thereto,
Anyone skilled in the art in the technical scope disclosed by the present invention, according to the technique and scheme of the present invention and its
Inventive concept is subject to equivalent substitution or change, should be covered by the protection scope of the present invention.
Claims (7)
1. a kind of high purity graphite alkene conducting particles, which is characterized in that its raw material matches as follows in parts by weight: graphite powder 60-
70 parts, 30-35 parts of potassium peroxydisulfate, 20-30 parts of phosphorus pentoxide, 60-80% concentration 20-30 parts of the concentrated sulfuric acid, potassium permanganate 20-
25 parts, 30-40 parts of deionized water, 15-20 parts of hydrochloric acid, 30-40 parts of hydrogen peroxide solution, 1-3 parts of sodium borohydride, surfactant 1-
3 parts and 3-5 parts of conductive black.
2. a kind of high purity graphite alkenyl conducting particles process for producing according to claim 1, which is characterized in that step
It is rapid as follows:
M1, the 60-80% concentration that graphite powder, potassium peroxydisulfate and phosphorus pentoxide are added to one third according to the weight ratio
In the concentrated sulfuric acid, and after stirring 3-5 minutes, it is living that surface is added between 60-70 degrees Celsius in the concentrated sulfuric acid temperature of 60-80% concentration
Property agent and conductive black, be again stirring for, after stirring, after 3-5 hour cooling, washing to neutrality, and drying；
M2, the sample after drying is put into 2/3rds concentrated sulfuric acid of 60-80% concentration, and the temperature control of the concentrated sulfuric acid exists
Within 0-10 degrees Celsius, potassium permanganate is added, the temperature of mixture is maintained at 0-20 degrees Celsius；
M3, the vessel for holding mixture are placed in 36-40 degrees Celsius of oil bath, 3-5 hours are kept the temperature, in the process of heat preservation
In, 1/5th deionized water is slowly added into vessel；
M4, be added 1/5th deionized water 8-12 minute after, remaining deionized water is mixed with hydrogen peroxide solution,
Mixed solution is all poured into the vessel for filling mixture, is filtered while hot；
M5, the mixture in M4 is washed using dilute hydrochloric acid solution, by being put into 500ML three-necked bottle for acquisition, water-bath adds
Heat, temperature are controlled at 90-100 degrees Celsius, and sodium borohydride is added, until there is flocculent deposit appearance, are stopped heating, are done
It is dry, obtain a kind of high purity graphite alkenyl conducting particles powder；
M6, to high purity graphite alkenyl conducting particles powder obtained in M5 and resin-oatmeal, infrared enhancing powder, conductive black powder,
The auxiliary agents such as coupling agent, surfactant, dispersing agent, antioxidant are mixed, ultrasonic disperse；It is squeezed out again by extruder, pelletizer
It is granulated, finally obtains a kind of high purity graphite alkenyl conducting particles.
3. a kind of high purity graphite alkene conducting particles, it is characterised in that: its raw material matches as follows in parts by weight: graphite powder 30-
35 parts, 15-20 parts of potassium peroxydisulfate, 10-15 parts of phosphorus pentoxide, 1-3 parts of sodium borohydride, 15-20 parts of deionized water, dioxygen it is water-soluble
10-15 parts of 20-25 parts of liquid and the concentrated sulfuric acid of 30-40% concentration.
4. a kind of high purity graphite alkenyl conducting particles process for producing according to claim 3, which is characterized in that step
It is rapid as follows:
H1, the 30-40% concentration that graphite powder, potassium peroxydisulfate and phosphorus pentoxide are added to one third according to the weight ratio
In the concentrated sulfuric acid, and the concentrated sulfuric acid temperature of 30-40% concentration is between 60-70 degrees Celsius, after stirring 3-5 minutes, after stirring,
After 3-5 hours cooling, washing to neutrality, and it is dry；
H2, M2, the sample after drying is put into 2/3rds concentrated sulfuric acid of 30-40% concentration, and the temperature control of the concentrated sulfuric acid
System is within 0-10 degrees Celsius；
H3, the vessel for holding mixture are placed in 36-40 degrees Celsius of oil bath, 3-5 hours are kept the temperature, in the process of heat preservation
In, 1/5th deionized water is slowly added into vessel；
H4, be added 1/5th deionized water 8-12 minute after, remaining deionized water is mixed with hydrogen peroxide solution,
Mixed solution is all poured into the vessel for filling mixture, is filtered while hot；
H5, the mixed solution obtained in H4 being put into 500ML three-necked bottle, heating water bath, temperature is controlled at 90-100 degrees Celsius,
Sodium borohydride is added, until there is flocculent deposit appearance, stops heating, is dried, obtains a kind of high purity graphite alkenyl and leads
Charged particle powder；
H6, to high purity graphite alkenyl conducting particles powder obtained in H5 and resin-oatmeal, infrared enhancing powder, conductive black powder,
The auxiliary agents such as coupling agent, surfactant, dispersing agent, antioxidant are mixed, ultrasonic disperse；It is squeezed out again by extruder, pelletizer
It is granulated, finally obtains a kind of high purity graphite alkenyl conducting particles.
5. a kind of high purity graphite alkenyl conducting particles process for producing according to claim 2 or 4, feature exist
In the process for producing process should carry out in dustless laboratory, and the temperature control in laboratory is Celsius in 20-24
Degree.
6. a kind of high purity graphite alkene conducting particles process for producing according to claim 2 or 4, which is characterized in that
During preparation, raw material is poured into the concentrated sulfuric acid in solution, needs to be poured slowly into, is sent out after avoiding raw material from contacting with the concentrated sulfuric acid
It is raw to splash.
7. a kind of high purity graphite alkene conducting particles process for producing according to claim 2 or 4, which is characterized in that
When carrying out H5 or M5 step, after occurring flocculent deposit in three-necked bottle, mixture is poured out, is filtered using sieve, mistake
After filter, it is being dried.
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| CN201910351816.1A CN110002436A (en) | 2019-04-28 | 2019-04-28 | A kind of high purity graphite alkene conducting particles and its process for producing |
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| CN201910351816.1A CN110002436A (en) | 2019-04-28 | 2019-04-28 | A kind of high purity graphite alkene conducting particles and its process for producing |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112624091A (en) * | 2020-12-22 | 2021-04-09 | 乐福之家纳米材料有限责任公司 | Graphene conductive particle manufacturing equipment |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104517664A (en) * | 2014-12-26 | 2015-04-15 | 苏州格瑞丰纳米科技有限公司 | Graphene cluster based carbon system electric heating slurry as well as preparation method and application thereof |
| CN106276874A (en) * | 2016-08-10 | 2017-01-04 | 安徽省宁国天成电工有限公司 | A kind of preparation method of heater Graphene |
| CN108503971A (en) * | 2018-03-02 | 2018-09-07 | 上海利物盛企业集团有限公司 | A kind of graphene conductive plastics and preparation method thereof |
| CN109587842A (en) * | 2018-11-08 | 2019-04-05 | 中国科学院山西煤炭化学研究所 | A kind of graphene-based self limiting temperature electric heating slurry and preparation method thereof and the application in electric heating floor system |
-
2019
- 2019-04-28 CN CN201910351816.1A patent/CN110002436A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104517664A (en) * | 2014-12-26 | 2015-04-15 | 苏州格瑞丰纳米科技有限公司 | Graphene cluster based carbon system electric heating slurry as well as preparation method and application thereof |
| CN106276874A (en) * | 2016-08-10 | 2017-01-04 | 安徽省宁国天成电工有限公司 | A kind of preparation method of heater Graphene |
| CN108503971A (en) * | 2018-03-02 | 2018-09-07 | 上海利物盛企业集团有限公司 | A kind of graphene conductive plastics and preparation method thereof |
| CN109587842A (en) * | 2018-11-08 | 2019-04-05 | 中国科学院山西煤炭化学研究所 | A kind of graphene-based self limiting temperature electric heating slurry and preparation method thereof and the application in electric heating floor system |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112624091A (en) * | 2020-12-22 | 2021-04-09 | 乐福之家纳米材料有限责任公司 | Graphene conductive particle manufacturing equipment |
| CN112624091B (en) * | 2020-12-22 | 2024-01-30 | 乐福之家纳米材料有限责任公司 | Graphene conductive particle manufacturing equipment |
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