CN109608942A - A kind of preparation method of carbon black base electric heating carbon slurry - Google Patents
A kind of preparation method of carbon black base electric heating carbon slurry Download PDFInfo
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- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
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Abstract
The invention discloses a kind of preparation methods of carbon black base electric heating carbon slurry, belong to technical field of function materials.The present invention according to parts by weight, successively takes 20~30 parts of Nano metal powders, 2~3 parts of tourmaline powders, 40~50 parts of starch, 3~5 parts of glycerol, 30~40 parts of water, by Nano metal powder, starch and glycerol mixing and ball milling are subsequently added into water and continue ball milling, dry, it crushes, the sieve of 100 mesh is crossed, carbonizes, obtains modified filler；According to parts by weight, by 60~80 parts of aqueous polyurethane emulsions, 20~30 parts of carbon blacks, 8~10 parts of modified fillers, 5~8 parts of modified graphene oxide homogenate, 5~8 parts of aqueous polyisocyanate curing agents, 30~50 parts of deionized waters, 5~8 parts of emulsifier for mixing mixing are to get carbon black base electric heating carbon slurry.The carbon black base electric heating carbon slurry of technical solution of the present invention preparation has the characteristics that excellent electric conductivity and mechanical property, has broad prospects in the development of functional material technology industry.
Description
Technical field
The invention discloses a kind of preparation methods of carbon black base electric heating carbon slurry, belong to technical field of function materials.
Background technique
Electric heating carbon slurry is one of conductive material, and main component has conductive filler, link stuff, solvent and auxiliary agent, can lead to
Cross the technique production heating element of coating or spraying.Be be distributed evenly in non-metal conductor carbon system particle thermoplasticity or
The thick slurry formed in thermosetting resin, has low in cost, and cost performance is high, and steady performance is electronics member device
Part encapsulation, electrode and interconnection critical material, be widely used in all conglomeraties such as thin film switch, medical electronics, communication apparatus.Carbon
Slurry through silk-screen printing, be heating and curing after figure film layer obtained there is good electric conductivity, and solidifying film layer is not oxidizable, performance
Stablize, acid and alkali resistance and solvent corrosion can play protection and conductive effect.Conductive carbon paste is applicable to PET, copper foil and line
The materials such as road plate generally require conductive carbon according to application field and to the different model that requires of solidifying film layer resistance
Slurry has strong adhesive force and antistripping characteristic with corresponding substrate.Binder is the film forming matter of electrocondution slurry.In electrocondution slurry,
Dispersing conductive fine particles form the suspended substance of the suitable silk-screen printing with certain viscosity and rheological behavior in a binder.Slurry silk
In solidification process after print, due to the volatilization of solvent, binder makes between conducting particles, it is stable to be formed between particle and substrate
In conjunction with.Common binder includes various synthetic resin, is divided into thermosetting property and thermoplasticity two major classes, mainly include epoxy resin,
Phenolic resin, polyester resin, acrylic resin etc..Since the intermolecular opposing force of thermoplastic resin is smaller, strand with point
Moving resistance between subchain is smaller, and after-tack of being heated returns to normal after cooling, shows flexible characteristic.Binder tree
Rouge is usually insulator, and since binder itself is non-conductive, if solidification temperature does not reache a certain level, electrically conductive particles are just not
Easily form closely connection.If adding different binders in same conductive filler, after cured film forming, each film layer has
Different electric conductivity, this is related with the coherency of resin.The performances such as coherency, viscosity and the adhesive force of various binders are not
Together, therefore the electrocondution slurry that need to make overall plans substrate, condition of cure, the physicochemical property of film forming matter etc. that are acted on, it selects different
Binder resin, and consider the factors such as resinous molecular structure, polarity, molecular weight, glass transition temperature to the shadow of slurry service performance
It rings.
And conventional carbon black base electric heating carbon starches the problem of can not further increasing there is also electric conductivity and mechanical property.Cause
How this, improve the shortcomings that conventional carbon black base electric heating carbon is starched, and is that it is promoted and is applied to obtain the promotion of more high combination property
Broader field meets industrial production demand urgent problem to be solved.
Summary of the invention
The present invention solves the technical problem of: for conventional carbon black base electric heating carbon slurry electric conductivity and mechanical property without
The problem of method further increases provides a kind of preparation method of carbon black base electric heating carbon slurry.
In order to solve the above-mentioned technical problem, the technical scheme adopted by the invention is that:
A kind of preparation method of carbon black base electric heating carbon slurry, specific preparation process is as follows:
(1) according to parts by weight, 20~30 parts of Nano metal powders are successively taken, 2~3 parts of tourmaline powders, 40~50 parts of starch, 3~5
Part glycerol, 30~40 parts of water, by Nano metal powder, starch and glycerol mixing and ball milling are subsequently added into water and continue ball milling, dry, powder
It is broken, the sieve of 100 mesh is crossed, charing obtains modified filler；
(2) according to parts by weight, by 60~80 parts of aqueous polyurethane emulsions, 20~30 parts of carbon blacks, 8~10 parts of modified fillers, 5~
8 parts of modified graphene oxide homogenate, 5~8 parts of aqueous polyisocyanate curing agents, 30~50 parts of deionized waters, 5~8 parts of emulsifications
Agent is stirred to get carbon black base electric heating carbon slurry.
Step (1) Nano metal powder is copper nanoparticle, any one in nanometer iron powder or nano zinc powder.
Step (1) starch is glutinous rice starch, cornstarch, starch from sweet potato, in potato starch or wheaten starch
Any one.
Step (2) the aqueous polyurethane emulsion solid content is 50~60%.
The preparation process of step (2) modified graphene oxide homogenate are as follows: by graphene oxide and water in mass ratio 1:
10~1:20 is stirred, and ammonium hydroxide is then added dropwise and adjusts pH to 8.6~8.9, mixing ultrasound obtains mixed slurry, by (N- amidino groups)
Dodecylacrylamide is mixed with methoxy poly (ethylene glycol) 1:1~2:1 in mass ratio, and methoxy poly (ethylene glycol) quality is added
0.1~0.2 times of paracide and 0.07~0.10 times of methoxy poly (ethylene glycol) quality of ferrocene, are stirred, then plus
Enter 1~2 times of methoxy poly (ethylene glycol) quality of mixed slurry and 0.01~0.02 times of methoxy poly (ethylene glycol) quality of toluene two
Isocyanates is stirred to get modified graphene oxide homogenate.
Step (2) the aqueous polyisocyanate curing agent is that polyisocyanate curing agent JX-516 can be dispersed in water, and water can
It is described to disperse the arbitrary steps (2) that polyisocyanate curing agent JX-518 or water can be dispersed in polyisocyanate curing agent JX-519
Emulsifier is dodecyl alcohol polyoxyethylene ether sodium sulfate, ammonium lauryl sulfate, ammonium lauryl sulfate, coconut acyl methyl ox
Sodium sulfonate, any one in ethoxylated dodecyl alcohol carboxylic acid sodium or 1-isobutyl-3,5-dimethylhexylphosphoric acid.
The beneficial effects of the present invention are:
The present invention is by addition modified graphene oxide homogenate, firstly, during the preparation process, graphene oxide is mixed with water,
Then pH is adjusted by addition ammonium hydroxide, ammonium hydroxide may make the carboxylic ions at graphene oxide layer structure edge, so that oxidation
Graphene ribbon negative electrical charge enables graphene oxide good dispersion in system due to mutually exclusive between like charges,
Secondary, (N- amidino groups) dodecylacrylamide and methoxy poly (ethylene glycol) are anti-under the catalytic action of paracide and ferrocene
It answers, generation molecular structure is the block copolymer with parents' performance, which can be self-assembly of imitated vesicle structure, connect
Addition toluene di-isocyanate(TDI), toluene di-isocyanate(TDI) can be reacted with water, generate carbon dioxide and amine substance, carbon dioxide
Generation can be reacted with the amidine group in the block copolymer, and amidine group is made to become positively charged lotus, can in absorption system band it is negative
The graphene oxide of charge enables graphene oxide is good to disperse, simultaneously as like charges are mutually exclusive to make vesica
Inside configuration volume increases, and is conducive to the further dispersion of graphene oxide, in use, the vesica of expansion it is heated so that
Carbon dioxide in system releases, so that imitated vesicle structure loses the positive charge of original band, meanwhile, it is adsorbed on imitated vesicle structure table
Face due to the charge lost constraint, and, it can be achieved that further dispersion, effectively prevents oxygen under the action of carbon dioxide
The reunion of graphite alkene enables graphene oxide to form more current path in system, so that the electric conductivity of system
It can get a promotion, again, due to the fine dispersion of graphene oxide, so that the carbon black in system is not easy to reunite, so that aqueous poly-
Urethane can sufficiently wrap up carbon black, so that the mechanical property of system gets a promotion.
Specific embodiment
Graphene oxide and water 1:10~1:20 in mass ratio are placed in single-necked flask, in revolving speed be 400~600r/min
Under the conditions of, be stirred 30~50min, then into single-necked flask be added dropwise mass fraction be 20~30% ammonium hydroxide adjust pH to
8.6~8.9, and single-necked flask is placed in ultrasonic disperse instrument, under the conditions of supersonic frequency is 55~75kHz, mixing ultrasound 40
~60min obtains mixed slurry, by (N- amidino groups) dodecylacrylamide and methoxy poly (ethylene glycol) 1:1~2:1 in mass ratio
It is placed in three-necked flask, and 0.1~0.2 times of methoxy poly (ethylene glycol) quality of paracide and methoxy is added into three-necked flask
The ferrocene of 0.07~0.10 times of base polyethylene glycol quality, under the conditions of revolving speed is 300~500r/min, it is stirred 30~
1~2 times of methoxy poly (ethylene glycol) quality of mixed slurry and methoxy poly (ethylene glycol) is then added in 50min into three-necked flask
The toluene di-isocyanate(TDI) that 0.01~0.02 times of quality is stirred 60~80r/ under the conditions of revolving speed is 400~600r/min
To get modified graphene oxide homogenate under the conditions of min；According to parts by weight, 20~30 parts of Nano metal powders are successively taken, 2~3 parts
Tourmaline powder, 40~50 parts of starch, 3~5 parts of glycerol, 30~40 parts of water, by Nano metal powder, starch and glycerol are placed in ball mill
Water is then added into ball mill and continues ball milling, obtains ball milling material, ball milling material is then placed in baking by middle 40~60min of mixing and ball milling
It is dry to constant weight under the conditions of temperature is 105~110 DEG C in case, dry ball abrasive material is obtained, dry ball abrasive material is then placed in powder
It is crushed in broken machine, crosses the sieve of 100 mesh, obtain crushed material, then crushed material is placed in retort, and with 60~90mL/min rate
Nitrogen is filled with into furnace, under the conditions of temperature is 750~850 DEG C, after carbonizing 2~3h, obtain modified filler；According to parts by weight,
By 60~80 parts of aqueous polyurethane emulsions, 20~30 parts of carbon blacks, 8~10 parts of modified fillers, 5~8 parts of modified graphene oxides are even
Slurry, 5~8 parts of aqueous polyisocyanate curing agents, 30~50 parts of deionized waters, 5~8 parts of emulsifiers are placed in batch mixer, in turning
Under the conditions of speed is 400~600r/min, 40~60min is stirred to get carbon black base electric heating carbon slurry.The Nano metal powder is
Any one in copper nanoparticle, nanometer iron powder or nano zinc powder.The starch be glutinous rice starch, cornstarch, starch from sweet potato,
Any one in potato starch or wheaten starch.The aqueous polyurethane emulsion solid content is 50~60%.It is described aqueous poly-
Isocyanate curing agent is that polyisocyanate curing agent JX-516 can be dispersed in water, and polyisocyanate curing agent JX-518 can be dispersed in water
Or any one in polyisocyanate curing agent JX-519 can be dispersed in water.The emulsifier is Brij 35
Sodium sulphate, ammonium lauryl sulfate, ammonium lauryl sulfate, coconut acyl methyl taurine sodium, ethoxylated dodecyl alcohol carboxylic acid
Any one in sodium or 1-isobutyl-3,5-dimethylhexylphosphoric acid.
Example 1
Graphene oxide and water 1:20 in mass ratio are placed in single-necked flask, under the conditions of revolving speed is 600r/min, are stirred
The ammonium hydroxide that mass fraction is 30% is then added dropwise into single-necked flask and adjusts pH to 8.9, and single-necked flask is placed in ultrasound by 50min
In separating apparatus, under the conditions of supersonic frequency is 75kHz, ultrasound 60min is mixed, mixed slurry is obtained, by (N- amidino groups) dodecyl
Acrylamide and methoxy poly (ethylene glycol) 2:1 in mass ratio are placed in three-necked flask, and methoxyl group is added into three-necked flask and gathers
The paracide and 0.10 times of methoxy poly (ethylene glycol) quality of ferrocene that 0.2 times of quality of glycol, in revolving speed be 500r/min
Under the conditions of, it is stirred 50min, 2 times of methoxy poly (ethylene glycol) quality of mixed slurry and first are then added into three-necked flask
The toluene di-isocyanate(TDI) of 0.02 times of oxygroup polyethylene glycol quality is stirred 80r/min under the conditions of revolving speed is 600r/min
Under the conditions of to get modified graphene oxide homogenate；According to parts by weight, 30 parts of Nano metal powders are successively taken, 3 parts of tourmaline powders,
50 parts of starch, 5 parts of glycerol, 40 parts of water, by Nano metal powder, starch and glycerol are placed in mixing and ball milling 60min in ball mill, then
Water is added into ball mill and continues ball milling, obtains ball milling material, then ball milling material is placed in baking oven, under the conditions of temperature is 110 DEG C,
Drying obtains dry ball abrasive material, then dry ball abrasive material is placed in pulverizer and is crushed, cross the sieve of 100 mesh, must crush to constant weight
Material, then crushed material is placed in retort, and nitrogen is filled with into furnace with 90mL/min rate, in temperature be 850 DEG C of conditions
Under, after carbonizing 3h, obtain modified filler；According to parts by weight, by 80 parts of aqueous polyurethane emulsions, 30 parts of carbon blacks, 10 parts of modifications are filled out
Material, 58 parts of modified graphene oxide homogenate, 8 parts of aqueous polyisocyanate curing agents, 50 parts of deionized waters, 8 parts of emulsifiers are placed in
In batch mixer, under the conditions of revolving speed is 600r/min, 60min is stirred to get carbon black base electric heating carbon slurry.The nano metal
Powder is copper nanoparticle.The starch is glutinous rice starch.The aqueous polyurethane emulsion solid content is 60%.The aqueous poly- isocyanide
Acid esters curing agent is that polyisocyanate curing agent JX-516 can be dispersed in water.The emulsifier is Brij 35 sulphur
Sour sodium.
Example 2
Graphene oxide and water 1:20 in mass ratio are placed in single-necked flask, under the conditions of revolving speed is 600r/min, are stirred
The ammonium hydroxide that mass fraction is 30% is then added dropwise into single-necked flask and adjusts pH to 8.9, and single-necked flask is placed in ultrasound by 50min
In separating apparatus, under the conditions of supersonic frequency is 75kHz, ultrasound 60min is mixed, mixed slurry is obtained, by (N- amidino groups) dodecyl
Acrylamide and methoxy poly (ethylene glycol) 2:1 in mass ratio are placed in three-necked flask, and methoxyl group is added into three-necked flask and gathers
The paracide and 0.10 times of methoxy poly (ethylene glycol) quality of ferrocene that 0.2 times of quality of glycol, in revolving speed be 500r/min
Under the conditions of, it is stirred 50min, 2 times of methoxy poly (ethylene glycol) quality of mixed slurry and first are then added into three-necked flask
The toluene di-isocyanate(TDI) of 0.02 times of oxygroup polyethylene glycol quality is stirred 80r/min under the conditions of revolving speed is 600r/min
Under the conditions of to get modified graphene oxide homogenate；According to parts by weight, by 80 parts of aqueous polyurethane emulsions, 30 parts of carbon blacks, 58 parts
Modified graphene oxide homogenate, 8 parts of aqueous polyisocyanate curing agents, 50 parts of deionized waters, 8 parts of emulsifiers are placed in batch mixer
In, under the conditions of revolving speed is 600r/min, 60min is stirred to get carbon black base electric heating carbon slurry.The Nano metal powder is to receive
Rice copper powder.The aqueous polyurethane emulsion solid content is 60%.The aqueous polyisocyanate curing agent is that poly- isocyanide can be dispersed in water
Acid esters curing agent JX-516.The emulsifier is dodecyl alcohol polyoxyethylene ether sodium sulfate.
Example 3
According to parts by weight, 30 parts of Nano metal powders are successively taken, 3 parts of tourmaline powders, 50 parts of starch, 5 parts of glycerol, 40 parts of water will
Nano metal powder, starch and glycerol are placed in mixing and ball milling 60min in ball mill, and water is then added into ball mill and continues ball milling,
Ball milling material is obtained, then ball milling material is placed in baking oven, under the conditions of temperature is 110 DEG C, drying to constant weight obtains dry ball abrasive material,
Then dry ball abrasive material is placed in pulverizer and is crushed, crossed the sieve of 100 mesh, obtain crushed material, crushed material is then placed in retort
In, and nitrogen is filled with into furnace with 90mL/min rate, and under the conditions of temperature is 850 DEG C, after carbonizing 3h, obtain modified filler；It presses
Parts by weight meter, by 80 parts of aqueous polyurethane emulsions, 30 parts of carbon blacks, 10 parts of modified fillers, 8 parts of aqueous polyisocyanate solidifications
Agent, 50 parts of deionized waters, 8 parts of emulsifiers are placed in batch mixer, under the conditions of revolving speed is 600r/min, are stirred 60min, i.e.,
Obtain carbon black base electric heating carbon slurry.The Nano metal powder is copper nanoparticle.The starch is glutinous rice starch.The aqueous polyurethane cream
Fluid solid content is 60%.The aqueous polyisocyanate curing agent is that polyisocyanate curing agent JX-516 can be dispersed in water.The cream
Agent is dodecyl alcohol polyoxyethylene ether sodium sulfate.
Comparative example: the carbon black base electric heating carbon slurry of Yingtan material production Co., Ltd production.
Example 1 to the resulting carbon black base electric heating carbon of example 3 is starched and comparative example product carries out performance detection, specific detection side
Method is as follows:
1. resistivity measurement: using the digital four-point probe of ST-2253 type (Suzhou Jingge Electronic Co., Ltd.) to sample
Carry out resistivity measurement.
2. Mechanics Performance Testing: being cut using CP-25 hand microtome to electric heating carbon serous coat piece, prepare dumbbell shaped electricity
Hot carbon serous coat piece, then using XL-100A type universal testing machine (Guangzhou laboratory apparatus factory) test sample tensile strength and
Elongation at break.
Specific testing result is as shown in table 1:
1 carbon black base electric heating carbon of table starches specific testing result
| Detection project | Example 1 | Example 2 | Example 3 | Comparative example |
| Resistivity/Ω .cm | 30 | 80 | 75 | 135 |
| Tensile strength/MPa | 6.7 | 4.5 | 5.2 | 1.7 |
| Elongation at break/% | 2136 | 792 | 1035 | 624 |
By 1 testing result of table it is found that the carbon black base electric heating carbon slurry of technical solution of the present invention preparation have excellent electric conductivity and
The characteristics of mechanical property, has broad prospects in the development of functional material technology industry.
Claims (7)
1. a kind of preparation method of carbon black base electric heating carbon slurry, it is characterised in that specific preparation process is as follows:
(1) according to parts by weight, 20~30 parts of Nano metal powders are successively taken, 2~3 parts of tourmaline powders, 40~50 parts of starch, 3~5
Part glycerol, 30~40 parts of water, by Nano metal powder, starch and glycerol mixing and ball milling are subsequently added into water and continue ball milling, dry, powder
It is broken, the sieve of 100 mesh is crossed, charing obtains modified filler；
(2) according to parts by weight, by 60~80 parts of aqueous polyurethane emulsions, 20~30 parts of carbon blacks, 8~10 parts of modified fillers, 5~
8 parts of modified graphene oxide homogenate, 5~8 parts of aqueous polyisocyanate curing agents, 30~50 parts of deionized waters, 5~8 parts of emulsifications
Agent is stirred to get carbon black base electric heating carbon slurry.
2. a kind of preparation method of carbon black base electric heating carbon slurry according to claim 1, it is characterised in that: step (1) is described to be received
Rice metal powder is copper nanoparticle, any one in nanometer iron powder or nano zinc powder.
3. a kind of preparation method of carbon black base electric heating carbon slurry according to claim 1, it is characterised in that: step (1) described shallow lake
Powder is glutinous rice starch, cornstarch, starch from sweet potato, any one in potato starch or wheaten starch.
4. a kind of preparation method of carbon black base electric heating carbon slurry according to claim 1, it is characterised in that: step (2) described water
Property polyaminoester emulsion solid content be 50~60%.
5. a kind of preparation method of carbon black base electric heating carbon slurry according to claim 1, it is characterised in that: step (2) is described to be changed
Property graphene oxide homogenate preparation process are as follows: graphene oxide is stirred with water 1:10~1:20 in mass ratio, then
Ammonium hydroxide is added dropwise and adjusts pH to 8.6~8.9, mixing ultrasound obtains mixed slurry, by (N- amidino groups) dodecylacrylamide and methoxy
Base polyethylene glycol 1:1~2:1 in mass ratio mixing, and be added 0.1~0.2 times of methoxy poly (ethylene glycol) quality paracide and
The ferrocene that 0.07~0.10 times of methoxy poly (ethylene glycol) quality, is stirred, be subsequently added into methoxy poly (ethylene glycol) quality 1~
2 times of mixed slurry and 0.01~0.02 times of methoxy poly (ethylene glycol) quality of toluene di-isocyanate(TDI), are stirred to get changing
Property graphene oxide homogenate.
6. a kind of preparation method of carbon black base electric heating carbon slurry according to claim 1, it is characterised in that: step (2) described water
Property polyisocyanate curing agent be that polyisocyanate curing agent JX-516 can be dispersed in water, polyisocyanate curing agent can be dispersed in water
Any one in polyisocyanate curing agent JX-519 can be dispersed in JX-518 or water.
7. a kind of preparation method of carbon black base electric heating carbon slurry according to claim 1, it is characterised in that: step (2) described cream
Agent is dodecyl alcohol polyoxyethylene ether sodium sulfate, ammonium lauryl sulfate, ammonium lauryl sulfate, coconut acyl methyl ox sulphur
Sour sodium, any one in ethoxylated dodecyl alcohol carboxylic acid sodium or 1-isobutyl-3,5-dimethylhexylphosphoric acid.
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| CN110723963A (en) * | 2019-10-31 | 2020-01-24 | 中冶武汉冶金建筑研究院有限公司 | Blast furnace tapping channel castable containing nano alumina and preparation method thereof |
| CN110723963B (en) * | 2019-10-31 | 2022-06-03 | 中冶武汉冶金建筑研究院有限公司 | Blast furnace tapping channel castable containing nano alumina and preparation method thereof |
| US12024636B2 (en) | 2021-05-07 | 2024-07-02 | Taiwan Textile Research Institute | Conductive coating and manufacturing method thereof |
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