CN108864593A - A kind of method that modified carbon nano-tube prepares antistatic polyvinyl chloride material - Google Patents
A kind of method that modified carbon nano-tube prepares antistatic polyvinyl chloride material Download PDFInfo
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- CN108864593A CN108864593A CN201810557616.7A CN201810557616A CN108864593A CN 108864593 A CN108864593 A CN 108864593A CN 201810557616 A CN201810557616 A CN 201810557616A CN 108864593 A CN108864593 A CN 108864593A
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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
- C08K9/10—Encapsulated 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
- C08K3/041—Carbon nanotubes
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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
- C08K2201/011—Nanostructured additives
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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
- C08K2201/017—Additives being an antistatic agent
Abstract
The invention discloses a kind of methods that modified carbon nano-tube prepares antistatic polyvinyl chloride material, are related to anti-static material field, include the following steps：First by carbon nanotube through peroxidating and high-temperature calcination after purification, the reagents such as pyrroles, ammonium persulfate are added after the reaction of ice bath temperature control, after decompression filters cleaning, modified carbon nano-tube obtained by drying, carbon nanotube and processing aid are carried out it is high mixed, after being kneaded and being hot-forming to get；Polypyrrole is subjected to surface package modification to carbon nanotube in preparation method of the present invention, the synergistic effect of polypyrrole and carbon nanotube has dual antistatic effect, polypyrrole carries out activation modification to carbon nanotube simultaneously, the dispersion and compatibility of carbon nanotube can be enhanced, improve the comprehensive performance of antistatic polyvinyl chloride material.
Description
Technical field
The present invention relates to anti-static material fields, and in particular to a kind of modified carbon nano-tube prepares antistatic polyvinyl chloride material
The method of material.
Background technique
Polyvinyl chloride is one of maximum general-purpose plastics of yield in the world, very widely used.In construction material, industry system
Product, tubing, wire and cable, packaging film, sealing material, fiber etc. are widely used, due to pvc material surface
Resistance it is high, electrical insulating property is good, it is easy to cause electrostatic accumulation, once taking electrostatic, just be not easy to eliminate, when accumulation of static electricity arrives
To a certain degree, it is easy for generating spark, electronic component is caused to damage, explosion accident on fire occurs for product library, coal mine, oil depot etc..
In recent years, it is widely applied with polymer material in fields such as industry, the people's livelihood, since its high insulation performance is led
It causes easy Accumulating charge in use and generates electrostatic, so that cause fire, explosion and damage electronic component, therefore study, open
There is the polymer material of antistatic property to become an important directions in field of compound material for hair and production.Eliminate polymeric material
Material generates how electrostatic charge is revealed rapidly, reduce accumulation by having its source in for electrostatic.The approach of solution mainly has two：First is that table
Face is connected, but ontology is connected, and surface conducting is to add small molecule antistatic agent by surface of polymer material coating or inside,
It forms surface conductive layer and achievees the purpose that antistatic.Ontology conducting approach belongs to the permanently antistatic technology of polymer material,
Related to the exploitation of conductive agent and optimization, the polymer material for ontology conducting is that conductive agent is blended in resin matrix in fact
It is existing.
One kind is disclosed in special table 2002-500237 bulletin adds antistatic agent polyether system in rubber to eliminate polymer
The method of electrostatic, preparation method is simple, easy to operate, and cost of material is low, but in the case of using polyether system, exists and ask as follows
Topic：Polyethers decomposes at high temperature, does not show sufficient antistatic effect.Particularly, even if only carrying out the silicon rubber of thermohardening type
After carrying out heat cure in the solidfied material of glue composition, antistatic effect also almost disappears, and directly affects the antistatic effect of material.
European patent EP 1134268 discloses a kind of quaternary ammonium salt antistatic agent, and the volume resistance of polyurethane product can be made to reach
To 107Ω or so, but this antistatic agent exists simultaneously following disadvantage：(1) these antistatic agents have ambient humidity relatively strong
Dependence；(2) durability is poor：Antistatic agent molecule, which is easy to move back, moves to material surface to volatilize, so that antistatic effect
Fruit cannot be lasting.
Summary of the invention
Aiming at the problems existing in the prior art, the present invention provides a kind of modified carbon nano-tubes to prepare pvc material
Method, polypyrrole is subjected to surface package modification to carbon nanotube in preparation method of the present invention, polypyrrole and carbon nanotube
Synergistic effect has dual antistatic effect, while polypyrrole carries out activation modification to carbon nanotube, and carbon nanotube can be enhanced
Dispersion and compatibility, improve antistatic polyvinyl chloride material comprehensive performance.
In order to achieve the above object, the present invention is achieved through the following technical solutions：
A kind of method that modified carbon nano-tube prepares antistatic polyvinyl chloride material, includes the following steps：
(1) carbon nanotube is added in acid potassium bichromate solution, is uniformly mixed, is heated to 140 degrees Celsius,
It after being heated to reflux 2-4 hours, is washed repeatedly with deionized water, until filtrate is placed in calcining kiln roasting 4-5 after filtrate is in neutrality
Hour is to get purifying carbon nano-tube；
(2) pyrroles and purifying carbon nano-tube are added in the hydrochloric acid solution of 1 mol/L, low temperature is in merging ice bath with 300-
500 revs/min of speed stirs 10-15 minutes, obtains mixing suspension；
(3) it dissolves ammonium persulfate into the hydrochloric acid solution of 1 mol/L, stirring and dissolving is uniform, and it is molten to obtain ammonium persulfate acidity
Liquid；
(4) ammonium persulfate acid solution obtained in step (2) is slowly added dropwise to step (1) and mixing suspension is made
In, it keeps ice bath with 300-500 revs/min of agitation and dropping during being added dropwise, after completion of dropwise addition, is persistently placed in ice bath with 800-
1200 revs/min of speed is stirred to react 20-24 hours；
(5) after filtering the reactant decompression in step (3), filtrate, which is cleaned with deionized water repeatedly to filtrate pH value, is
Property after, filtrate is placed in baking oven at 50 c, dry 20 hours to get the modified carbon nano-tube；
(6) Corvic, processing aid and modified carbon nano-tube are added in high-speed mixer after mixing, it will
It is kneaded to prolong for 6-10 minutes in mixed material two-roll mill and is pressed into flaky composite material, be made one after vulcanizing press hot pressing
Determine the composite board of thickness.
Preferably, acid potassium bichromate solution is sulfuric acid potassium bichromate solution, the volume of potassium bichromate in the step (1)
Concentration is 0.25 mol/L, and the volumetric concentration of sulfuric acid is 50-55%.
Preferably, the maturing temperature in the step (1) is 700-800 degrees Celsius.
Preferably, the quality proportioning of pyrroles and purifying carbon nano-tube is 1 in the step (2):2-3.
Preferably, the ice bath temperature control is at 0-3 degrees Celsius.
Preferably, the dosage of ammonium persulfate is 0.56-0.62 times of carbon nanotube dosage in step (3).
Preferably, Corvic, processing aid and modified carbon nano-tube mass ratio are 100 in the step (6):
15-20:7-12。
Preferably, the processing aid includes：15-20 parts of repefral, 5-9 parts of epoxidized soybean oil, tristearin
Sour zinc 7-12 parts, 3-5 parts of lauryl sodium sulfate, 3-5 parts of sodium phosphite and 2-4 parts of melamine.
Preferably, the temperature of double rod open mills is 165-175 degrees Celsius in the step (6), front and back roller slewing rate ratio
It is 1:1-1.2.
Preferably, vulcanizing press hot pressing temperature is 150-160 degrees Celsius in the step (6), hot pressing pressure 12-
18MPa, hot pressing time are 8-12 minutes.
The present invention has following beneficial effect：
(1) polypyrrole is subjected to surface package modification, polypyrrole and carbon nanometer to carbon nanotube in preparation method of the present invention
The synergistic effect of pipe has dual antistatic effect, while polypyrrole carries out activation modification to carbon nanotube, and carbon can be enhanced and receive
The dispersion and compatibility of mitron improve the comprehensive performance of antistatic polyvinyl chloride material.
(2) polypyrrole contains the high molecular material of conjugated structure, has certain electric conductivity, is added to polymeric matrix tree
In rouge, the antistatic property of polymer composite material can be enhanced, polypyrrole material compares the conductivity of carbon nanotube as conductive agent
It is lower, but the surface modification as carbon series conductive agent carbon nanotube, it can be enhanced compatible between carbon nanotube and resin matrix
Property, play a dual role of conductive agent and surfactant.
(3) after in preparation method of the present invention using acid potassium dichromate oxidation, by carbon nanotube be placed in calcining furnace into
Row high-temperature calcination removes impurity in carbon nanotube, enhances the intensity of carbon nanotube, reduces impurity to carbon nanotube anti-static
It influences.
(4) it in preparation method of the present invention in polyvinyl chloride and hot-forming modified carbon nano-tube melting, adds a certain amount of
Processing aid, improve the processability and stability of polymer material, be effectively improved the comprehensive performance of polymer material.
Specific embodiment
Below with reference to embodiment, further description of the specific embodiments of the present invention, and following embodiment is only used for more
Technical solution of the present invention is clearly demonstrated, and not intended to limit the protection scope of the present invention.
Embodiment 1
A kind of method that modified carbon nano-tube prepares antistatic polyvinyl chloride material, includes the following steps：
(1) carbon nanotube is added in acid potassium bichromate solution, is uniformly mixed, is heated to 140 degrees Celsius,
It after being heated to reflux 2 hours, is washed repeatedly with deionized water, until it is small that filtrate is placed in calcining kiln roasting 4 after filtrate is in neutrality
When to get purifying carbon nano-tube；
(2) pyrroles and purifying carbon nano-tube are added in the hydrochloric acid solution of 1 mol/L, low temperature is in merging ice bath with 300
Rev/min speed stir 10 minutes, obtain mixing suspension；
(3) it dissolves ammonium persulfate into the hydrochloric acid solution of 1 mol/L, stirring and dissolving is uniform, and it is molten to obtain ammonium persulfate acidity
Liquid；
(4) ammonium persulfate acid solution obtained in step (2) is slowly added dropwise to step (1) and mixing suspension is made
In, it keeps ice bath with 300 revs/min of agitation and droppings during being added dropwise, after completion of dropwise addition, is persistently placed in ice bath with 800 revs/min
The speed of clock is stirred to react 20 hours；
(5) after filtering the reactant decompression in step (3), filtrate, which is cleaned with deionized water repeatedly to filtrate pH value, is
Property after, filtrate is placed in baking oven at 50 c, dry 20 hours to get the modified carbon nano-tube；
(6) Corvic, processing aid and modified carbon nano-tube are added in high-speed mixer after mixing, it will
It is kneaded to prolong for 6 minutes in mixed material two-roll mill and is pressed into flaky composite material, be made after vulcanizing press hot pressing certain
The composite board of thickness.
Acid potassium bichromate solution is sulfuric acid potassium bichromate solution in step (1), and the volumetric concentration of potassium bichromate is 0.25
Mol/L, the volumetric concentration of sulfuric acid are 50%.
Maturing temperature in step (1) is 700 degrees Celsius.
The quality proportioning of pyrroles and carbon nanotube is 1 in step (2):2.
When carrying out ice bath cooling, ice bath temperature is controlled at 0-3 degrees Celsius.
The dosage of ammonium persulfate is 0.56 times of carbon nanotube dosage in step (3).
Corvic, processing aid and modified carbon nano-tube mass ratio are 100 in step (6):15:7.
Processing aid includes：15 parts of repefral, 5 parts of epoxidized soybean oil, 7 parts of zinc stearate, dodecyl
3 parts of sodium sulphate, 3 parts of sodium phosphite and 2 parts of melamine.
The temperature of double rod open mills is 165 degrees Celsius in step (6), and front and back roller slewing rate ratio is 1:1.
Vulcanizing press hot pressing temperature is 150 degrees Celsius, hot pressing pressure 12MPa in step (6), and hot pressing time is 8 points
Clock.
Embodiment 2
A kind of method that modified carbon nano-tube prepares antistatic polyvinyl chloride material, includes the following steps：
(1) carbon nanotube is added in acid potassium bichromate solution, is uniformly mixed, is heated to 140 degrees Celsius,
It after being heated to reflux 4 hours, is washed repeatedly with deionized water, until it is small that filtrate is placed in calcining kiln roasting 5 after filtrate is in neutrality
When to get purifying carbon nano-tube；
(2) pyrroles and purifying carbon nano-tube are added in the hydrochloric acid solution of 1 mol/L, low temperature is in merging ice bath with 500
Rev/min speed stir 15 minutes, obtain mixing suspension；
(3) it dissolves ammonium persulfate into the hydrochloric acid solution of 1 mol/L, stirring and dissolving is uniform, and it is molten to obtain ammonium persulfate acidity
Liquid；
(4) ammonium persulfate acid solution obtained in step (2) is slowly added dropwise to step (1) and mixing suspension is made
In, be added dropwise during keep ice bath with 500 revs/min of agitation and droppings, after completion of dropwise addition, persistently be placed in ice bath in 1200 turns/
The speed of minute is stirred to react 24 hours；
(5) after filtering the reactant decompression in step (3), filtrate, which is cleaned with deionized water repeatedly to filtrate pH value, is
Property after, filtrate is placed in baking oven at 50 c, dry 20 hours to get the modified carbon nano-tube；
(6) Corvic, processing aid and modified carbon nano-tube are added in high-speed mixer after mixing, it will
It is kneaded to prolong for 10 minutes in mixed material two-roll mill and is pressed into flaky composite material, be made after vulcanizing press hot pressing certain
The composite board of thickness.
Acid potassium bichromate solution is sulfuric acid potassium bichromate solution in the step (1), and the volumetric concentration of potassium bichromate is
0.25 mol/L, the volumetric concentration of sulfuric acid are 55%.
Maturing temperature in step (1) is 800 degrees Celsius.
The quality proportioning of pyrroles and carbon nanotube is 1 in step (2):3.
When carrying out ice bath cooling, ice bath temperature is controlled at 0-3 degrees Celsius.
The dosage of ammonium persulfate is 0.62 times of carbon nanotube dosage in step (3).
Corvic, processing aid and modified carbon nano-tube mass ratio are 100 in step (6):20:12.
Processing aid includes：20 parts of repefral, 9 parts of epoxidized soybean oil, 12 parts of zinc stearate, dodecyl
5 parts of sodium sulphate, 5 parts of sodium phosphite and 4 parts of melamine.
The temperature of double rod open mills is 175 degrees Celsius in step (6), and front and back roller slewing rate ratio is 1:1.2.
Vulcanizing press hot pressing temperature is 160 degrees Celsius, hot pressing pressure 18MPa in step (6), and hot pressing time is 12 points
Clock.
Embodiment 3
A kind of method that modified carbon nano-tube prepares antistatic polyvinyl chloride material, includes the following steps：
(1) carbon nanotube is added in acid potassium bichromate solution, is uniformly mixed, is heated to 140 degrees Celsius,
It after being heated to reflux 3 hours, is washed repeatedly with deionized water, until it is small that filtrate is placed in calcining kiln roasting 4.5 after filtrate is in neutrality
When to get purifying carbon nano-tube；
(2) pyrroles and purifying carbon nano-tube are added in the hydrochloric acid solution of 1 mol/L, low temperature is in merging ice bath with 300-
500 revs/min of speed stirs 12 minutes, obtains mixing suspension；
(3) it dissolves ammonium persulfate into the hydrochloric acid solution of 1 mol/L, stirring and dissolving is uniform, and it is molten to obtain ammonium persulfate acidity
Liquid；
(4) ammonium persulfate acid solution obtained in step (2) is slowly added dropwise to step (1) and mixing suspension is made
In, be added dropwise during keep ice bath with 400 revs/min of agitation and droppings, after completion of dropwise addition, persistently be placed in ice bath in 1000 turns/
The speed of minute is stirred to react 22 hours；
(5) after filtering the reactant decompression in step (3), filtrate, which is cleaned with deionized water repeatedly to filtrate pH value, is
Property after, filtrate is placed in baking oven at 50 c, dry 20 hours to get the modified carbon nano-tube；
(6) Corvic, processing aid and modified carbon nano-tube are added in high-speed mixer after mixing, it will
It is kneaded to prolong for 8 minutes in mixed material two-roll mill and is pressed into flaky composite material, be made after vulcanizing press hot pressing certain
The composite board of thickness.
Acid potassium bichromate solution is sulfuric acid potassium bichromate solution in step (1), and the volumetric concentration of potassium bichromate is 0.25
Mol/L, the volumetric concentration of sulfuric acid are 52%.
Maturing temperature in step (1) is 750 degrees Celsius.
The quality proportioning of pyrroles and purifying carbon nano-tube is 1 in step (2):2.5.
When carrying out ice bath cooling, ice bath temperature is controlled at 0-3 degrees Celsius.
The dosage of ammonium persulfate is 0.6 times of carbon nanotube dosage in step (3).
Corvic, processing aid and modified carbon nano-tube mass ratio are 100 in step (6):17:10.
Processing aid includes：18 parts of repefral, 7 parts of epoxidized soybean oil, 9 parts of zinc stearate, dodecyl
4 parts of sodium sulphate, 4 parts of sodium phosphite and 2.5 parts of melamine.
The temperature of double rod open mills is 170 degrees Celsius in step (6), and front and back roller slewing rate ratio is 1:1.1.
Vulcanizing press hot pressing temperature is 155 degrees Celsius, hot pressing pressure 14MPa in step (6), and hot pressing time is 10 points
Clock.
Embodiment 4
A kind of method that modified carbon nano-tube prepares antistatic polyvinyl chloride material, includes the following steps：
(1) carbon nanotube is added in acid potassium bichromate solution, is uniformly mixed, is heated to 140 degrees Celsius,
It after being heated to reflux 3.5 hours, is washed repeatedly with deionized water, until filtrate is placed in calcining kiln roasting 4.5 after filtrate is in neutrality
Hour is to get purifying carbon nano-tube；
(2) pyrroles and purifying carbon nano-tube are added in the hydrochloric acid solution of 1 mol/L, low temperature is in merging ice bath with 450
Rev/min speed stir 14 minutes, obtain mixing suspension；
(3) it dissolves ammonium persulfate into the hydrochloric acid solution of 1 mol/L, stirring and dissolving is uniform, and it is molten to obtain ammonium persulfate acidity
Liquid；
(4) ammonium persulfate acid solution obtained in step (2) is slowly added dropwise to step (1) and mixing suspension is made
In, be added dropwise during keep ice bath with 450 revs/min of agitation and droppings, after completion of dropwise addition, persistently be placed in ice bath in 1100 turns/
The speed of minute is stirred to react 23 hours；
(5) after filtering the reactant decompression in step (3), filtrate, which is cleaned with deionized water repeatedly to filtrate pH value, is
Property after, filtrate is placed in baking oven at 50 c, dry 20 hours to get the modified carbon nano-tube；
(6) Corvic, processing aid and modified carbon nano-tube are added in high-speed mixer after mixing, it will
It is kneaded to prolong for 8 minutes in mixed material two-roll mill and is pressed into flaky composite material, be made after vulcanizing press hot pressing certain
The composite board of thickness.
Acid potassium bichromate solution is sulfuric acid potassium bichromate solution in step (1), and the volumetric concentration of potassium bichromate is 0.25
Mol/L, the volumetric concentration of sulfuric acid are 54%.
Maturing temperature in step (1) is 780 degrees Celsius.
The quality proportioning of pyrroles and purifying carbon nano-tube is 1 in step (2):2.8.
When carrying out ice bath cooling, ice bath temperature is controlled at 0-3 degrees Celsius.
The dosage of ammonium persulfate is 0.61 times of carbon nanotube dosage in step (3).
Corvic, processing aid and modified carbon nano-tube mass ratio are 100 in step (6):18:11.
Processing aid includes：19 parts of repefral, 7 parts of epoxidized soybean oil, 11 parts of zinc stearate, dodecyl
4.5 parts of sodium sulphate, 4.5 parts of sodium phosphite and 3.5 parts of melamine.
The temperature of double rod open mills is 172 degrees Celsius in step (6), and front and back roller slewing rate ratio is 1:1.15.
Vulcanizing press hot pressing temperature is 158 degrees Celsius, hot pressing pressure 16MPa in step (6), and hot pressing time is 11 points
Clock.
Comparative example 1
It is mixed that 100 parts of Corvic, 15 parts of zinc stearate, 7 parts of epoxidized soybean oil, 6 parts of polypyrrole are added to high speed
In conjunction machine after mixing, it puts into double screw extruder and carries out extruding pelletization under 180 degrees Celsius to get antistatic polychlorostyrene
Vinyl material.
Comparative example 2
By 100 parts of Corvic, 15 parts of carbon nanotube, 7 parts of epoxidized soybean oil, 3 parts of lauryl sodium sulfate additions
After mixing into high-speed mixer, it puts into double screw extruder and carries out extruding pelletization under 180 degrees Celsius to get anti-
Electrostatic pvc material.
By antistatic polyvinyl chloride material made from antistatic polyvinyl chloride material made from embodiment 1-4 and comparative example 1-2
Material is tested for the property, and test result see the table below 1：
Table 1：
Comparative example is that addition polypyrrole is antistatic agent, and comparative example 2 is that addition carbon nanotube is antistatic agent, is surveyed from upper table
The specific resistance that examination value can be seen that embodiment 1-4 is respectively less than the specific resistance of comparative example 1-2, illustrates that polypyrrole is modified in the present invention
The pvc material antistatic property of carbon nanotube preparation, has and is obviously improved.
The specific resistance value tested after the heating of embodiment 1-4 and comparative example 1 can be seen that single polypyrrole in comparative example
It is poor as antistatic agent thermal stability, and the antistatic property of material of the present invention has good thermal stability.
It can be seen that in comparative example 2 from the tensile strength values and elongation at break values of embodiment 1-4 and comparative example 2
Antistatic agent carbon nanotube can not show a candle to the present invention without the mechanical property that the material being prepared in polymer is added in any modification
By the composite material of the modified carbon nanotube of polypyrrole and polymer preparation, illustrate that polypyrrole has surface to carbon nanotube
Activation effect.
The foregoing is only a preferred embodiment of the present invention, is not intended to restrict the invention, although referring to aforementioned reality
Applying example, invention is explained in detail, for those skilled in the art, still can be to aforementioned each implementation
Technical solution documented by example is modified or equivalent replacement of some of the technical features.It is all in essence of the invention
Within mind and principle, any modification, equivalent replacement, improvement and so on be should all be included in the protection scope of the present invention.
Claims (10)
1. a kind of method that modified carbon nano-tube prepares antistatic polyvinyl chloride material, which is characterized in that include the following steps：
(1) carbon nanotube is added in acid potassium bichromate solution, is uniformly mixed, be heated to 140 degrees Celsius, heating
It after reflux 2-4 hours, is washed repeatedly with deionized water, until it is small that filtrate is placed in calcining kiln roasting 4-5 after filtrate is in neutrality
When to get purifying carbon nano-tube；
(2) pyrroles and purifying carbon nano-tube are added in the hydrochloric acid solution of 1 mol/L, low temperature is in merging ice bath with 300-500
Rev/min speed stir 10-15 minutes, obtain mixing suspension；
(3) it dissolves ammonium persulfate into the hydrochloric acid solution of 1 mol/L, stirring and dissolving is uniform, obtains ammonium persulfate acid solution；
(4) ammonium persulfate acid solution obtained in step (2) is slowly added dropwise to step (1) and is made in mixing suspension, drop
It keeps ice bath with 300-500 revs/min of agitation and dropping during adding, after completion of dropwise addition, is persistently placed in ice bath with 800-1200
Rev/min speed be stirred to react 20-24 hours；
(5) after filtering the reactant decompression in step (3), it is neutral that filtrate, which is cleaned with deionized water repeatedly to filtrate pH value,
Afterwards, filtrate is placed in baking oven at 50 c, dry 20 hours to get the modified carbon nano-tube；
(6) Corvic, processing aid and modified carbon nano-tube are added in high-speed mixer after mixing, will be mixed
It is kneaded to prolong for 6-10 minutes in material two-roll mill and is pressed into flaky composite material, certain thickness is made after vulcanizing press hot pressing
The composite board of degree.
2. the method that modified carbon nano-tube according to claim 1 prepares antistatic polyvinyl chloride material, which is characterized in that
Acid potassium bichromate solution is sulfuric acid potassium bichromate solution in the step (1), the volumetric concentration of potassium bichromate is 0.25 mole/
It rises, the volumetric concentration of sulfuric acid is 50-55%.
3. the method that modified carbon nano-tube according to claim 1 prepares antistatic polyvinyl chloride material, which is characterized in that
Maturing temperature in the step (1) is 700-800 degrees Celsius.
4. the method that modified carbon nano-tube according to claim 1 prepares antistatic polyvinyl chloride material, which is characterized in that
The quality proportioning of pyrroles and carbon nanotube is 1 in the step (2):2-3.
5. the method that modified carbon nano-tube according to claim 1 prepares antistatic polyvinyl chloride material, which is characterized in that
The ice bath temperature control is at 0-3 degrees Celsius.
6. the method that modified carbon nano-tube according to claim 1 prepares antistatic polyvinyl chloride material, which is characterized in that
The dosage of ammonium persulfate is 0.56-0.62 times of carbon nanotube dosage in the step (3).
7. the method that modified carbon nano-tube according to claim 1 prepares antistatic polyvinyl chloride material, which is characterized in that
Corvic, processing aid and modified carbon nano-tube mass ratio are 100 in the step (6):15-20:7-12.
8. the method for preparing antistatic polyvinyl chloride material according to modified carbon nano-tube described in right 7, which is characterized in that described
Processing aid includes：15-20 parts of repefral, 5-9 parts of epoxidized soybean oil, 7-12 parts of zinc stearate, dodecyl
3-5 parts of sodium sulphate, 3-5 parts of sodium phosphite and 2-4 parts of melamine.
9. the method that modified carbon nano-tube according to claim 1 prepares antistatic polyvinyl chloride material, which is characterized in that
The temperature of double rod open mills is 165-175 degrees Celsius in the step (6), and front and back roller slewing rate ratio is 1:1-1.2.
10. the method that modified carbon nano-tube according to claim 1 prepares antistatic polyvinyl chloride material, feature exist
In vulcanizing press hot pressing temperature is 150-160 degrees Celsius, hot pressing pressure 12-18MPa in the step (6), hot pressing time
It is 8-12 minutes.
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Cited By (3)
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|---|---|---|---|---|
| CN109777007A (en) * | 2019-02-22 | 2019-05-21 | 华研(佛山)纳米材料有限公司 | A kind of carbon nanotube polyvinyl chloride composite materials and preparation method thereof |
| CN113529202A (en) * | 2021-06-17 | 2021-10-22 | 杭州叶茂纺织有限公司 | Antistatic DTY (draw textured yarn) and preparation process thereof |
| CN113860289A (en) * | 2021-10-21 | 2021-12-31 | 江苏天奈科技股份有限公司 | Method for purifying carbon nano tube |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109777007A (en) * | 2019-02-22 | 2019-05-21 | 华研(佛山)纳米材料有限公司 | A kind of carbon nanotube polyvinyl chloride composite materials and preparation method thereof |
| CN113529202A (en) * | 2021-06-17 | 2021-10-22 | 杭州叶茂纺织有限公司 | Antistatic DTY (draw textured yarn) and preparation process thereof |
| CN113860289A (en) * | 2021-10-21 | 2021-12-31 | 江苏天奈科技股份有限公司 | Method for purifying carbon nano tube |
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