CN113881166B - Multifunctional paste and preparation method thereof - Google Patents

Multifunctional paste and preparation method thereof Download PDF

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CN113881166B
CN113881166B CN202111294678.1A CN202111294678A CN113881166B CN 113881166 B CN113881166 B CN 113881166B CN 202111294678 A CN202111294678 A CN 202111294678A CN 113881166 B CN113881166 B CN 113881166B
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carbon nanotube
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彭小权
陈名海
王小斌
石红义
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Jiangxi Copper Technology Research Institute Co ltd
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Abstract

The invention belongs to the technical field of materials, and particularly relates to a multifunctional paste and a preparation method thereof. The multifunctional paste comprises the following components in percentage by mass: 50-70% of PVC paste resin powder, 20-40% of paste resin plasticizer and 0.1-10% of high-dispersion carbon nanotube composition. The preparation method comprises the following steps: preparing a plasticizer emulsion; shearing and dispersing the carbon nano tube; concentrating and drying the dispersion; and (4) preparing the multifunctional paste. The invention has the beneficial effects that: the multifunctional paste is used in the preparation process of the high-dispersion carbon nano tube composition, and the high-dispersion carbon nano tube-emulsion dispersion is formed under the promotion of high-speed shearing and the interaction force between the micro-nano emulsion-carbon nano tube bundle and the environment-friendly plasticizer molecules. The high-dispersion carbon nanotube composition has the advantages of no pulverization, no oil leakage, high dispersion and convenient use, and is particularly suitable for the fields of permanent antistatic, electric conduction and electromagnetic shielding with low toxicity, health, environmental protection and safety.

Description

Multifunctional paste and preparation method thereof
Technical Field
The invention belongs to the technical field of materials, and particularly relates to a multifunctional paste and a preparation method thereof.
Background
At present, polyvinyl chloride (PVC) paste resin powder is mixed with a plasticizer and stirred to form a stable suspension, which is called PVC plastisol. PVC plastisols are converted to PVC articles by heating alone. The PVC plastisol material has the advantages of convenient preparation, stable performance, excellent product performance, good chemical stability, certain mechanical strength and easy coloring, and can be widely applied to the fields of gloves, wallpaper, curtains, artificial leather, vinyl toys, soft trademarks, wallpaper, paint coatings, foamed plastics and the like.
However, the volume resistance of the multifunctional paste product without the antistatic agent is as high as 1014Ω~1017Omega cm, the static electricity dust absorption, the discharge and the breakdown are easily caused, and fire, explosion, production obstacle and other emergency conditions are caused when the static electricity dust absorption, the discharge and the breakdown are serious. It is necessary to endow the multifunctional pasted surface with antistatic performance in order to widen the application of the multifunctional pasted product in the fields of oil and gas mines, dangerous goods warehouses, electronics, wireless communication and the like. The most common method for improving the antistatic performance of the surface of the multifunctional paste product is to add a small-molecule antistatic agent, but the small-molecule antistatic agent generally has the defects of poor antistatic effect, strong dependence on environmental humidity, easy migration and pollution to the surface of the product, gradual loss of the electrostatic effect and the like.
The multifunctional paste product can be endowed with permanent antistatic performance under severe industrial and mining conditions by adding fillers with certain conductive performance, such as antistatic fillers of conductive carbon black, graphite, carbon Nano Tubes (CNT) and the like. Among them, compared with conductive carbon black and graphite, carbon nanotubes have better processability, less addition amount and more excellent product machinery, and are preferred fillers for permanent antistatic functional materials.
However, the carbon nano tube has the problems of difficult dispersion, difficult processing, easy agglomeration and the like, and is directly applied to an antistatic multifunctional paste product processing system, so the effect is not good. On the other hand, the carbon nanotube powder is easy to float physically, a large amount of dust is generated in the actual processing process, and the harm to the health of production operators is great. In addition, patent CN 103205068A "an antistatic plastic dipping product and its preparation method" clearly indicates that the addition of antistatic agent can significantly reduce the resistivity of the product and has a flame retardant effect, but the addition of antistatic agent can sharply increase the viscosity of the multifunctional paste plastic dipping solution, and only by adding a proper amount of dispersant, the system can meet the plastic dipping process conditions, thereby preparing the flame retardant and antistatic product. The solutions proposed by the authors for adding suitable dispersants have the following drawbacks: (1) The antistatic agent with huge specific surface area can reach the oil absorption value which is several times of the weight of the antistatic agent, the viscosity of the system is obviously increased, the stirring is difficult, and the defects of uneven distribution, unstable antistatic property and the like of the antistatic agent in a multifunctional paste product are inevitably caused. (2) The addition of the dispersant does indeed reduce the viscosity of the multifunctional paste dip, however if one wants to obtain a homogeneous multifunctional paste dip under relatively simple conditions (such as simple mechanical stirring), it is necessary to add a large amount of dispersant for the dispersion of the antistatic agent, which inevitably leads to softening of the multifunctional paste product and a reduction in mechanical properties.
Disclosure of Invention
The present invention discloses a multifunctional paste and a method for preparing the same, which have solved any of the above technical problems and other potential problems of the prior art.
In order to solve the technical problems, the technical scheme of the invention is as follows: the multifunctional paste has the functions of static resistance, electric conduction and electromagnetic shielding, and comprises the following components in percentage by mass: 50-70% of PVC paste resin powder, 20-40% of paste resin plasticizer and 0.1-10% of high-dispersion carbon nanotube composition.
Further, the PVC paste resin powder comprises one or more of P4472, KH31, LK-170 and LP 010F;
the paste resin plasticizer is an environment-friendly plasticizer, and the environment-friendly plasticizer contains an environment-friendly plasticizer of benzene rings.
Further, the high-dispersion carbon nanotube composition comprises the following components in parts by weight: emulsifier: 0.1-1 part, carbon nanotube: 10-50 parts of environment-friendly plasticizer: 50-100 parts.
Further, the diameter of agglomerates in the highly dispersed carbon nanotubes is <5 μm.
Further, the emulsifier is one or more of sucrose ester, ethylene oxide-propylene oxide block copolymer, alkylphenol polyoxyethylene and polyether organic silicon;
the carbon nanotube is
Figure BDA0003336187090000021
NC7000、
Figure BDA0003336187090000022
FT9000、
Figure BDA0003336187090000023
One or more of GT 210;
the environment-friendly plasticizer is an environment-friendly plasticizer containing benzene rings.
Further, the environment-friendly plasticizer containing the benzene ring comprises one or more of octyl terephthalate, diisononyl phthalate, diisodecyl phthalate, diisoundecyl phthalate, diisononyl cyclohexane-1, 2-dicarboxylate, C9-C11 mixed alcohol terephthalate, trioctyl trimellitate, trinonyl trimellitate, trimellitate and polyester plasticizer.
Another object of the present invention is to provide a process for preparing the above multifunctional paste, characterized in that it comprises in particular the following steps:
s1) preparing a plasticizer emulsion;
s2) shearing and dispersing the carbon nano tube, concentrating and drying the dispersion;
s3) preparing multifunctional paste.
Further, the specific steps of S1) are as follows:
s1.1) weighing the materials according to the design components, mixing the environment-friendly plasticizer and the emulsifier, emulsifying at the rotating speed of 500-3000 r/min for 1-30 min,
s1.2) adding absolute ethyl alcohol with the dosage ten times that of the environment-friendly plasticizer, and then starting an emulsification pump again to shear, emulsify and disperse for 1-30 min at a high speed to obtain the plasticizer emulsion.
Further, the specific steps of S2) are:
s2.1) adding the carbon nano tubes into the plasticizer emulsion obtained in S1.2), and shearing and dispersing for 1-30 min at the rotating speed of 500-2000 r/min to obtain a dispersion;
s2.2) transferring the dispersion obtained in the S2.1) into a filter press, carrying out filter pressing concentration, and drying in a drying oven at 90-110 ℃ for 2-4 h to obtain the high-dispersion carbon nanotube composition.
Further, S3.1) uniformly mixing PVC paste resin powder and paste resin plasticizer with the high-dispersion carbon nanotube composition obtained in S2) to obtain paste,
s3.2) coating the paste obtained in S3.1) into a coating with the thickness of 90-110 mu m by a blade coater, and gelatinizing for 30-120min in an oven at the temperature of 120-180 ℃ to obtain the multifunctional paste.
The invention has the following beneficial effects:
when the carbon nano tube is used in the field of permanent antistatic multifunctional paste resin materials, in order to obtain better fluidity, a large amount of additional plasticizer is usually required to obtain better fluidity, and the addition of excessive plasticizer inevitably causes the mechanical property of the terminal multifunctional paste product to be sharply reduced or even become invalid.
An environment-friendly plasticizer-ethanol emulsification system is used as a wetting dispersant to fully shear and disperse multi-walled carbon nanotubes, the carbon nanotubes and benzene rings in the environment-friendly plasticizer have strong intermolecular acting force and good affinity, under the shearing action, the multi-walled carbon nanotubes emulsified and dispersed by the dispersant immediately enter a plasticizer emulsion oil phase under the intermolecular acting force and are limited in the size range of emulsion particles, and a high-dispersion carbon nanotube composition is obtained after drying (attached figures 1 and 4).
The low-boiling point ethanol which is dissociated outside the infiltrated and dispersed carbon nano tube-plasticizer-emulsifier system is easily and fully removed by concentration, filtration and heating, so that the solvent with low molecular weight in the solvent is effectively prevented from being mixed into the terminal product, and the comprehensive mechanical property of the terminal product is basically not influenced.
Compared with the conductive carbon black antistatic agent, the high-dispersion carbon nano tube can reach higher antistatic grade (shown in the attached table II) under the condition of the same addition amount, and the antistatic effect is better.
The invention adopts the traditional processing equipment and process, avoids introducing homogenizing equipment, ultrasonic equipment or special customized machinery with high cost and energy consumption, effectively controls the processing machinery and energy consumption cost, has lower comprehensive production cost and is easy to popularize on a large scale.
The high-dispersion carbon nanotube composition for the multifunctional paste, prepared by the invention, is used for products obtained after the multifunctional paste resin is used, and has the advantages of good mechanical property, no oil leakage on the surface, no precipitation, lasting and stable antistatic property and strong practicability, and is favorable for expanding the large-scale application of the multifunctional paste products in the fields of oil and gas mines, dangerous goods warehouses, electronics, wireless communication and the like.
Drawings
FIG. 1 is a schematic diagram of a process for preparing a highly dispersed carbon nanotube composition in a multifunctional paste according to the present invention.
Fig. 2a is a schematic of the surface topography of a multi-walled carbon nanotube GT 300.
FIG. 2b is a schematic surface topography of 50% GT300-TOTM highly dispersed composition.
FIG. 3 is a schematic diagram showing the dispersion and distribution of carbon nanotubes on the surface of the multifunctional paste resin film.
Fig. 4 is a schematic diagram of a highly dispersed carbon nanotube composition (tested after dilution to 10% from a 30% carbon tube composition).
Detailed Description
The technical solution of the present invention is further explained with reference to the accompanying drawings and specific embodiments.
The multifunctional paste has antistatic, conductive and electromagnetic shielding functions, and comprises the following components in percentage by mass: 50-70% of PVC paste resin powder, 20-40% of paste resin plasticizer and 0.1-10% of high-dispersion carbon nanotube composition.
The PVC paste resin powder comprises one or more of P4472, KH31, LK-170 or LP 010F;
the paste resin plasticizer is an environment-friendly plasticizer, and the environment-friendly plasticizer contains an environment-friendly plasticizer of benzene rings.
The high-dispersion carbon nano tube composition comprises the following components in parts by weight: emulsifier: 0.1-1 part, carbon nanotube: 10-50 parts of environment-friendly plasticizer: 50-100 parts.
The diameter of agglomerates in the highly dispersed carbon nanotubes is <5 μm.
The emulsifier is one or more of sucrose ester, ethylene oxide-propylene oxide block copolymer, alkylphenol polyoxyethylene ether and polyether organic silicon;
the carbon nanotube is
Figure BDA0003336187090000041
NC7000、
Figure BDA0003336187090000042
FT9000、
Figure BDA0003336187090000043
One or more of GT 210;
the environment-friendly plasticizer is an environment-friendly plasticizer containing benzene rings.
The environment-friendly plasticizer containing the benzene ring comprises one or more of octyl terephthalate, diisononyl phthalate, diisodecyl phthalate, diisoundecyl phthalate, cyclohexane 1, 2-diisononyl phthalate, C9-C11 mixed alcohol terephthalate, trioctyl trimellitate, trinonyl trimellitate, trimellitate and polyester plasticizers.
As shown in fig. 1, the present invention provides a method for preparing the multifunctional paste, which specifically comprises the following steps:
s1) preparing a plasticizer emulsion;
s2) shearing and dispersing the carbon nano tube, concentrating and drying the dispersion;
s3) preparing multifunctional paste.
The S1) comprises the following specific steps:
s1.1) weighing the materials according to the design components, mixing the environment-friendly plasticizer and the emulsifier, emulsifying at the rotating speed of 500-3000 r/min for 1-30 min,
s1.2) adding absolute ethyl alcohol with the dosage ten times that of the environment-friendly plasticizer, and then starting an emulsification pump again to shear, emulsify and disperse for 1-30 min at a high speed to obtain the plasticizer emulsion.
The S2) comprises the following specific steps:
s2.1) adding the carbon nano tube into the medium plasticizer emulsion obtained in the S1.2), and shearing and dispersing for 1-30 min at the rotating speed of 500-2000 r/min to obtain a dispersion;
s2.2) transferring the dispersion obtained in the S2.1) into a filter press, carrying out filter pressing concentration, and drying in a drying oven at 90-110 ℃ for 2-4 h to obtain the high-dispersion carbon nanotube composition.
S3.1) PVC paste resin powder and paste resin plasticizer are uniformly mixed with the high-dispersion carbon nano tube composition obtained in S2) to obtain paste,
s3.2) coating the paste obtained in S3.1) into a coating with the thickness of 90-110 mu m by using a blade coater, gelatinizing in an oven at the temperature of 120-180 ℃ for 30-120min to obtain multifunctional paste, and obtaining the volume resistance of the multifunctional paste<10-10Ω.cm,。
The invention provides a multifunctional paste and a preparation method thereof. The preparation method adopts an environment-friendly plasticizer-ethanol emulsion as a carrier, disperses the carbon nano tubes in the ethanol emulsion, and fully shears and disperses to obtain the carbon nano tube-emulsion dispersoid. The dispersion is subjected to pressure filtration and concentration to obtain a carbon nano tube-plasticizer concentrate, and the carbon nano tube-plasticizer concentrate is fully dried in an oven to obtain the high-dispersion carbon nano tube composition. The prepared high-dispersion carbon nano tube composition is mixed with the paste resin liquid and is gelatinized at high temperature to obtain the multifunctional paste. The multifunctional paste is applied to the fields of permanent antistatic, electric conduction and electromagnetic shielding materials, and is particularly suitable for the fields of permanent antistatic, electric conduction and electromagnetic shielding with low toxicity, health, environmental protection and safety.
Preferably, the multifunctional paste can be applied to the fields of permanent antistatic, conductive, electromagnetic shielding and other multifunctional paste products. More preferably, the multifunctional paste is applied to the fields of permanent antistatic, electric conduction and electromagnetic shielding with low toxicity, health, environmental protection and safety, and mainly comprises the fields of permanent antistatic of wall paper, children toys, industrial conveying belts, plastic runways, medical gloves and window and door curtain materials.
Example 1
Mixing 50 parts of DOTP plasticizer and 0.1 part of polyether organic silicon emulsifier, slightly stirring, and transferring to an emulsification pump forStrongly emulsifying and mixing for 3min. After mixing, it was poured into a 5L container containing 200 parts ethanol to form a coarse dispersion emulsion. Starting a high-speed dispersion machine, maintaining the rotating speed at 1500r/min, and shearing and dispersing the coarsely dispersed emulsion at a high speed for 10min by using a high-speed stirring paddle to obtain the micro-nano emulsion. Stopping stirring after the preset stirring time is reached, and adding 10 parts of multi-walled carbon nano-tubes into the emulsion
Figure BDA0003336187090000061
GT300, and stirring at high speed for 20min, and stopping stirring again. Transferring the mixed solution after the secondary dispersion to a 300-mesh filter screen to separate the free ethanol to obtain a concentrated paste. Transferring the concentrated paste into a 110 ℃ oven, and baking for 8h. And (3) collecting the fully dried materials, transferring the materials into a charging hopper of a screw granulator, and performing room-temperature extrusion granulation to obtain the 20% high-dispersion carbon nanotube composition, wherein the percentage is 20% GT300-DOTP. 100 parts of PVC paste resin powder LK-170 and 100 parts of DOTP plasticizer were mixed with 20 parts of 20% GT300-DOTP and stirred to obtain a PVC paste. The PVC paste was applied to a 100 μm thick coating with an applicator and gelatinized in an oven at 150 ℃ for 2 hours to prepare a multifunctional paste.
Example 2
100 parts of DINCH plasticizer and 1 part of alkylphenol polyoxyethylene ether emulsifier are mixed, slightly stirred and transferred to an emulsification pump for strong emulsification and mixing for 3min. After mixing, it was poured into a 5L container containing 1000 parts of ethanol to form a coarse dispersion emulsion. Starting a high-speed dispersion machine, maintaining the rotating speed at 1500r/min, and shearing and dispersing the coarsely dispersed emulsion at a high speed for 10min by using a high-speed stirring paddle to obtain the micro-nano emulsion. Stopping stirring after the preset stirring time is reached, and adding 50 parts of multi-walled carbon nano-tubes into the emulsion
Figure BDA0003336187090000062
And (3) NC7000, continuing to stir at high speed for dispersion for 20min, and then stopping stirring again. Transferring the mixed solution after the secondary dispersion to a 300-mesh filter screen to separate the free ethanol to obtain a concentrated paste. Transferring the concentrated paste into a 110 ℃ oven, and baking for 8h. After the fully dried materials are collected, the materials are rotatedTransferring into a charging hopper of a screw granulator, and performing extrusion granulation at room temperature to obtain a 50% high-dispersion carbon nanotube composition, which is recorded as 50% NC7000-DINCH. 100 parts of PVC paste resin powder P4472, 150 parts of DINCH plasticizer and 50 parts of 50% NC7000-DINCH were mixed and stirred to obtain a PVC paste. The PVC paste was applied to a 100 μm thick coating with an applicator and gelatinized in an oven at 180 ℃ for 1 hour to prepare a multifunctional paste.
Example 3
75 parts of 911P plasticizer and 0.55 part of sucrose ester emulsifier are mixed, slightly stirred and transferred to an emulsification pump for strong emulsification and mixing for 3min. After mixing, it was poured into a 5L container containing 500 parts ethanol to form a coarse dispersion emulsion. Starting a high-speed dispersion machine, maintaining the rotating speed at 1500r/min, and shearing and dispersing the coarsely dispersed emulsion at a high speed for 10min by using a high-speed stirring paddle to obtain the micro-nano emulsion. Stopping stirring after the preset stirring time is reached, and adding 25 parts of multi-walled carbon nano-tubes into the emulsion
Figure BDA0003336187090000063
FT9000, dispersion was continued with high-speed stirring for 20min, and then stirring was stopped again. Transferring the mixed solution after the secondary dispersion to a 300-mesh filter screen to separate the free ethanol to obtain a concentrated paste. Transferring the concentrated paste into a 110 ℃ oven, and baking for 8h. And (3) collecting the fully dried materials, transferring the materials into a feed hopper of a screw granulator, and performing room-temperature extrusion granulation to obtain the 33% high-dispersion carbon nanotube composition, wherein the mark is 33% FT9000-911P. 100 parts of PVC paste resin powder LP010F, 200 parts of 911P plasticizer and 33 parts of 33-percent FT900-911P were mixed and stirred to obtain a PVC paste. The PVC paste was applied to a 100 μm thick coating with an applicator and gelatinized in an oven at 160 ℃ for 1.5 hours to prepare a multifunctional paste.
Example 4
25 parts of DIDP plasticizer, 25 parts of DUP plasticizer and 0.1 part of ethylene oxide-propylene oxide block copolymer emulsifier were mixed, gently stirred, and transferred to an emulsification pump for intensive emulsification mixing for 3min. After mixing, it was poured into a 5L container containing 200 parts ethanol to form a coarse dispersion emulsion. Starting the high-speed dispersion machine, maintaining the rotating speed at 1500r/min, and benefitingAnd (4) shearing and dispersing the coarsely dispersed emulsion for 10min at a high speed by using a high-speed stirring paddle to obtain the micro-nano emulsion. Stopping stirring after the preset stirring time is reached, and adding 5 parts of multi-walled carbon nano-tubes into the emulsion
Figure BDA0003336187090000071
GT300, 5 parts multi-wall carbon nano-tube
Figure BDA0003336187090000072
And NC7000, continuously stirring at high speed for dispersing for 20min, and then stopping stirring again. Transferring the mixed solution after the secondary dispersion to pass through a 300-mesh filter screen to separate the free ethanol to obtain a concentrated paste. Transferring the concentrated paste into a 110 ℃ oven, and baking for 8h. Collecting the fully dried material, transferring into the charging hopper of a screw granulator, and performing extrusion granulation at room temperature to obtain 20% highly dispersed carbon nanotube composition, as 20% GT300/NC7000-DIDP/DUP. 100 parts of PVC paste resin powder LP010F, 80 parts of 911P plasticizer and 20 parts of 20-percent GT300/NC7000-DIDP/DUP were mixed and stirred to obtain a PVC paste. The PVC paste was applied to a 100 μm thick coating with an applicator and gelatinized in an oven at 150 ℃ for 2 hours to prepare a multifunctional paste.
Example 5
Mixing 30 parts of TOTM plasticizer, 30 parts of TINTM plasticizer, 30 parts of TM380 plasticizer and 1 part of alkylphenol polyoxyethylene ether emulsifier, slightly stirring, and transferring to an emulsification pump for strong emulsification and mixing for 3min. After mixing, it was poured into a 5L container containing 1000 parts of ethanol to form a coarse dispersion emulsion. Starting a high-speed dispersion machine, maintaining the rotating speed at 1500r/min, and shearing and dispersing the coarsely dispersed emulsion at a high speed for 10min by using a high-speed stirring paddle to obtain the micro-nano emulsion. Stopping stirring after the preset stirring time is reached, and adding 45 parts of multi-walled carbon nano tubes into the emulsion
Figure BDA0003336187090000073
And (3) NC7000, continuing to stir at high speed for dispersion for 20min, and then stopping stirring again. Transferring the mixed solution after the secondary dispersion to a 300-mesh filter screen to separate the free ethanol to obtain a concentrated paste. Transferring the concentrated paste to a 110 deg.C ovenAnd (4) baking for 8 hours. Collecting the fully dried material, transferring into the hopper of a screw granulator, and performing extrusion granulation at room temperature to obtain 50% highly dispersed carbon nanotube composition, as 50% NC7000-TOTM/TINTM/TM380. 100 parts of PVC paste resin powder KH31, 40 parts of TOTM plasticizer, 20 parts of TINTM plasticizer, 20 parts of TM380 plasticizer and 20 parts of 50% NC7000-TOTM/TINTM/TM380 were mixed and stirred to obtain a PVC paste. The PVC paste was applied to a 100 μm thick coating using an applicator and gelatinized in an oven at 180 ℃ for 1 hour to prepare a multifunctional paste.
Comparative example 1
The ethanol in example 1 was replaced with equal mass of DOTP plasticizer, and the other ingredients and procedures were maintained. The resulting highly dispersed carbon nanotube compositions were evaluated according to the corresponding test standards.
Comparative example 2
Example 1 replacing the carbon nanotubes with an equal mass of conductive carbon black (
Figure BDA0003336187090000083
VXC 72R), other components and steps were kept constant. The multifunctional paste resin obtained was evaluated according to the corresponding test standards.
Characterization of the properties of the carbon nanotube composition
Figure BDA0003336187090000081
Characterization of multifunctional paste resin Properties of appendix II
Figure BDA0003336187090000082
Figure BDA0003336187090000091
As can be seen from the performance characterization test of the carbon nanotube composition attached to the table, the carbon nanotube composition for the multifunctional paste resin, prepared by the invention, has the carbon nanotube content ranging from 20% to 50%, the actual content basically consistent with the set value, low volume resistivity, good surface conductivity and no shedding and chalking phenomena. From the characterization results of example 5 in the characterization of the performance of the multifunctional paste resin of the second attached form, it can be seen that the multifunctional paste prepared by using the highly dispersed carbon nanotube composition in the patent of the invention has no dust emission phenomenon, and the multifunctional paste resin film has smooth and particle-free surface, no stickiness on the surface and no oil bleeding. In contrast, in comparative example 1, it can be seen that the carbon tubes in the carbon tube composition obtained by the method of directly adding the dispersant are fine and are entangled with each other seriously (fig. 2, left figure), and the multifunctional paste resin film prepared from the composition exhibits the poor characteristics of high surface resistance value, sticky surface and the like. In comparative example 2, it can be seen that, when the carbon nanotubes are replaced with the conductive carbon black of equal mass, the prepared multifunctional paste resin film has a non-smooth surface, an antistatic property on the surface, and a high resistance.
As can be seen from 50% of the surface morphology of the GT300-TOTM highly dispersed composition, the carbon tubes within the highly concentrated carbon tube dispersed composition prepared by this method are thicker and shorter than before dispersion and less entangled with each other (FIG. 2, right drawing), which facilitates dilution and dispersion in the matrix paste resin system. From the SEM images of the dispersion and distribution of the carbon nanotubes on the surface of the multifunctional paste resin film, the multifunctional paste resin film with different carbon nanotube contents prepared by the invention has the advantages that the carbon nanotubes are uniformly dispersed and distributed in the paste resin, and the agglomeration amount is small (figure 3).
The multifunctional paste and the preparation method thereof provided by the embodiment of the application are described in detail above. The above description of the embodiments is only for the purpose of helping to understand the method of the present application and its core idea; meanwhile, for a person skilled in the art, according to the idea of the present application, there may be variations in the specific embodiments and the application scope, and in summary, the content of the present specification should not be construed as a limitation to the present application.
As used in the specification and claims, certain terms are used to refer to particular components. As one skilled in the art will appreciate, manufacturers may refer to a component by different names. This specification and claims do not intend to distinguish between components that differ in name but not function. In the following description and in the claims, the terms "include" and "comprise" are used in an open-ended fashion, and thus should be interpreted to mean "include, but not limited to. "substantially" means within an acceptable error range, and a person skilled in the art can solve the technical problem within a certain error range to substantially achieve the technical effect. The description which follows is a preferred embodiment of the present application, but is made for the purpose of illustrating the general principles of the application and not for the purpose of limiting the scope of the application. The protection scope of the present application shall be subject to the definitions of the appended claims.
It is also noted that the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a good or system that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such good or system. Without further limitation, an element defined by the phrases "comprising one of \8230;" does not exclude the presence of additional like elements in an article or system comprising the element.
It should be understood that the term "and/or" as used herein is merely a relationship that describes an associated object, meaning that three relationships may exist, e.g., a and/or B, may represent: a exists alone, A and B exist simultaneously, and B exists alone. In addition, the character "/" herein generally indicates that the former and latter associated objects are in an "or" relationship.
The foregoing description shows and describes several preferred embodiments of the present application, but as aforementioned, it is to be understood that the application is not limited to the forms disclosed herein, but is not to be construed as excluding other embodiments and is capable of use in various other combinations, modifications, and environments and is capable of changes within the scope of the application as described herein, commensurate with the above teachings, or the skill or knowledge of the relevant art. And that modifications and variations may be effected by those skilled in the art without departing from the spirit and scope of the application, which is to be protected by the claims appended hereto.

Claims (7)

1. A method for preparing a multifunctional paste, characterized in that it comprises in particular the following steps:
s1) preparing a plasticizer emulsion;
the method comprises the following specific steps: s1.1) mixing an environment-friendly plasticizer and an emulsifier, emulsifying for 1-30min at the rotating speed of 500-3000 r/min, and then S1.2) adding absolute ethyl alcohol with the amount ten times of that of the environment-friendly plasticizer, and starting an emulsifying pump again to shear, emulsify and disperse for 1-30 min at a high speed to obtain a plasticizer emulsion;
s2) shearing and dispersing the carbon nano tube, concentrating and drying the dispersion;
the method comprises the following specific steps: s2.1) adding the carbon nano tube into the plasticizer emulsion obtained in the S1.2), and shearing and dispersing for 1-30 min at the rotating speed of 500-2000 r/min to obtain a dispersion; s2.2) transferring the dispersion obtained in the S2.1) into a filter press, carrying out filter pressing concentration, and drying in an oven at 90-110 ℃ for 2-4 h to obtain a high-dispersion carbon nanotube composition;
s3) preparing multifunctional paste;
the specific steps of S3) are as follows: s3.1) uniformly mixing PVC paste resin powder, paste resin plasticizer and the high-dispersion carbon nanotube composition obtained in S2) to obtain paste, S3.2) coating the paste obtained in S3.1) into a coating with the thickness of 90-110 microns by using a blade coater, and gelatinizing for 30-120min in an oven with the temperature of 120-180 ℃ to obtain the multifunctional paste with the functions of static resistance, electric conduction and electromagnetic shielding.
2. The method of claim 1, wherein the: 50-70% of PVC paste resin powder, 20-40% of paste resin plasticizer and 0.1-10% of high-dispersion carbon nanotube composition.
3. The method according to claim 1, characterized in that said PVC paste resin powder comprises one or more of P4472, KH31, LK-170, LP 010F; the paste resin plasticizer is an environment-friendly plasticizer, and the environment-friendly plasticizer contains an environment-friendly plasticizer of benzene rings.
4. The method of claim 1, wherein the highly dispersed carbon nanotube composition comprises the following components in parts by weight: emulsifier: 0.1-1 part, carbon nanotube: 10-50 parts of environment-friendly plasticizer: 50 to 100 portions.
5. The method of claim 4, wherein the diameter of agglomerates in the highly dispersed carbon nanotube composition is <5 μm.
6. The method of claim 4, wherein the emulsifier is one or more of sucrose ester, ethylene oxide-propylene oxide block copolymer, alkylphenol ethoxylate and polyether organic silicon; the carbon nanotube is NANOCYL
Figure DEST_PATH_IMAGE001
NC7000、CNANO
Figure 539785DEST_PATH_IMAGE001
FT9000、DAZHAN
Figure 934994DEST_PATH_IMAGE001
One or more of GT 210; the environment-friendly plasticizer is an environment-friendly plasticizer containing benzene rings.
7. The method according to claim 4, wherein the environment-friendly plasticizer is an environment-friendly plasticizer containing a benzene ring, and the environment-friendly plasticizer containing a benzene ring comprises one or more of octyl terephthalate, diisononyl phthalate, diisodecyl phthalate, diisoundecyl phthalate, cyclohexane 1, 2-diisononyl phthalate, C9-C11 mixed alcohol terephthalate, trimellitate and polyester plasticizer.
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