CN112480639B - Efficient super-tough conductive PC material and preparation method thereof - Google Patents
Efficient super-tough conductive PC material and preparation method thereof Download PDFInfo
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L69/00—Compositions of polycarbonates; Compositions of derivatives of polycarbonates
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
- B29B7/00—Mixing; Kneading
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
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- B29B9/06—Making granules by dividing preformed material in the form of filamentary material, e.g. combined with extrusion
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
- B29C48/022—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor characterised by the choice of material
- B29C48/023—Extruding materials comprising incompatible ingredients
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
- B29C48/03—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor characterised by the shape of the extruded material at extrusion
- B29C48/04—Particle-shaped
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
- B29C48/25—Component parts, details or accessories; Auxiliary operations
- B29C48/36—Means for plasticising or homogenising the moulding material or forcing it through the nozzle or die
- B29C48/375—Plasticisers, homogenisers or feeders comprising two or more stages
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
- B29C48/25—Component parts, details or accessories; Auxiliary operations
- B29C48/36—Means for plasticising or homogenising the moulding material or forcing it through the nozzle or die
- B29C48/50—Details of extruders
- B29C48/76—Venting, drying means; Degassing means
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
- B29C48/25—Component parts, details or accessories; Auxiliary operations
- B29C48/92—Measuring, controlling or regulating
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/20—Compounding polymers with additives, e.g. colouring
- C08J3/22—Compounding polymers with additives, e.g. colouring using masterbatch techniques
- C08J3/226—Compounding polymers with additives, e.g. colouring using masterbatch techniques using a polymer as a carrier
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C2945/00—Indexing scheme relating to injection moulding, i.e. forcing the required volume of moulding material through a nozzle into a closed mould
- B29C2945/76—Measuring, controlling or regulating
- B29C2945/76494—Controlled parameter
- B29C2945/76531—Temperature
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29K—INDEXING SCHEME ASSOCIATED WITH SUBCLASSES B29B, B29C OR B29D, RELATING TO MOULDING MATERIALS OR TO MATERIALS FOR MOULDS, REINFORCEMENTS, FILLERS OR PREFORMED PARTS, e.g. INSERTS
- B29K2069/00—Use of PC, i.e. polycarbonates or derivatives thereof, as moulding material
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- C08J2369/00—Characterised by the use of polycarbonates; Derivatives of polycarbonates
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2469/00—Characterised by the use of polycarbonates; Derivatives of polycarbonates
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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- C08K2201/001—Conductive additives
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- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
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Abstract
The invention discloses a high-efficiency super-tough conductive PC material and a preparation method thereof. The material comprises 75-90 parts of polycarbonate, 10-15 parts of conductive PC master batch, 2-5 parts of toughening agent, 0.2-0.5 part of antioxidant and 0.2-0.5 part of dispersant by mass; wherein, the conductive PC master batch comprises 25 to 35 parts of silicon co-polycarbonate powder, 30 to 40 parts of polycarbonate, 30 to 40 parts of conductive filler, 0.1 to 0.5 part of antioxidant and 0.3 to 1 part of dispersant by mass. The high-efficiency super-tough conductive PC material provided by the invention has the advantages that the dispersion effect is improved through the conductive PC master batch, the purposes of reducing the surface resistivity of the PC material and improving the conductive efficiency can be achieved, the toughening effect is realized, the impact property of the PC material is improved, and the wide market prospect is realized.
Description
Technical Field
The invention belongs to the technical field of conductive modified plastics, and particularly relates to a high-efficiency super-tough conductive PC material and a preparation method thereof.
Background
The polycarbonate (PC for short) has the characteristics of high toughness, high rigidity and high heat resistance, is very suitable for the production of electric products, has more and more applications in the fields of electronics, integrated circuit packaging, electromagnetic shielding and the like, and has wide market prospect.
Most of the existing conductive modified plastics are directly added with conductive fillers and conductive fibers in PC/PCT to be dispersed in the whole system matrix, and the addition amount of the conductive agent is too large, so that the cost is increased. In the prior art, a method of adopting PC conductive master batches is adopted, but the addition amount of the carbon nano tubes is large, the pretreatment process is complex, and the toughening effect is not realized.
In order to more effectively improve the surface resistivity of PC, reduce the addition of a conductive agent and improve the impact property of a material, a new PC conductive processing technology and a new PC conductive formula system are urgently needed.
Disclosure of Invention
The invention aims to overcome the defects of the prior art, provides a high-efficiency super-tough conductive PC material and a preparation method thereof, and solves the problem of both conductivity modification and toughness enhancement in the background technology.
One of the technical schemes adopted by the invention for solving the technical problems is as follows: the high-efficiency super-tough conductive PC material is prepared from the following raw materials in parts by mass:
the conductive PC master batch is prepared from the following raw materials in parts by mass:
in a preferred embodiment of the invention, the composition comprises the following raw materials in parts by mass:
the conductive PC master batch is prepared from the following raw materials in parts by mass:
the second technical scheme adopted by the invention for solving the technical problems is as follows: the preparation method of the high-efficiency super-tough conductive PC material comprises the following steps:
s10, uniformly mixing silicon copolymerization PC powder, polycarbonate, conductive filler, antioxidant and dispersing agent according to a mass part ratio, and granulating in a double-screw extruder to prepare conductive PC master batches; wherein the temperature of each section of the double-screw extruder is 250-290 ℃;
s20, uniformly mixing the polycarbonate, the conductive PC master batch, the antioxidant, the flexibilizer and the dispersing agent according to the mass part ratio, and adding the mixture into a double-screw extruder, wherein the temperature of each section of the double-screw extruder is 250-290 ℃.
In a preferred embodiment of the present invention, the step S10 adopts a segmented temperature setting:
1. a feed inlet: 250-270 ℃;
2. conveying and melting: melting the materials at 260-280 ℃;
3. mixing: 280-300 ℃;
4. exhausting: 280-300 ℃; wherein the dispersion temperature of the conductive filler is 280 ℃;
5. extrusion section/die: 260-280 ℃.
Compared with the background technology, the technical scheme has the following advantages:
1. according to the preparation method of the high-efficiency super-tough conductive PC material, the conductive PC master batch is prepared for the first time, and then the high-efficiency super-tough conductive PC material is prepared by taking the conductive PC master batch as a raw material, so that the surface resistivity of an alloy material is reduced and the conductive efficiency is improved while a small amount of conductive filler is added;
2. compared with the PC conductive master batch prepared by directly using the carbon nano tube, the addition of about 50% of conductive filler can be reduced, and the impact property of the material is greatly improved; the high-efficiency super-tough conductive PC material has high conductive efficiency, does not need to depend on a large amount of conductive filler, has high impact strength, is suitable for occasions with higher requirements on the toughness of the material, and has wide market prospect;
3. the invention sets the subsection temperature: 1. a feed inlet: 250-270 ℃; 2. conveying and melting: melting the materials at 260-280 ℃; 3. mixing: the shearing effect is ensured at the temperature of 280-300 ℃; 4. exhausting: preventing material from overflowing at 280-300 deg.C; wherein the temperature of 280 ℃ is suitable for the dispersion of the carbon nano tube; 5. the extrusion section/die head temperature of 260-280 ℃ ensures the mixing of the latter section and avoids the degradation of the material due to high temperature.
Detailed Description
In the following embodiments 1 to 3, the preparation method of the highly efficient super-tough conductive PC material is as follows:
s10, uniformly mixing silicon copolymerized PC, a conductive filler, an antioxidant and a dispersing agent according to a weight part ratio, and then granulating in a double-screw extruder to prepare conductive PC master batches; wherein the temperature of each section of the double-screw extruder is 250-300 ℃; in this step, different sections should set up different temperatures, 1, charge door: 250-270 ℃; 2. conveying and melting: melting the materials at 260-280 ℃; 3. mixing: the shearing effect is ensured at the temperature of 280-300 ℃; 4. exhausting: preventing material from overflowing at 280-300 deg.C; wherein the temperature of 280 ℃ is suitable for the dispersion of the carbon nano tube; 5. the temperature of the extrusion section/die head is 260-280 ℃ to ensure the mixing of the rear section and avoid the material degradation due to high temperature.
S20, uniformly mixing the PC, the conductive PC master batch, the antioxidant, the toughening agent and the dispersing agent according to the weight part ratio, and adding the mixture into a double-screw extruder, wherein the temperature of each section of the double-screw extruder is 250-290 ℃; in the step, the mixing effect of the master batch and the PC needs the temperature of more than 250 ℃; if it is too low, the dispersion of the carbon nanotubes is not favored, but the temperature is not higher than 290 ℃ so as to avoid the material degradation.
Wherein the conductive filler is a multi-walled carbon nanotube. The multi-walled carbon nanotubes are interwoven to form a dendritic network structure.
The toughening agent comprises at least one of organosilicon-styrene-acrylate copolymer, ethylene-acrylate-glycidyl methacrylate copolymer, ethylene-glycidyl methacrylate copolymer, styrene grafted maleic anhydride and ethylene-vinyl acetate copolymer.
The antioxidant comprises at least one of hindered phenol antioxidant, thioester antioxidant and phosphite antioxidant.
The dispersing agent comprises at least one of stearate, stearamide, E wax, silicone powder and PETS.
The content of polysilicon in the silicon copolymerized PC powder is 15-25wt%. The existence of the silicon copolymerized PC powder can greatly improve the impact strength of the material and endow the material with higher toughness.
The raw materials used in the following examples or comparative examples are commercially available products:
PC is 2405 series produced by Kesimong; the silicon copolymerization PC powder is a Xintong color D-0013 series; the carbon black is AC-80 series produced by the Czech republic of China; the carbon nanotube is CP series of products of Korean LG company; the dispersant in the conductive PC master batch is American Longsha PETS. In addition, the raw materials used are all commercial products or prepared by the conventional methods in the field unless otherwise specified.
The following examples or comparative examples relate to three PC conductive masterbatches, as shown in Table 1
TABLE 1
Name of raw materials | 1# Master batch | 2# Master batch | 3# Master batch |
Polycarbonate resin | 36 portions of | 66 portions of | 66 portions of |
Silicon copolymerized polycarbonate | 30 portions of | -- | -- |
Carbon black | 33 portions of | ||
Carbon nanotube | 33 portions of | 33 portions of | -- |
Antioxidant 168 | 0.3 part | 0.3 part | 0.3 part |
Dispersant PETS | 0.7 portion of | 0.7 portion of | 0.7 portion of |
Examples 1 to 3 and comparative examples 1 to 6 Components, as shown in Table 2
TABLE 2
The conductive PCs prepared in the above examples and comparative examples were prepared into a sample plate, and surface resistance was measured using a ZC36 type high resistance meter, and the measurement results are specifically shown in table 3:
TABLE 3
As is clear from Table 3, the samples of examples 1, 2 and 3 had a maximum number of surface resistances of 10 in the order of the maximum number of surface resistances 4 And comparative examples 3 and 4 have surface resistances of up to 10 11 From the above, it is understood that the conductive effect of the carbon nanotubes is much better than that of the carbon black at the same addition ratio. And comparing example 1 and example 2 with comparative example 5 and comparative example 6, while reaching 10 4 The PC conductive master batch prepared by the method has the advantages that the addition of conductive fillers can be reduced by about 50% compared with the PC conductive master batch prepared by directly using the carbon nano tube, and the impact property of the material is greatly improved. In the examples 2 and 3 and the comparative examples 1 and 2, only the silicon copolymerized PC is added under the same carbon nanotube content, the surface resistance of the material can be improved by one order of magnitude, and the toughness of the material can be improved by about 50%.
It can be seen from this that:
the carbon nano tube adopted in the invention has better conductive effect than carbon black; and the conductive PC master batch is fully dispersed in the polycarbonate matrix, so that the dispersion effect of the conductive filler is improved, and the carbon nano tube is easier to bridge to form a conductive network structure.
In addition, due to the addition of the silicon copolymerized PC powder, the impact strength of the material is greatly improved, and the influence of the conductive filler on the impact performance is improved. And because the silicon copolymerization PC is powder, the silicon copolymerization PC can be better mixed with the carbon nano tube, namely, the silicon copolymerization PC can be better fed and dispersed during production, and the carbon nano tube can be easier to form a conductive network structure so as to reduce the addition amount of the carbon nano tube.
Therefore, the high-efficiency super-tough conductive PC material prepared by the method has high conductive efficiency, does not need to depend on a large amount of conductive filler, has high impact strength, is suitable for occasions with higher requirements on the toughness of the material, and has wide market prospect.
The above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; while the invention has been described in detail and with reference to the foregoing embodiments, it will be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; and the modifications or the substitutions do not make the essence of the corresponding technical solutions depart from the scope of the technical solutions of the embodiments of the present invention.
Claims (8)
1. A high-efficiency super-tough conductive PC material is characterized in that: the composition comprises the following raw materials in parts by mass:
the conductive PC master batch is prepared from the following raw materials in parts by mass:
the conductive filler is a multi-walled carbon nanotube, and the multi-walled carbon nanotube is interwoven to form a dendritic network structure.
4. the highly efficient super tough conductive PC material of claim 1, wherein: the toughening agent comprises at least one of organosilicon-styrene-acrylate copolymer, ethylene-acrylate-glycidyl methacrylate copolymer, ethylene-glycidyl methacrylate copolymer, styrene grafted maleic anhydride and ethylene-vinyl acetate copolymer.
5. The high efficiency super tough conductive PC material of claim 1, wherein: the antioxidant comprises at least one of hindered phenol antioxidant, thioester antioxidant and phosphite antioxidant.
6. The highly efficient super tough conductive PC material of claim 1, wherein: the content of polysilicon in the silicon copolymerized PC powder is 15-25wt%.
7. The method for preparing the high-efficiency super-tough conductive PC material as claimed in any one of claims 1 to 6, wherein the method comprises the following steps: the method comprises the following steps:
s10, uniformly mixing silicon copolymerization PC powder, polycarbonate, conductive filler, antioxidant and dispersing agent according to a mass part ratio, and granulating in a double-screw extruder to prepare conductive PC master batches; wherein the temperature of each section of the double-screw extruder is 250-290 ℃;
s20, uniformly mixing the polycarbonate, the conductive PC master batch, the antioxidant, the toughening agent and the dispersing agent according to the mass part ratio, and adding the mixture into a double-screw extruder, wherein the temperature of each section of the double-screw extruder is 250-290 ℃.
8. The method for producing according to claim 7, characterized in that: the step S10 adopts a segmented temperature setting:
1. a feeding port: 250-270 ℃;
2. conveying and melting: melting the materials at 260-280 deg.C;
3. mixing: 280 ℃;
4. exhausting: 280 ℃; wherein the dispersion temperature of the conductive filler is 280 ℃;
5. extrusion section/die: 260-280 ℃.
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