CN114750441B - Magnetic orientation arrangement wave-absorbing thermoplastic wire and preparation method thereof - Google Patents

Magnetic orientation arrangement wave-absorbing thermoplastic wire and preparation method thereof Download PDF

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CN114750441B
CN114750441B CN202210514983.5A CN202210514983A CN114750441B CN 114750441 B CN114750441 B CN 114750441B CN 202210514983 A CN202210514983 A CN 202210514983A CN 114750441 B CN114750441 B CN 114750441B
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wave
absorbing
thermoplastic
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CN114750441A (en
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周金堂
刘一杰
罗成
何晓璇
姚正军
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Nanjing University of Aeronautics and Astronautics
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Nanjing University of Aeronautics and Astronautics
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B29WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29DPRODUCING PARTICULAR ARTICLES FROM PLASTICS OR FROM SUBSTANCES IN A PLASTIC STATE
    • B29D99/00Subject matter not provided for in other groups of this subclass
    • B29D99/0078Producing filamentary materials
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B29WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29BPREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
    • B29B7/00Mixing; Kneading
    • B29B7/002Methods
    • B29B7/005Methods for mixing in batches
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B29WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29BPREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
    • B29B7/00Mixing; Kneading
    • B29B7/80Component parts, details or accessories; Auxiliary operations
    • B29B7/88Adding charges, i.e. additives
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B29WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29CSHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C48/00Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
    • B29C48/03Extrusion 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
    • B29C48/05Filamentary, e.g. strands
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B29WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29CSHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C48/00Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
    • B29C48/14Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor characterised by the particular extruding conditions, e.g. in a modified atmosphere or by using vibration
    • B29C48/142Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor characterised by the particular extruding conditions, e.g. in a modified atmosphere or by using vibration using force fields, e.g. gravity or electrical fields
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B29WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29CSHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C48/00Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
    • B29C48/14Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor characterised by the particular extruding conditions, e.g. in a modified atmosphere or by using vibration
    • B29C48/144Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor characterised by the particular extruding conditions, e.g. in a modified atmosphere or by using vibration at the plasticising zone
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L27/00Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers
    • C08L27/02Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers not modified by chemical after-treatment
    • C08L27/04Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers not modified by chemical after-treatment containing chlorine atoms
    • C08L27/06Homopolymers or copolymers of vinyl chloride
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L61/00Compositions of condensation polymers of aldehydes or ketones; Compositions of derivatives of such polymers
    • C08L61/04Condensation polymers of aldehydes or ketones with phenols only
    • C08L61/16Condensation polymers of aldehydes or ketones with phenols only of ketones with phenols
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L77/00Compositions of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Compositions of derivatives of such polymers
    • C08L77/02Polyamides derived from omega-amino carboxylic acids or from lactams thereof
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B29WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29LINDEXING SCHEME ASSOCIATED WITH SUBCLASS B29C, RELATING TO PARTICULAR ARTICLES
    • B29L2031/00Other particular articles
    • B29L2031/731Filamentary material, i.e. comprised of a single element, e.g. filaments, strands, threads, fibres
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00Specific properties of additives
    • C08K2201/01Magnetic additives

Abstract

The invention discloses a magnetic orientation arrangement wave-absorbing thermoplastic wire and a preparation method thereof, wherein the preparation method comprises the following steps: dissolving thermoplastic resin by using an organic solvent; step two, adding wave-absorbing powder into the dissolved thermoplastic resin, stirring and dispersing, and evaporating the organic solvent to obtain a colloid mixture; washing the colloid mixture, removing the residual organic solvent, and drying to obtain a thermoplastic wave-absorbing master batch; step four, mixing the thermoplastic wave-absorbing master batch with an auxiliary agent to obtain a mixed material; and step five, adding the mixed material into a double-screw extruder for drawing wires, applying an external magnetic field in front of a machine head of the double-screw extruder, drawing the wires, and finally solidifying to obtain the wave-absorbing thermoplastic wires in magnetic orientation arrangement. The material of the invention has excellent electromagnetic wave absorption performance and mechanical performance.

Description

Magnetic orientation arrangement wave-absorbing thermoplastic wire and preparation method thereof
Technical Field
The invention belongs to the field of materials, relates to a wave-absorbing material, and particularly relates to a magnetic orientation arrangement wave-absorbing thermoplastic wire material and a preparation method thereof.
Background
The current information age brings the development of electronic science and technology, and more electronic devices gradually become the mainstream of society, covering the aspects of household, military, medical treatment, communication, production and the like. With the popularization of electronic devices, electromagnetic radiation is inevitably brought about by the use of electromagnetic waves, and the electromagnetic radiation can have bad influence on various fields in life. For example, the precise electronic components interfere with each other, so that the service life of the precise electronic components is shortened; it can cause insomnia, headache, and cardiovascular diseases.
In recent years, research, production and use of electromagnetic wave absorbing materials are gradually and widely concerned by various countries, and meanwhile, on the basis of traditional wave absorbing materials, the pursuit of thin, light, wide and strong wave absorbing materials is a key point and a hot point of research. Under such new requirements, thermoplastic resins have been increasingly focused on the current research because of their low density, reusability, and excellent electrical properties. However, the magnetic absorbent is not easy to disperse and agglomerate due to its high density, which not only causes a decrease in magnetic properties, but also causes a decrease in mechanical properties due to agglomeration of magnetic particles. Based on the current problems, the dispersion of the magnetic particles and the directional arrangement of the magnetic particles are significant to the improvement of the magnetic loss capacity of the wave-absorbing material.
Disclosure of Invention
The invention provides a magnetic orientation arrangement wave-absorbing thermoplastic wire and a preparation method thereof, which aim to overcome the defects of the prior art.
In order to realize the aim, the invention provides a preparation method of a magnetic orientation arrangement wave-absorbing thermoplastic wire material, which is characterized in that: the method comprises the following steps:
firstly, dissolving thermoplastic resin by using an organic solvent;
step two, adding wave-absorbing powder into the dissolved thermoplastic resin, stirring and dispersing, and evaporating the organic solvent to obtain a colloid mixture;
washing the colloid mixture, removing the residual organic solvent, and drying to obtain a thermoplastic wave-absorbing master batch;
step four, mixing the thermoplastic wave-absorbing master batch with an auxiliary agent to obtain a mixed material;
and step five, adding the mixed material into a double-screw extruder for drawing wires, applying an external magnetic field in front of a machine head of the double-screw extruder, drawing the wires, and finally solidifying to obtain the wave-absorbing thermoplastic wires in magnetic orientation arrangement.
Further, the invention provides a preparation method of the magnetic orientation arrangement wave-absorbing thermoplastic wire, which can also have the following characteristics: the composite material comprises the following raw materials in parts by weight: 60-70 parts of thermoplastic resin, 25-30 parts of wave-absorbing powder and 5-10 parts of auxiliary agent.
Further, the invention provides a preparation method of the magnetic orientation arrangement wave-absorbing thermoplastic wire, which can also have the following characteristics: wherein the thermoplastic resin is one or more of Polyetheretherketone (PEEK), polyvinyl chloride (PVC), nylon 6 (PA 6), nylon 66 (PA 66) and polylactic acid (PLA).
Further, the invention provides a preparation method of the magnetic orientation arrangement wave-absorbing thermoplastic wire, which can also have the following characteristics: the wave-absorbing powder is a mixture of carbonyl iron and graphene, and each wave-absorbing powder accounts for 5-95% of the total weight of the wave-absorbing powder.
Further, the invention provides a preparation method of the magnetic orientation arrangement wave-absorbing thermoplastic wire, which can also have the following characteristics: wherein the auxiliary agent consists of a plasticizer, a coupling agent, a toughening agent and a lubricant, and each auxiliary agent accounts for 20-50% of the total weight of the auxiliary agent; the plasticizer is one or more of glycerol, sebacic acid di (2-ethylhexyl) ester, phthalic acid di (2-ethyl) ester and adipic acid diethylene glycol ester; the coupling agent is one or more of phthalate ester coupling agent and silane coupling agent; the toughening agent is maleic anhydride grafted polymer; the lubricant is one or more of trihydroxy methyl propane, pentaerythritol stearate and liquid paraffin.
Further, the invention provides a preparation method of the magnetic orientation arrangement wave-absorbing thermoplastic wire, which can also have the following characteristics: the specific method for dissolving the thermoplastic resin in the first step comprises the following steps: according to parts by weight, dissolving 20-30 parts of thermoplastic resin by 60-70 parts of organic solvent at 40-200 ℃, stirring for 15min at the stirring speed of 150-400 rpm; the organic solvent is one or more of chloroform, formic acid, diphenyl sulfone and tetrahydrofuran.
Further, the invention provides a preparation method of the magnetic orientation arrangement wave-absorbing thermoplastic wire, which also has the following characteristics: wherein, in the third step, the specific method for washing comprises the following steps: adding the colloid mixture into deionized water, and stirring by using a glass rod while adding to obtain a viscous solution; standing the viscous solution for a period of time, precipitating, filtering, wrapping the precipitate with a filter screen, soaking in deionized water at room temperature for 24h, and changing water every 4 h;
the drying conditions were: dried overnight under vacuum at 70 ℃.
Further, the invention provides a preparation method of the magnetic orientation arrangement wave-absorbing thermoplastic wire, which can also have the following characteristics: in the fifth step, the temperature and the screw rotating speed of each zone in the double-screw extruder are as follows: the first is 150-180 ℃, the second is 160-230 ℃, the third is 160-280 ℃, the fourth is 170-290 ℃, the fifth is 200-300 ℃, the sixth is 200-330 ℃, the seventh is 200-350 ℃, and the screw rotation speed is 60-120r/min.
Further, the invention provides a preparation method of the magnetic orientation arrangement wave-absorbing thermoplastic wire, which can also have the following characteristics: in the fifth step, the magnetic flux of the external magnetic field is 0.15T-0.3T, and the direction of the magnetic field is parallel to the extrusion direction.
The invention also protects the magnetic orientation arrangement wave-absorbing thermoplastic wire prepared by the preparation method.
The invention has the beneficial effects that: the invention provides a magnetic orientation arrangement wave-absorbing thermoplastic wire material and a preparation method thereof, wherein wave-absorbing powder is uniformly dispersed by a low-temperature solution method of firstly dissolving thermoplastic resin and then dispersing wave-absorbing powder in the low-temperature solution in the first step and the second step and a high-temperature melting extrusion method in the fifth step through the two-step dispersion; in addition, the oriented arrangement of the magnetic wave-absorbing powder in the thermoplastic resin matrix is realized by means of an external magnetic field, so that the magnetic oriented arrangement wave-absorbing thermoplastic wire is prepared. The wave-absorbing performance test result and the mechanical performance test result show that compared with the wire without an external magnetic field, the magnetic thermoplastic wire prepared by the invention has greatly improved and optimized mechanical performance and magnetic loss capacity, the magnetic oriented thermoplastic wire can improve the magnetic conductivity of the material to the maximum extent and reduce the filling amount of magnetic powder, and the prepared composite material has low density and low cost, has good electromagnetic wave absorption performance, has wide application prospect in the novel composite material, and has important application value in the fields of communication, vehicle-mounted radar and national defense.
Drawings
FIG. 1 is a wave-absorbing property test result chart of each example and comparative example.
Detailed Description
The present invention is further illustrated by the following examples.
Example 1
The embodiment provides a magnetic orientation arrangement wave-absorbing thermoplastic wire, which comprises the following raw materials: 68 parts of thermoplastic resin, 25 parts of wave-absorbing powder and 7 parts of auxiliary agent. Wherein the thermoplastic resin is nylon 6 (PA 6); the wave-absorbing powder is a mixture of carbonyl iron and graphene, wherein the weight content of the carbonyl iron is 95%, and the weight content of the graphene is 5%; the auxiliary agent consists of a plasticizer, a coupling agent, a toughening agent and a lubricant, wherein the plasticizer is sebacic acid di (2-ethylhexyl) ester and accounts for 30% of the total content of the auxiliary agent, the coupling agent is a phthalate ester coupling agent and accounts for 20% of the total content of the auxiliary agent, the toughening agent is a maleic anhydride grafted polymer and accounts for 30% of the total content of the auxiliary agent, and the lubricant is liquid paraffin and accounts for 20% of the total content of the auxiliary agent.
The preparation method of the magnetic orientation arrangement wave-absorbing thermoplastic wire comprises the following steps:
step one, dissolving PA6 particles by using an analytically pure formic acid solution at 60 ℃ (the mass ratio of the formic acid solution to the PA6 is 70: 3), adjusting the rotating speed of a stirrer to be 150-400rpm, and reacting for 15min.
Step two, adding wave-absorbing powder after the dissolution is finished, dispersing the wave-absorbing powder by stirring, evaporating formic acid, and cooling to room temperature to form a colloidal mixture;
step three, adding the colloid mixture into deionized water, and stirring by using a glass rod while adding to obtain a viscous solution; standing the viscous solution for a period of time, precipitating, filtering, wrapping the precipitate with a filter screen, soaking in deionized water at room temperature for 24h, and changing water every 4h to remove the residual organic solvent;
drying the obtained precipitate in a vacuum oven at 70 ℃ overnight to obtain a thermoplastic wave-absorbing master batch;
step four, adding the thermoplastic wave-absorbing master batch and the auxiliary agent into a mixer, and mixing uniformly to obtain a mixed material;
step five, adding the mixed material into a double-screw extruder for wire drawing, and controlling the temperature and the screw rotation speed of each zone, wherein the first zone is 180 ℃, the second zone is 230 ℃, the third zone is 250 ℃, the fourth zone is 250 ℃, the fifth zone is 260 ℃, the sixth zone is 260 ℃, the seventh zone is 265 ℃ and the screw rotation speed is 60-120r/min;
applying an external magnetic field with the magnetic flux of 0.3T and the magnetic field direction parallel to the extrusion direction in front of a head of a double-screw extruder, drawing the wire, and finally curing to obtain the wave-absorbing thermoplastic wire in magnetic orientation arrangement.
Example 2
The embodiment provides a magnetic orientation arrangement wave-absorbing thermoplastic wire, which comprises the following raw materials: 68 parts of thermoplastic resin, 25 parts of wave-absorbing powder and 7 parts of auxiliary agent. Wherein the thermoplastic resin is polyvinyl chloride; the wave-absorbing powder is a mixture of carbonyl iron and graphene, wherein the weight content of the carbonyl iron is 93%, and the weight content of the graphene is 7%; the auxiliary agent consists of a plasticizer, a coupling agent, a toughening agent and a lubricant, wherein the plasticizer is glycerol and accounts for 20% of the total content of the auxiliary agent, the coupling agent is a silane coupling agent and accounts for 25% of the total content of the auxiliary agent, the toughening agent is a maleic anhydride grafted polymer and accounts for 30% of the total content of the auxiliary agent, and the lubricant is trihydroxy methyl propane and accounts for 25% of the total content of the auxiliary agent.
The preparation method of the magnetic orientation arrangement wave-absorbing thermoplastic wire comprises the following steps:
step one, dissolving polyvinyl chloride particles by using tetrahydrofuran at 40 ℃ (the mass ratio of the tetrahydrofuran to the polyvinyl chloride is 70: 3), adjusting the rotating speed of a stirrer to be 150-400rpm, and reacting for 15min.
Step two, adding wave-absorbing powder after the dissolution is finished, dispersing the wave-absorbing powder by stirring, evaporating formic acid, and cooling to room temperature to form a colloidal mixture;
adding the colloid mixture into deionized water, and stirring by using a glass rod while adding to obtain a viscous solution; standing the viscous solution for a period of time, precipitating, filtering, wrapping the precipitate with a filter screen, soaking in deionized water at room temperature for 24h, and changing water every 4h to remove the residual organic solvent;
drying the obtained precipitate in a vacuum oven at 70 ℃ overnight to obtain a thermoplastic wave-absorbing master batch;
step four, adding the thermoplastic wave-absorbing master batch and the auxiliary agent into a mixer, and mixing uniformly to obtain a mixed material;
step five, adding the mixed material into a double-screw extruder for wire drawing, and controlling the temperature and the screw rotation speed of each zone, wherein the first zone is 180 ℃, the second zone is 230 ℃, the third zone is 250 ℃, the fourth zone is 250 ℃, the fifth zone is 260 ℃, the sixth zone is 260 ℃, the seventh zone is 265 ℃ and the screw rotation speed is 60-120r/min;
applying an external magnetic field with the magnetic flux of 0.3T and the direction of the magnetic field parallel to the extrusion direction in front of a machine head of the double-screw extruder, drawing the wire material, and finally solidifying to obtain the wave-absorbing thermoplastic wire material in magnetic orientation arrangement.
Example 3
The embodiment provides a magnetic orientation arrangement wave-absorbing thermoplastic wire, which comprises the following raw materials: 70 parts of thermoplastic resin, 25 parts of wave-absorbing powder and 5 parts of auxiliary agent. Wherein the thermoplastic resin is polyether-ether-ketone; the wave-absorbing powder is a mixture of carbonyl iron and graphene, wherein the weight content of the carbonyl iron is 95%, and the weight content of the graphene is 5%; the auxiliary agent consists of a plasticizer, a coupling agent, a toughening agent and a lubricant, wherein the plasticizer is phthalic acid di (2-ethyl) ester and accounts for 30% of the total content of the auxiliary agent, the coupling agent is a phthalate ester coupling agent and accounts for 25% of the total content of the auxiliary agent, the toughening agent is a maleic anhydride grafted polymer and accounts for 20% of the total content of the auxiliary agent, and the lubricant is trihydroxy methyl propane and accounts for 25% of the total content of the auxiliary agent.
The preparation method of the magnetic orientation arrangement wave-absorbing thermoplastic wire comprises the following steps:
step one, dissolving polyether-ether-ketone particles by diphenyl sulfone at 200 ℃ (the mass ratio of diphenyl sulfone to polyether-ether-ketone is 70: 3), adjusting the rotating speed of a stirrer to be 150-400rpm, and reacting for 15min.
Step two, adding wave-absorbing powder after the dissolution is finished, dispersing the wave-absorbing powder by stirring, evaporating formic acid, and cooling to room temperature to form a colloidal mixture;
step three, adding the colloid mixture into deionized water, and stirring by using a glass rod while adding to obtain a viscous solution; standing the viscous solution for a period of time, precipitating, filtering, wrapping the precipitate with a filter screen, soaking in deionized water at room temperature for 24h, and changing water every 4h to remove the residual organic solvent;
drying the obtained precipitate in a vacuum oven at 70 ℃ overnight to obtain a thermoplastic wave-absorbing master batch;
step four, adding the thermoplastic wave-absorbing master batch and the auxiliary agent into a mixer, and mixing uniformly to obtain a mixed material;
step five, adding the mixed material into a double-screw extruder for wire drawing, and controlling the temperature and the screw rotation speed of each zone, wherein the first zone is 180 ℃, the second zone is 230 ℃, the third zone is 250 ℃, the fourth zone is 250 ℃, the fifth zone is 260 ℃, the sixth zone is 260 ℃, the seventh zone is 265 ℃ and the screw rotation speed is 60-120r/min;
applying an external magnetic field with the magnetic flux of 0.3T and the direction of the magnetic field parallel to the extrusion direction in front of a machine head of the double-screw extruder, drawing the wire material, and finally solidifying to obtain the wave-absorbing thermoplastic wire material in magnetic orientation arrangement.
Comparative example 1
The composition and the preparation method of the magnetic orientation arrangement wave-absorbing thermoplastic wire are basically the same as those of the embodiment 1, and the difference is that: in step five of the preparation method, an external magnetic field is not applied in front of the head of the twin-screw extruder.
Comparative example 2
The composition and the preparation method of the magnetic orientation arrangement wave-absorbing thermoplastic wire are basically the same as those of the embodiment 1, and the difference is that: no wave-absorbing powder is added.
And (3) performance testing:
the wires prepared in the examples 1-3 and the comparative examples 1-2 are laid in layers according to a designed structure, and are uniformly arranged, and then the wires are cured at normal temperature by taking epoxy resin as an adhesive to prepare the wave-absorbing resin composite board. And testing the reflectivity of the flat plate by using an arch method in the wave-absorbing darkroom and testing the mechanical property of the obtained composite plate. The results of the wave absorption test are shown in FIG. 1, and the results of the mechanical properties test are shown in Table 1.
TABLE 1 mechanical Properties of examples 1-3 and comparative examples 1-2
Performance index Example 1 Example 2 Example 3 Comparative example 1 Comparative example 2
Tensile strength/Mpa 100 98 200 70 90
Modulus of elasticity/MPa 2785 2505 3660 2180 2000
Impact strength kJ/m 2 8.7 7.4 19.7 4.9 5.7
As shown in figure 1, through the test of a vector network analyzer, it can be seen that compared with the wire without applied external magnetic field, the real part and the imaginary part of the magnetic conductivity of the thermoplastic wire in magnetic orientation arrangement are greatly improved, which shows the effective action of the external magnetic field, and the external magnetic field realizes the magnetic orientation arrangement of the wave-absorbing component.
The invention provides a preparation method of a thermoplastic wire with magnetic orientation arrangement, which uniformly disperses wave-absorbing powder by a two-step dispersion method of a low-temperature solution method and a high-temperature melt extrusion method, and realizes the orientation arrangement of the magnetic wave-absorbing powder in a thermoplastic resin matrix by means of an external magnetic field. The thermoplastic wire with the directionally arranged magnetic particles prepared by the preparation method provided by the invention has improved mechanical properties and wave-absorbing efficiency, and has important practical significance in the application of wave-absorbing materials in the future.

Claims (7)

1. A preparation method of magnetic orientation arrangement wave-absorbing thermoplastic wire is characterized by comprising the following steps:
the method comprises the following steps:
firstly, dissolving thermoplastic resin by using an organic solvent;
step two, adding wave-absorbing powder into the dissolved thermoplastic resin, stirring and dispersing, and evaporating the organic solvent to obtain a colloid mixture; the wave-absorbing powder is a mixture of carbonyl iron and graphene, and each wave-absorbing powder accounts for 5-95% of the total weight of the wave-absorbing powder;
washing the colloid mixture, removing the residual organic solvent, and drying to obtain a thermoplastic wave-absorbing master batch;
step four, mixing the thermoplastic wave-absorbing master batch with an auxiliary agent to obtain a mixed material;
fifthly, adding the mixed material into a double-screw extruder for drawing, applying an external magnetic field in front of a machine head of the double-screw extruder, drawing the wire material, and finally solidifying to obtain the wave-absorbing thermoplastic wire material in magnetic orientation arrangement; the magnetic flux of the external magnetic field is 0.15T-0.3T, and the direction of the magnetic field is parallel to the extrusion direction;
the composite material comprises the following raw materials in parts by weight: 60-70 parts of thermoplastic resin, 25-30 parts of wave-absorbing powder and 5-10 parts of auxiliary agent.
2. The preparation method of the magnetic orientation arrangement wave-absorbing thermoplastic wire material according to claim 1, characterized in that:
wherein the thermoplastic resin is one or more of polyether-ether-ketone, polyvinyl chloride, nylon 6, nylon 66 and polylactic acid.
3. The preparation method of the magnetic orientation arrangement wave-absorbing thermoplastic wire material according to claim 1, characterized in that:
the auxiliary agent comprises a plasticizer, a coupling agent, a toughening agent and a lubricating agent, wherein each auxiliary agent accounts for 20-50% of the total weight of the auxiliary agent;
the plasticizer is one or more of glycerol, sebacic acid di (2-ethylhexyl) ester, phthalic acid di (2-ethyl) ester and adipic acid diethylene glycol ester; the coupling agent is one or more of phthalate ester coupling agent and silane coupling agent; the toughening agent is maleic anhydride grafted polymer; the lubricant is one or more of trimethylolpropane, pentaerythritol stearate and liquid paraffin.
4. The preparation method of the magnetic orientation arrangement wave-absorbing thermoplastic wire material according to claim 1, characterized by comprising the following steps:
the specific method for dissolving the thermoplastic resin in the first step comprises the following steps: dissolving 20 to 30 parts by weight of thermoplastic resin in 60 to 70 parts by weight of organic solvent at 40 to 200 ℃, stirring at the rotating speed of 150 to 400rpm, and stirring for 15min;
the organic solvent is one or more of chloroform, formic acid, diphenyl sulfone and tetrahydrofuran.
5. The preparation method of the magnetic orientation arrangement wave-absorbing thermoplastic wire material according to claim 1, characterized in that:
wherein, in the third step, the specific method for washing comprises the following steps: adding the colloid mixture into deionized water, and stirring while adding to obtain a viscous solution; standing the viscous solution, precipitating, filtering, wrapping the precipitate with a filter screen, soaking in deionized water at room temperature for 24 hr, and changing water every 4 hr;
the drying conditions were: dried overnight under vacuum at 70 ℃.
6. The preparation method of the magnetic orientation arrangement wave-absorbing thermoplastic wire material according to claim 1, characterized in that:
in the fifth step, the temperature and the screw rotating speed of each zone in the double-screw extruder are as follows: the first zone is 150-180 ℃, the second zone is 160-230 ℃, the third zone is 160-280 ℃, the fourth zone is 170-290 ℃, the fifth zone is 200-300 ℃, the sixth zone is 200-330 ℃, the seventh zone is 200-350 ℃, and the screw rotation speed is 60-120r/min.
7. The magnetically-aligned wave-absorbing thermoplastic wire prepared by the preparation method of any one of claims 1 to 6.
CN202210514983.5A 2022-05-12 2022-05-12 Magnetic orientation arrangement wave-absorbing thermoplastic wire and preparation method thereof Active CN114750441B (en)

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CN113088065A (en) * 2021-04-06 2021-07-09 常州昊天新材料科技有限公司 Modified film type wave-absorbing material and preparation method thereof

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CN102666686A (en) * 2009-10-07 2012-09-12 波利玛利欧洲股份公司 Expandable thermoplastic nanocomposite polymeric compositions with an improved thermal insulation capacity
CN110615977A (en) * 2019-09-16 2019-12-27 南京林业大学 Multifunctional polylactic acid composite material and preparation method thereof
CN110835466A (en) * 2019-10-23 2020-02-25 上海太朔材料技术有限公司 Inductor packaging powder based on thermoplastic high polymer material and production process thereof
CN113088065A (en) * 2021-04-06 2021-07-09 常州昊天新材料科技有限公司 Modified film type wave-absorbing material and preparation method thereof

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