CN114479435A - Preparation method of electromagnetic shielding magnetic-conducting polymer alloy and product thereof - Google Patents

Preparation method of electromagnetic shielding magnetic-conducting polymer alloy and product thereof Download PDF

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CN114479435A
CN114479435A CN202111646248.1A CN202111646248A CN114479435A CN 114479435 A CN114479435 A CN 114479435A CN 202111646248 A CN202111646248 A CN 202111646248A CN 114479435 A CN114479435 A CN 114479435A
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electromagnetic shielding
polymer alloy
manganese
shielding magnetic
nickel
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王俊龙
郑大权
陈艳丽
喻文斌
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Kunshan Keyun New Engineering Material Technology Co ltd
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    • H05K9/00Screening of apparatus or components against electric or magnetic fields
    • H05K9/0073Shielding materials
    • H05K9/0081Electromagnetic shielding materials, e.g. EMI, RFI shielding
    • H05K9/0083Electromagnetic shielding materials, e.g. EMI, RFI shielding comprising electro-conductive non-fibrous particles embedded in an electrically insulating supporting structure, e.g. powder, flakes, whiskers

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Abstract

The invention discloses a preparation method of an electromagnetic shielding and magnetic conducting polymer alloy and a product thereof, wherein the resin base material selects one or more of PPA, PP, PE and PET as a matrix polymer resin raw material; doping ferrite by adopting manganese/nickel elements through a hydrothermal synthesis method, and preparing nano powder through high-temperature sintering; mixing the electromagnetic shielding magnetic powder with a surface modifier in a high-speed kneading mode to prepare a reinforced modified material; and compounding the reinforced modified material and the resin powder, mixing by a premixer, and extruding by a double screw to obtain the electromagnetic shielding magnetic conductive high polymer material. The electromagnetic shielding magnetic conductive nano material can improve the binding force and the dispersity with a matrix resin material after being subjected to surface modification by a silicon surfactant, is favorable for improving the electromagnetic shielding performance of a high-molecular alloy material, and has the effects of obviously enhancing the mechanical property and reducing the cost due to the fact that the nano material has the function of enhancing and toughening.

Description

Preparation method of electromagnetic shielding magnetic-conducting polymer alloy and product thereof
Technical Field
The invention belongs to the technical field of high-performance polymer alloy materials, and particularly relates to a preparation method of an electromagnetic shielding and magnetic conducting polymer alloy and a product thereof.
Background
With the rapid development of the global industrialization process, people can fully enjoy the convenience and happiness of the modernization in the aspects of work, study, traffic, communication and the like, and simultaneously silently bear the negative effects of excessive electromagnetic radiation on human bodies and the environment. Electromagnetic radiation is a substance with a special form, and refers to a phenomenon that after electromagnetic energy is separated from a field source, the electromagnetic energy is transmitted to a far distance in the form of electromagnetic waves and does not return to the field source any more. Electromagnetic radiation has the characteristics of wide frequency band, large information amount, strong resolution and the like, and is widely applied to industries such as radar, communication, medical treatment and health care at present.
However, the excessive electromagnetic radiation also causes electromagnetic pollution, such as various electronic and electrical devices used in daily life and industrial production processes of people, and also includes signal transmission systems and communication, high-voltage transmission lines and the like.
The prior art product is mainly shielded by a metal material, and the mechanism of the prior art product is that a cage effect is formed by the conversion of an electromagnetic field to protect objects in the material.
Disclosure of Invention
This section is for the purpose of summarizing some aspects of embodiments of the invention and to briefly introduce some preferred embodiments. In this section, as well as in the abstract and the title of the invention of this application, simplifications or omissions may be made to avoid obscuring the purpose of the section, the abstract and the title, and such simplifications or omissions are not intended to limit the scope of the invention.
The present invention has been made keeping in mind the above and/or other problems occurring in the prior art.
Therefore, the present invention aims to overcome the defects in the prior art and provide a preparation method of an electromagnetic shielding magnetic conductive polymer alloy.
In order to solve the technical problems, the invention provides the following technical scheme: a method for preparing electromagnetic shielding magnetic conductive polymer alloy comprises,
selection of resin base material: one or more of PPA, PP, PE and PET is/are selected as a matrix polymer resin raw material for the resin base material;
preparing an electromagnetic shielding magnetic material: doping ferrite by adopting manganese/nickel elements through a hydrothermal synthesis method, and preparing nano powder through high-temperature sintering;
carrying out surface modification on the electromagnetic shielding magnetic material: mixing the electromagnetic shielding magnetic powder with a surface modifier in a high-speed kneading mode to prepare a reinforced modified material;
preparing electromagnetic shielding magnetic polymer alloy: and compounding the reinforced modified material and the resin powder, mixing by a premixer, and extruding by a double screw to obtain the electromagnetic shielding magnetic conductive high polymer material.
As a preferred scheme of the preparation method of the electromagnetic shielding and magnetic conducting polymer alloy, the method comprises the following steps: the particle size of the matrix polymer resin is 100-500 meshes.
As a preferred scheme of the preparation method of the electromagnetic shielding and magnetic conducting polymer alloy, the method comprises the following steps: the mass percentage of the resin base material in the electromagnetic shielding magnetic conductive polymer alloy is 50-90%.
As a preferred scheme of the preparation method of the electromagnetic shielding and magnetic conducting polymer alloy, the method comprises the following steps: the electromagnetic shielding magnetic material is prepared by doping ferrite with manganese/nickel elements, wherein the manganese and the nickel adopt soluble salts, the ferrite is prepared by reacting soluble ferrous/ferric iron with alkali, and the doping amount of the manganese and the nickel elements is 0.1-3%.
As a preferred scheme of the preparation method of the electromagnetic shielding and magnetic conducting polymer alloy, the method comprises the following steps: the preparation method of the electromagnetic shielding magnetic material comprises the steps of adopting a hydrothermal synthesis method, enabling the synthesis temperature to be 100-220 ℃, enabling the reaction time to be 2-8 hours, enabling the pH value during the reaction to be 4-8, filtering the prepared powder, and sintering at 300-500 ℃ to obtain the manganese/nickel doped ferrite nano material.
As a preferred scheme of the preparation method of the electromagnetic shielding and magnetic conducting polymer alloy, the method comprises the following steps: the electromagnetic shielding magnetic polymer alloy comprises a manganese/nickel doped ferrite nano material, wherein the addition amount of the manganese/nickel doped ferrite nano material is 10-50%.
As a preferred scheme of the preparation method of the electromagnetic shielding and magnetic conducting polymer alloy, the method comprises the following steps: the electromagnetic shielding magnetic material is subjected to surface modification, and is dispersed at normal temperature in a high-speed kneading mode, wherein the rotating speed is 2000-5000 r/min.
As a preferred scheme of the preparation method of the electromagnetic shielding and magnetic conducting polymer alloy, the method comprises the following steps: the surface modifier comprises methyl silicone oil, polydimethylsiloxane and polycyclomethyl siloxane, and the dosage of the surface modifier is 0.1-3% of the mass of the electromagnetic shielding magnetic conducting material.
As a preferred scheme of the preparation method of the electromagnetic shielding and magnetic conducting polymer alloy, the method comprises the following steps: the preparation of the electromagnetic shielding magnetic conductive polymer alloy comprises the following steps,
mixing the electromagnetic shielding and magnetic conductive nano material and resin powder through a premixer, and performing blending extrusion granulation through a double-screw extruder to prepare the electromagnetic shielding and magnetic conductive nano material; the mixing speed of the premixer is 200-600r/min, the working temperature is normal temperature, the double-screw extrusion processing temperature is 160-300 ℃, the working efficiency is 1-10 MHZ, and the electromagnetic shielding and magnetic conducting polymer alloy material is obtained through extrusion by a machine head, water cooling, short cutting and drying.
The invention also aims to overcome the defects in the prior art and provide a product prepared by the preparation method of the electromagnetic shielding magnetic conductive polymer alloy
The invention has the beneficial effects that:
the electromagnetic shielding magnetic conductive nano material can improve the binding force and the dispersibility with a matrix resin material after being subjected to surface modification by a silicon surfactant, is favorable for improving the electromagnetic shielding performance of a high-molecular alloy material, and can generate an obvious effect of enhancing the mechanical performance, improve the added value of products and reduce the cost because the nano material has the function of enhancing and toughening.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings needed to be used in the description of the embodiments will be briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings based on these drawings without inventive exercise. Wherein:
FIG. 1 is a diagram showing the dispersion of a powder in a resin measured by a casting method in example 19 of the present invention.
Detailed Description
In order to make the aforementioned objects, features and advantages of the present invention more comprehensible, specific embodiments thereof are described in detail below with reference to examples of the specification.
In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present invention, but the present invention may be practiced in other ways than those specifically described and will be readily apparent to those of ordinary skill in the art without departing from the spirit of the present invention, and therefore the present invention is not limited to the specific embodiments disclosed below.
Furthermore, reference herein to "one embodiment" or "an embodiment" means that a particular feature, structure, or characteristic described in connection with the embodiment is included in at least one implementation of the invention. The appearances of the phrase "in one embodiment" in various places in the specification are not necessarily all referring to the same embodiment, nor are separate or alternative embodiments mutually exclusive of other embodiments.
Example 1:
selection of resin base material: PPA powder (high temperature resistant nylon) is selected as a matrix polymer resin raw material of the resin base material, and the content is 90%;
the electromagnetic shielding nano material is manganese/nickel doped ferrite, and is prepared by synthesizing through a hydrothermal method, wherein the reaction temperature is 100 ℃, the reaction time is 2 hours, the reaction pH value is 4, the manganese and nickel doping amount is 0.1%, and nano powder is prepared by firing at 300 ℃, wherein the raw material is ferric chloride, the pH value is adjusted through ammonia water, and manganese and nickel are chlorides, specifically manganese chloride and nickel chloride;
performing surface modification on the electromagnetic shielding nano material, selecting polydimethylsiloxane as a surface modifier, wherein the using amount of the polydimethylsiloxane is 0.5 percent of that of the nano powder, performing surface modification through high-speed kneading equipment at the rotating speed of 3500r/min at room temperature;
preparing electromagnetic shielding magnetic polymer alloy: mixing the electromagnetic shielding and magnetic conducting nano material and resin powder at the normal temperature of a pre-mixer at the rotating speed of 200-600r/min and the addition of the electromagnetic shielding and magnetic conducting material of 10 percent, carrying out blending extrusion granulation by a double-screw extruder at the processing temperature of 285 ℃ and the working efficiency of 6MHZ, and carrying out extrusion, water cooling, short cutting and drying by a machine head to obtain the electromagnetic shielding and magnetic conducting polymer alloy material.
The mechanical strength is increased by 5% according to GB/T1843-2008 detection, the toughness is increased by 2% according to GB/T1451-.
Example 2:
selection of resin base material: PPA powder (high temperature resistant nylon) is selected as a matrix polymer resin raw material of the resin base material, and the content is 90%;
the electromagnetic shielding nano material is manganese/nickel doped ferrite, is synthesized and prepared by a hydrothermal method, the reaction temperature is 140 ℃, the reaction time is 2 hours, the reaction pH value is 4, the manganese and nickel doping amount is 0.1%, and the nano powder is prepared by firing at 300 ℃, wherein the raw material is ferric chloride, the pH value is adjusted by ammonia water, and manganese and nickel are chlorides, specifically manganese chloride and nickel chloride;
performing surface modification on the electromagnetic shielding nano material, selecting polydimethylsiloxane as a surface modifier, wherein the using amount of the polydimethylsiloxane is 0.5 percent of that of the nano powder, performing surface modification through high-speed kneading equipment at the rotating speed of 3500r/min at room temperature;
preparing electromagnetic shielding magnetic polymer alloy: mixing the electromagnetic shielding and magnetic conducting nano material and resin powder at the normal temperature of a pre-mixer at the rotating speed of 200-600r/min and the addition of the electromagnetic shielding and magnetic conducting material of 10 percent, carrying out blending extrusion granulation by a double-screw extruder at the processing temperature of 285 ℃ and the working efficiency of 6MHZ, and carrying out extrusion, water cooling, short cutting and drying by a machine head to obtain the electromagnetic shielding and magnetic conducting polymer alloy material.
The mechanical strength is increased by 7% according to GB/T1843-2008 detection, the toughness is increased by 3% according to GB/T1451-.
Example 3:
selection of resin base material: PPA powder (high temperature resistant nylon) is selected as a matrix polymer resin raw material of the resin base material, and the content is 90%; the electromagnetic shielding nano material is manganese/nickel doped ferrite, is synthesized and prepared by a hydrothermal method, the reaction temperature is 180 ℃, the reaction time is 2 hours, the reaction pH value is 4, the manganese and nickel doping amount is 0.1%, and the nano powder is prepared by firing at 300 ℃, wherein the raw material is ferric chloride, the pH value is adjusted by ammonia water, and manganese and nickel are chlorides, specifically manganese chloride and nickel chloride;
performing surface modification on the electromagnetic shielding nano material, selecting polydimethylsiloxane as a surface modifier, wherein the usage amount of the polydimethylsiloxane is 0.5 percent of that of the nano powder, performing surface modification through high-speed kneading equipment at the rotating speed of 3500r/min at room temperature;
preparing electromagnetic shielding magnetic polymer alloy: mixing the electromagnetic shielding and magnetic conducting nano material and resin powder at the normal temperature of a pre-mixer at the rotating speed of 200-600r/min and the addition of the electromagnetic shielding and magnetic conducting material of 10 percent, carrying out blending extrusion granulation by a double-screw extruder at the processing temperature of 285 ℃ and the working efficiency of 6MHZ, and carrying out extrusion, water cooling, short cutting and drying by a machine head to obtain the electromagnetic shielding and magnetic conducting polymer alloy material.
The mechanical strength is increased by 7% according to GB/T1843-2008 detection, the toughness is increased by 4% according to GB/T1451-.
Example 4:
selection of resin base material: PPA powder (high temperature resistant nylon) is selected as a matrix polymer resin raw material of the resin base material, and the content is 90%; the electromagnetic shielding nano material is manganese/nickel doped ferrite, and is prepared by synthesizing through a hydrothermal method, wherein the reaction temperature is 200 ℃, the reaction time is 2 hours, the reaction pH value is 4, the manganese and nickel doping amount is 0.1%, and nano powder is prepared by firing at 300 ℃, wherein the raw material is ferric chloride, the pH value is adjusted through ammonia water, and manganese and nickel are chlorides, specifically manganese chloride and nickel chloride;
performing surface modification on the electromagnetic shielding nano material, selecting polydimethylsiloxane as a surface modifier, wherein the using amount of the polydimethylsiloxane is 0.5 percent of that of the nano powder, performing surface modification through high-speed kneading equipment at the rotating speed of 3500r/min at room temperature;
preparing electromagnetic shielding magnetic polymer alloy: mixing the electromagnetic shielding and magnetic conducting nano material and resin powder at the normal temperature of a pre-mixer at the rotating speed of 200-600r/min and the addition of the electromagnetic shielding and magnetic conducting material of 10 percent, carrying out blending extrusion granulation by a double-screw extruder at the processing temperature of 285 ℃ and the working efficiency of 6MHZ, and carrying out extrusion, water cooling, short cutting and drying by a machine head to obtain the electromagnetic shielding and magnetic conducting polymer alloy material. The mechanical strength is increased by 5 percent according to GB/T1843-2008 detection, the toughness is increased by 3 percent according to GB/T1451-
And (3) detecting the electromagnetic shielding performance, wherein the 30 MHz-230 MHz shielding performance is 31%, the 230 MHz-1 GHz shielding performance is 29%, and the 1 GHz-18 GHz shielding performance is 24%.
When the reaction temperature is further increased, the shielding effect is deteriorated because the reaction speed is too slow or even incomplete when the temperature is too low, which is disadvantageous to the formation of the nanomaterial, and when the temperature is too high, the reaction is too violent, which is not uniform in the structure of the nanomaterial, and thus the reaction temperature is preferably 180 ℃.
Example 5:
selection of resin base material: PPA powder (high temperature resistant nylon) is selected as a matrix polymer resin raw material of the resin base material, and the content is 90%;
the electromagnetic shielding nano material is manganese/nickel doped ferrite, is synthesized and prepared by a hydrothermal method, the reaction temperature is 180 ℃, the reaction time is 4 hours, the reaction pH value is 4, the manganese and nickel doping amount is 0.1%, and the nano powder is prepared by firing at 300 ℃, wherein the raw material is ferric chloride, the pH value is adjusted by ammonia water, and manganese and nickel are chlorides, specifically manganese chloride and nickel chloride;
performing surface modification on the electromagnetic shielding nano material, selecting polydimethylsiloxane as a surface modifier, wherein the using amount of the polydimethylsiloxane is 0.5 percent of that of the nano powder, performing surface modification through high-speed kneading equipment at the rotating speed of 3500r/min at room temperature;
preparing electromagnetic shielding magnetic polymer alloy: mixing the electromagnetic shielding and magnetic conducting nano material and resin powder at the normal temperature of a pre-mixer at the rotating speed of 200-600r/min and the addition of the electromagnetic shielding and magnetic conducting material of 10 percent, carrying out blending extrusion granulation by a double-screw extruder at the processing temperature of 285 ℃ and the working efficiency of 6MHZ, and carrying out extrusion, water cooling, short cutting and drying by a machine head to obtain the electromagnetic shielding and magnetic conducting polymer alloy material.
The mechanical strength is increased by 8 percent according to GB/T1843-2008 detection, the toughness is increased by 4 percent according to GB/T1451-
And (3) detecting the electromagnetic shielding performance, wherein the 30 MHz-230 MHz shielding performance is 33%, the 230 MHz-1 GHz shielding performance is 33%, and the 1 GHz-18 GHz shielding performance is 28%.
Example 6:
selection of resin base material: PPA powder (high temperature resistant nylon) is selected as a matrix polymer resin raw material of the resin base material, and the content is 90%;
the electromagnetic shielding nano material is manganese/nickel doped ferrite, is synthesized and prepared by a hydrothermal method, the reaction temperature is 180 ℃, the reaction time is 6 hours, the reaction pH value is 4, the manganese and nickel doping amount is 0.1%, and the nano powder is prepared by firing at 300 ℃, wherein the raw material is ferric chloride, the pH value is adjusted by ammonia water, and manganese and nickel are chlorides, specifically manganese chloride and nickel chloride;
performing surface modification on the electromagnetic shielding nano material, selecting polydimethylsiloxane as a surface modifier, wherein the using amount of the polydimethylsiloxane is 0.5 percent of that of the nano powder, performing surface modification through high-speed kneading equipment at the rotating speed of 3500r/min at room temperature;
preparing electromagnetic shielding magnetic polymer alloy: mixing the electromagnetic shielding and magnetic conducting nano material and resin powder at normal temperature by a pre-mixer at the rotating speed of 200-600r/min and the adding amount of the electromagnetic shielding and magnetic conducting material of 10 percent, extruding and granulating by a double-screw extruder at the processing temperature of 285 ℃ and the working efficiency of 6MHZ, and extruding by a machine head, water cooling, chopping and drying to obtain the electromagnetic shielding and magnetic conducting polymer alloy material.
The mechanical strength is increased by 7% according to GB/T1843-2008 detection, the toughness is increased by 3% according to GB/T1451-.
The nano material will aggregate when the reaction time is continuously increased, which is not beneficial to the improvement of performance, so the reaction time is optimal when 4 h.
Example 7:
selection of resin base material: PPA powder (high temperature resistant nylon) is selected as a matrix polymer resin raw material of the resin base material, and the content is 90%;
the electromagnetic shielding nano material is manganese/nickel doped ferrite, is synthesized and prepared by a hydrothermal method, the reaction temperature is 180 ℃, the reaction time is 4 hours, the reaction pH value is 5, the manganese and nickel doping amount is 0.1%, and the nano powder is prepared by firing at 300 ℃, wherein the raw material is ferric chloride, the pH value is adjusted by ammonia water, and manganese and nickel are chlorides, specifically manganese chloride and nickel chloride;
performing surface modification on the electromagnetic shielding nano material, selecting polydimethylsiloxane as a surface modifier, wherein the using amount of the polydimethylsiloxane is 0.5 percent of that of the nano powder, performing surface modification through high-speed kneading equipment at the rotating speed of 3500r/min at room temperature; preparing electromagnetic shielding magnetic polymer alloy: mixing the electromagnetic shielding and magnetic conducting nano material and resin powder at the normal temperature of a pre-mixer at the rotating speed of 200-600r/min and the addition of the electromagnetic shielding and magnetic conducting material of 10 percent, carrying out blending extrusion granulation by a double-screw extruder at the processing temperature of 285 ℃ and the working efficiency of 6MHZ, and carrying out extrusion, water cooling, short cutting and drying by a machine head to obtain the electromagnetic shielding and magnetic conducting polymer alloy material.
The mechanical strength is increased by 9 percent according to GB/T1843-2008 detection, the toughness is increased by 4 percent according to GB/T1451-
And (3) detecting the electromagnetic shielding performance, wherein the 30 MHz-230 MHz shielding performance is 34%, the 230 MHz-1 GHz shielding performance is 35%, and the 1 GHz-18 GHz shielding performance is 30%.
Example 8:
selection of resin base material: PPA powder (high temperature resistant nylon) is selected as a matrix polymer resin raw material for the resin base material, and the content is 90%;
the electromagnetic shielding nano material is manganese/nickel doped ferrite, is synthesized and prepared by a hydrothermal method, the reaction temperature is 180 ℃, the reaction time is 4 hours, the reaction pH value is 6, the manganese and nickel doping amount is 0.1%, and the nano powder is prepared by firing at 300 ℃, wherein the raw material is ferric chloride, the pH value is adjusted by ammonia water, and manganese and nickel are chlorides, specifically manganese chloride and nickel chloride;
performing surface modification on the electromagnetic shielding nano material, selecting polydimethylsiloxane as a surface modifier, wherein the using amount of the polydimethylsiloxane is 0.5 percent of that of the nano powder, performing surface modification through high-speed kneading equipment at the rotating speed of 3500r/min at room temperature; preparing electromagnetic shielding magnetic polymer alloy: mixing the electromagnetic shielding and magnetic conducting nano material and resin powder at normal temperature by a pre-mixer at the rotating speed of 200-600r/min and the adding amount of the electromagnetic shielding and magnetic conducting material of 10 percent, extruding and granulating by a double-screw extruder at the processing temperature of 285 ℃ and the working efficiency of 6MHZ, and extruding by a machine head, water cooling, chopping and drying to obtain the electromagnetic shielding and magnetic conducting polymer alloy material. The mechanical strength is increased by 9 percent according to GB/T1843-2008 detection, the toughness is increased by 5 percent according to GB/T1451-
And (3) detecting the electromagnetic shielding performance, wherein the 30 MHz-230 MHz shielding performance is 36%, the 230 MHz-1 GHz shielding performance is 36%, and the 1 GHz-18 GHz shielding performance is 32%.
Example 9:
selection of resin base material: PPA powder (high temperature resistant nylon) is selected as a matrix polymer resin raw material of the resin base material, and the content is 90%;
the electromagnetic shielding nano material is manganese/nickel doped ferrite, is synthesized and prepared by a hydrothermal method, the reaction temperature is 180 ℃, the reaction time is 4 hours, the reaction pH value is 7, the manganese and nickel doping amount is 0.1%, and the nano powder is prepared by firing at 300 ℃, wherein the raw material is ferric chloride, the pH value is adjusted by ammonia water, and manganese and nickel are chlorides, specifically manganese chloride and nickel chloride;
performing surface modification on the electromagnetic shielding nano material, selecting polydimethylsiloxane as a surface modifier, wherein the using amount of the polydimethylsiloxane is 0.5 percent of that of the nano powder, performing surface modification through high-speed kneading equipment at the rotating speed of 3500r/min at room temperature;
preparing electromagnetic shielding magnetic polymer alloy: mixing the electromagnetic shielding and magnetic conducting nano material and resin powder at the normal temperature of a pre-mixer at the rotating speed of 200-600r/min and the addition of the electromagnetic shielding and magnetic conducting material of 10 percent, carrying out blending extrusion granulation by a double-screw extruder at the processing temperature of 285 ℃ and the working efficiency of 6MHZ, and carrying out extrusion, water cooling, short cutting and drying by a machine head to obtain the electromagnetic shielding and magnetic conducting polymer alloy material.
The mechanical strength is increased by 7% according to GB/T1843-2008 detection, the toughness is increased by 3% according to GB/T1451-.
The reaction pH is increased further, at which time significant sedimentation occurs, so that nanoparticles are not uniformly generated, resulting in a decrease in performance, and the optimum reaction pH is 6.
Example 10:
selection of resin base material: PPA powder (high temperature resistant nylon) is selected as a matrix polymer resin raw material of the resin base material, and the content is 90%;
the electromagnetic shielding nano material is manganese/nickel doped ferrite, is synthesized and prepared by a hydrothermal method, the reaction temperature is 180 ℃, the reaction time is 4 hours, the reaction pH value is 6, the manganese and nickel doping amount is 0.4%, and the nano powder is prepared by firing at 300 ℃, wherein the raw material is ferric chloride, the pH value is adjusted by ammonia water, and manganese and nickel are chlorides, specifically manganese chloride and nickel chloride;
performing surface modification on the electromagnetic shielding nano material, selecting polydimethylsiloxane as a surface modifier, wherein the using amount of the polydimethylsiloxane is 0.5 percent of that of the nano powder, performing surface modification through high-speed kneading equipment at the rotating speed of 3500r/min at room temperature; preparing electromagnetic shielding magnetic polymer alloy: mixing the electromagnetic shielding and magnetic conducting nano material and resin powder at the normal temperature of a pre-mixer at the rotating speed of 200-600r/min and the addition of the electromagnetic shielding and magnetic conducting material of 10 percent, carrying out blending extrusion granulation by a double-screw extruder at the processing temperature of 285 ℃ and the working efficiency of 6MHZ, and carrying out extrusion, water cooling, short cutting and drying by a machine head to obtain the electromagnetic shielding and magnetic conducting polymer alloy material. The mechanical strength is increased by 9 percent according to GB/T1843-2008 detection, the toughness is increased by 5 percent according to GB/T1451-
And (3) detecting the electromagnetic shielding performance, wherein the 30 MHz-230 MHz shielding performance is 38%, the 230 MHz-1 GHz shielding performance is 37%, and the 1 GHz-18 GHz shielding performance is 35%.
Example 11:
selection of resin base material: PPA powder (high temperature resistant nylon) is selected as a matrix polymer resin raw material of the resin base material, and the content is 90%;
the electromagnetic shielding nano material is manganese/nickel doped ferrite, is synthesized and prepared by a hydrothermal method, the reaction temperature is 180 ℃, the reaction time is 4 hours, the reaction pH value is 6, the manganese and nickel doping amount is 0.8%, and the nano powder is prepared by firing at 300 ℃, wherein the raw material is ferric chloride, the pH value is adjusted by ammonia water, and manganese and nickel are chlorides, specifically manganese chloride and nickel chloride;
performing surface modification on the electromagnetic shielding nano material, selecting polydimethylsiloxane as a surface modifier, wherein the usage amount of the polydimethylsiloxane is 0.5 percent of that of the nano powder, performing surface modification through high-speed kneading equipment at the rotating speed of 3500r/min at room temperature;
preparing electromagnetic shielding magnetic polymer alloy: mixing the electromagnetic shielding and magnetic conducting nano material and resin powder at the normal temperature of a pre-mixer at the rotating speed of 200-600r/min and the addition of the electromagnetic shielding and magnetic conducting material of 10 percent, carrying out blending extrusion granulation by a double-screw extruder at the processing temperature of 285 ℃ and the working efficiency of 6MHZ, and carrying out extrusion, water cooling, short cutting and drying by a machine head to obtain the electromagnetic shielding and magnetic conducting polymer alloy material.
The mechanical strength is increased by 9% according to GB/T1843-2008 detection, the toughness is increased by 5% according to GB/T1451-.
Example 12:
selection of resin base material: PPA powder (high temperature resistant nylon) is selected as a matrix polymer resin raw material of the resin base material, and the content is 90%;
the electromagnetic shielding nano material is manganese/nickel doped ferrite, is synthesized and prepared by a hydrothermal method, the reaction temperature is 180 ℃, the reaction time is 4 hours, the reaction pH value is 6, the manganese and nickel doping amount is 1.2%, and the nano powder is prepared by firing at 300 ℃, wherein the raw material is ferric chloride, the pH value is adjusted by ammonia water, and manganese and nickel are chlorides, specifically manganese chloride and nickel chloride;
performing surface modification on the electromagnetic shielding nano material, selecting polydimethylsiloxane as a surface modifier, wherein the using amount of the polydimethylsiloxane is 0.5 percent of that of the nano powder, performing surface modification through high-speed kneading equipment at the rotating speed of 3500r/min at room temperature;
preparing electromagnetic shielding magnetic polymer alloy: mixing the electromagnetic shielding and magnetic conducting nano material and resin powder at the normal temperature of a pre-mixer at the rotating speed of 200-600r/min and the addition of the electromagnetic shielding and magnetic conducting material of 10 percent, carrying out blending extrusion granulation by a double-screw extruder at the processing temperature of 285 ℃ and the working efficiency of 6MHZ, and carrying out extrusion, water cooling, short cutting and drying by a machine head to obtain the electromagnetic shielding and magnetic conducting polymer alloy material.
The mechanical strength is increased by 9% according to GB/T1843-2008 detection, the toughness is increased by 5% according to GB/T1451-.
Example 13:
selection of resin base material: PPA powder (high temperature resistant nylon) is selected as a matrix polymer resin raw material of the resin base material, and the content is 90%;
the electromagnetic shielding nano material is manganese/nickel doped ferrite, is synthesized and prepared by a hydrothermal method, the reaction temperature is 180 ℃, the reaction time is 4 hours, the reaction pH value is 6, the manganese and nickel doping amount is 1.6%, and the nano powder is prepared by firing at 300 ℃, wherein the raw material is ferric chloride, the pH value is adjusted by ammonia water, and manganese and nickel are chlorides, specifically manganese chloride and nickel chloride;
performing surface modification on the electromagnetic shielding nano material, selecting polydimethylsiloxane as a surface modifier, wherein the using amount of the polydimethylsiloxane is 0.5 percent of that of the nano powder, performing surface modification through high-speed kneading equipment at the rotating speed of 3500r/min at room temperature;
preparing an electromagnetic shielding magnetic conductive polymer alloy: mixing the electromagnetic shielding and magnetic conducting nano material and resin powder at the normal temperature of a pre-mixer at the rotating speed of 200-600r/min and the addition of the electromagnetic shielding and magnetic conducting material of 10 percent, carrying out blending extrusion granulation by a double-screw extruder at the processing temperature of 285 ℃ and the working efficiency of 6MHZ, and carrying out extrusion, water cooling, short cutting and drying by a machine head to obtain the electromagnetic shielding and magnetic conducting polymer alloy material.
The mechanical strength is increased by 9% according to GB/T1843-2008 detection, the toughness is increased by 5% according to GB/T1451-.
Example 14:
selection of resin base material: PPA powder (high temperature resistant nylon) is selected as a matrix polymer resin raw material of the resin base material, and the content is 90%;
the electromagnetic shielding nano material is manganese/nickel doped ferrite, is synthesized and prepared by a hydrothermal method, the reaction temperature is 180 ℃, the reaction time is 4 hours, the reaction pH value is 6, the manganese and nickel doping amount is 2.0%, and the nano powder is prepared by firing at 300 ℃, wherein the raw material is ferric chloride, the pH value is adjusted by ammonia water, and manganese and nickel are chlorides, specifically manganese chloride and nickel chloride;
performing surface modification on the electromagnetic shielding nano material, selecting polydimethylsiloxane as a surface modifier, wherein the using amount of the polydimethylsiloxane is 0.5 percent of that of the nano powder, performing surface modification through high-speed kneading equipment at the rotating speed of 3500r/min at room temperature; preparing electromagnetic shielding magnetic polymer alloy: mixing the electromagnetic shielding and magnetic conducting nano material and resin powder at the normal temperature of a pre-mixer at the rotating speed of 200-600r/min and the addition of the electromagnetic shielding and magnetic conducting material of 10 percent, carrying out blending extrusion granulation by a double-screw extruder at the processing temperature of 285 ℃ and the working efficiency of 6MHZ, and carrying out extrusion, water cooling, short cutting and drying by a machine head to obtain the electromagnetic shielding and magnetic conducting polymer alloy material.
The mechanical strength is increased by 9% according to GB/T1843-2008 detection, the toughness is increased by 5% according to GB/T1451-.
At this time, the doping amount of manganese and nickel elements is continuously increased, and the shielding performance is basically not changed, so that the effect is best when the doping amount is 1.6%.
Example 15:
selection of resin base material: PPA powder (high temperature resistant nylon) is selected as a matrix polymer resin raw material of the resin base material, and the content is 90%;
the electromagnetic shielding nano material is manganese/nickel doped ferrite, is synthesized and prepared by a hydrothermal method, the reaction temperature is 180 ℃, the reaction time is 4 hours, the reaction pH value is 6, the manganese and nickel doping amount is 1.6%, and the nano powder is prepared by firing at 400 ℃, wherein the raw material is ferric chloride, the pH value is adjusted by ammonia water, and manganese and nickel are chlorides, in particular manganese chloride and nickel chloride;
performing surface modification on the electromagnetic shielding nano material, selecting polydimethylsiloxane as a surface modifier, wherein the using amount of the polydimethylsiloxane is 0.5 percent of that of the nano powder, performing surface modification through high-speed kneading equipment at the rotating speed of 3500r/min at room temperature;
preparing electromagnetic shielding magnetic polymer alloy: mixing the electromagnetic shielding and magnetic conducting nano material and resin powder at normal temperature by a pre-mixer at the rotating speed of 200-600r/min and the adding amount of the electromagnetic shielding and magnetic conducting material of 10 percent, extruding and granulating by a double-screw extruder at the processing temperature of 285 ℃ and the working efficiency of 6MHZ, and extruding by a machine head, water cooling, chopping and drying to obtain the electromagnetic shielding and magnetic conducting polymer alloy material. The mechanical strength is increased by 10% according to GB/T1843-2008 detection, the toughness is increased by 6% according to GB/T1451-.
Example 16:
selection of resin base material: PPA powder (high temperature resistant nylon) is selected as a matrix polymer resin raw material of the resin base material, and the content is 90%;
the electromagnetic shielding nano material is manganese/nickel doped ferrite, is synthesized and prepared by a hydrothermal method, the reaction temperature is 180 ℃, the reaction time is 4 hours, the reaction pH value is 6, the manganese and nickel doping amount is 1.6%, and the nano powder is prepared by firing at 450 ℃, wherein the raw material is ferric chloride, the pH value is adjusted by ammonia water, and manganese and nickel are chlorides, specifically manganese chloride and nickel chloride;
performing surface modification on the electromagnetic shielding nano material, selecting polydimethylsiloxane as a surface modifier, wherein the using amount of the polydimethylsiloxane is 0.5 percent of that of the nano powder, performing surface modification through high-speed kneading equipment at the rotating speed of 3500r/min at room temperature; preparing electromagnetic shielding magnetic polymer alloy: mixing the electromagnetic shielding and magnetic conducting nano material and resin powder at the normal temperature of a pre-mixer at the rotating speed of 200-600r/min and the addition of the electromagnetic shielding and magnetic conducting material of 10 percent, carrying out blending extrusion granulation by a double-screw extruder at the processing temperature of 285 ℃ and the working efficiency of 6MHZ, and carrying out extrusion, water cooling, short cutting and drying by a machine head to obtain the electromagnetic shielding and magnetic conducting polymer alloy material. The mechanical strength is increased by 11% according to GB/T1843-2008 detection, the toughness is increased by 6% according to GB/T1451-.
Example 17:
selection of resin base material: PPA powder (high temperature resistant nylon) is selected as a matrix polymer resin raw material of the resin base material, and the content is 90%;
the electromagnetic shielding nano material is manganese/nickel doped ferrite, is synthesized and prepared by a hydrothermal method, the reaction temperature is 180 ℃, the reaction time is 4 hours, the reaction pH value is 6, the manganese and nickel doping amount is 1.6%, and the nano powder is prepared by firing at 500 ℃, wherein the raw material is ferric chloride, the pH value is adjusted by ammonia water, and manganese and nickel are chlorides, in particular manganese chloride and nickel chloride;
performing surface modification on the electromagnetic shielding nano material, selecting polydimethylsiloxane as a surface modifier, wherein the using amount of the polydimethylsiloxane is 0.5 percent of that of the nano powder, performing surface modification through high-speed kneading equipment at the rotating speed of 3500r/min at room temperature; preparing electromagnetic shielding magnetic polymer alloy: mixing the electromagnetic shielding and magnetic conducting nano material and resin powder at normal temperature by a pre-mixer at the rotating speed of 200-600r/min and the adding amount of the electromagnetic shielding and magnetic conducting material of 10 percent, extruding and granulating by a double-screw extruder at the processing temperature of 285 ℃ and the working efficiency of 6MHZ, and extruding by a machine head, water cooling, chopping and drying to obtain the electromagnetic shielding and magnetic conducting polymer alloy material. The mechanical strength is increased by 11% according to GB/T1843-2008 detection, the toughness is increased by 6% according to GB/T1451-.
The shielding performance is not changed when the temperature is continuously increased, which shows that the nano material forms a uniform structure when being burnt at 450 ℃.
Example 18:
selection of resin base material: PPA powder (high temperature resistant nylon) is selected as a matrix polymer resin raw material of the resin base material, and the content is 80%;
the electromagnetic shielding nano material is manganese/nickel doped ferrite, is synthesized and prepared by a hydrothermal method, the reaction temperature is 180 ℃, the reaction time is 4 hours, the reaction pH value is 6, the manganese and nickel doping amount is 1.6%, and the nano powder is prepared by firing at 450 ℃, wherein the raw material is ferric chloride, the pH value is adjusted by ammonia water, and manganese and nickel are chlorides, specifically manganese chloride and nickel chloride;
performing surface modification on the electromagnetic shielding nano material, selecting polydimethylsiloxane as a surface modifier, wherein the using amount of the polydimethylsiloxane is 0.5 percent of that of the nano powder, performing surface modification through high-speed kneading equipment at the rotating speed of 3500r/min at room temperature; preparing electromagnetic shielding magnetic polymer alloy: mixing the electromagnetic shielding and magnetic conducting nano material and resin powder at the normal temperature of a pre-mixer at the rotating speed of 200-600r/min and the addition of the electromagnetic shielding and magnetic conducting material of 20 percent, performing blending extrusion granulation by a double-screw extruder at the processing temperature of 285 ℃ and the working efficiency of 6MHZ, and performing extrusion, water cooling, short cutting and drying by a machine head to obtain the electromagnetic shielding and magnetic conducting polymer alloy material. The mechanical strength is increased by 13% according to GB/T1843-2008 detection, the toughness is increased by 8% according to GB/T1451-.
Example 19:
selection of resin base material: PPA powder (high temperature resistant nylon) is selected as a matrix polymer resin raw material of the resin base material, and the content is 70%;
the electromagnetic shielding nano material is manganese/nickel doped ferrite, is synthesized and prepared by a hydrothermal method, the reaction temperature is 180 ℃, the reaction time is 4 hours, the reaction pH value is 6, the manganese and nickel doping amount is 1.6%, and the nano powder is prepared by firing at 450 ℃, wherein the raw material is ferric chloride, the pH value is adjusted by ammonia water, and manganese and nickel are chlorides, specifically manganese chloride and nickel chloride;
performing surface modification on the electromagnetic shielding nano material, selecting polydimethylsiloxane as a surface modifier, wherein the using amount of the polydimethylsiloxane is 0.5 percent of that of the nano powder, performing surface modification through high-speed kneading equipment at the rotating speed of 3500r/min at room temperature; preparing electromagnetic shielding magnetic polymer alloy: mixing the electromagnetic shielding and magnetic conducting nano material and resin powder at the normal temperature of a pre-mixer at the rotating speed of 200-600r/min and the addition of the electromagnetic shielding and magnetic conducting material of 30 percent, carrying out blending extrusion granulation by a double-screw extruder at the processing temperature of 285 ℃ and the working efficiency of 6MHZ, and carrying out extrusion, water cooling, short cutting and drying by a machine head to obtain the electromagnetic shielding and magnetic conducting polymer alloy material.
The mechanical strength is increased by 12% according to GB/T1843-2008 detection, the toughness is increased by 7% according to GB/T1451-.
Example 20:
selection of resin base material: PPA powder (high temperature resistant nylon) is selected as a matrix polymer resin raw material of the resin base material, and the content is 60%;
the electromagnetic shielding nano material is manganese/nickel doped ferrite, is synthesized and prepared by a hydrothermal method, the reaction temperature is 180 ℃, the reaction time is 4 hours, the reaction pH value is 6, the manganese and nickel doping amount is 1.6%, and the nano powder is prepared by firing at 450 ℃, wherein the raw material is ferric chloride, the pH value is adjusted by ammonia water, and manganese and nickel are chlorides, specifically manganese chloride and nickel chloride;
performing surface modification on the electromagnetic shielding nano material, selecting polydimethylsiloxane as a surface modifier, wherein the using amount of the polydimethylsiloxane is 0.5 percent of that of the nano powder, performing surface modification through high-speed kneading equipment at the rotating speed of 3500r/min at room temperature; preparing electromagnetic shielding magnetic polymer alloy: mixing the electromagnetic shielding and magnetic conducting nano material and resin powder at normal temperature by a pre-mixer at the rotating speed of 200-600r/min and the adding amount of the electromagnetic shielding and magnetic conducting material of 40 percent, extruding and granulating by a double-screw extruder at the processing temperature of 285 ℃ and the working efficiency of 6MHZ, and extruding by a machine head, water cooling, chopping and drying to obtain the electromagnetic shielding and magnetic conducting polymer alloy material. The mechanical strength is increased by 4% according to GB/T1843-2008 detection, the toughness is increased by-8% according to GB/T1451-.
At the moment, the electromagnetic shielding performance continuously increases with the increase of the addition amount of the nano material, but the mechanical property is reduced.
Example 21:
selection of resin base material: PPA powder (high temperature resistant nylon) is selected as a matrix polymer resin raw material of the resin base material, and the content is 50%;
the electromagnetic shielding nano material is manganese/nickel doped ferrite, is synthesized and prepared by a hydrothermal method, the reaction temperature is 180 ℃, the reaction time is 4 hours, the reaction pH value is 6, the manganese and nickel doping amount is 1.6%, and the nano powder is prepared by firing at 450 ℃, wherein the raw material is ferric chloride, the pH value is adjusted by ammonia water, and manganese and nickel are chlorides, specifically manganese chloride and nickel chloride;
performing surface modification on the electromagnetic shielding nano material, selecting polydimethylsiloxane as a surface modifier, wherein the using amount of the polydimethylsiloxane is 0.5 percent of that of the nano powder, performing surface modification through high-speed kneading equipment at the rotating speed of 3500r/min at room temperature; preparing electromagnetic shielding magnetic polymer alloy: mixing the electromagnetic shielding and magnetic conducting nano material and resin powder at the normal temperature of a pre-mixer at the rotating speed of 200-600r/min and the addition of the electromagnetic shielding and magnetic conducting material of 50 percent, carrying out blending extrusion granulation by a double-screw extruder at the processing temperature of 285 ℃ and the working efficiency of 6MHZ, and carrying out extrusion, water cooling, short cutting and drying by a machine head to obtain the electromagnetic shielding and magnetic conducting polymer alloy material. The mechanical strength is increased by-9% according to GB/T1843-2008 detection, the toughness is increased by-18% according to GB/T1451-.
At the moment, the mechanical property is reduced more, the electromagnetic shielding property is not increased much, so the comprehensive consideration is that the optimal electromagnetic shielding nano material is added with 30 percent of the additive amount, the grade A is obtained when the electromagnetic shielding rate is more than 60 percent, particularly the high-frequency shielding is difficult to realize in the prior art, and the invention can achieve the grade A to the high-frequency shielding.
The invention provides a novel preparation technology of an electromagnetic shielding and magnetic conducting polymer alloy, which can meet the requirements of current and future production and use.
It should be noted that the above-mentioned embodiments are only for illustrating the technical solutions of the present invention and not for limiting, and although the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions may be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention, which should be covered by the claims of the present invention.

Claims (10)

1. A preparation method of an electromagnetic shielding magnetic polymer alloy is characterized by comprising the following steps: comprises the steps of (a) preparing a mixture of a plurality of raw materials,
selection of resin base material: one or more of PPA, PP, PE and PET is/are selected as a matrix polymer resin raw material for the resin base material;
preparing an electromagnetic shielding magnetic material: doping ferrite by adopting manganese/nickel elements through a hydrothermal synthesis method, and preparing nano powder through high-temperature sintering;
carrying out surface modification on the electromagnetic shielding magnetic material: mixing the electromagnetic shielding magnetic powder with a surface modifier in a high-speed kneading mode to prepare a reinforced modified material;
preparing electromagnetic shielding magnetic polymer alloy: and compounding the reinforced modified material and the resin powder, mixing by a premixer, and extruding by a double screw to obtain the electromagnetic shielding magnetic conductive high polymer material.
2. The method for preparing the electromagnetic shielding magnetic conductive polymer alloy according to claim 1, wherein the method comprises the following steps: the particle size of the matrix polymer resin is 100-500 meshes.
3. The method for preparing the electromagnetic shielding magnetic conductive polymer alloy according to claim 1 or 2, wherein the method comprises the following steps: the mass percentage of the resin base material in the electromagnetic shielding magnetic conductive polymer alloy is 50-90%.
4. The method for preparing the electromagnetic shielding magnetic conductive polymer alloy according to claim 1 or 2, wherein the method comprises the following steps: the electromagnetic shielding magnetic material is prepared by doping ferrite with manganese/nickel elements, wherein the manganese and the nickel adopt soluble salts, the ferrite is prepared by reacting soluble ferrous/ferric iron with alkali, and the doping amount of the manganese and the nickel elements is 0.1-3%.
5. The method for preparing the electromagnetic shielding magnetic conductive polymer alloy according to claim 1 or 2, wherein the method comprises the following steps: the preparation method of the electromagnetic shielding magnetic material comprises the steps of adopting a hydrothermal synthesis method, enabling the synthesis temperature to be 100-220 ℃, enabling the reaction time to be 2-8 hours, enabling the pH value during the reaction to be 4-8, filtering the prepared powder, and sintering at 300-500 ℃ to obtain the manganese/nickel doped ferrite nano material.
6. The method for preparing the electromagnetic shielding magnetic conductive polymer alloy according to claim 1 or 2, wherein the method comprises the following steps: the electromagnetic shielding magnetic polymer alloy comprises a manganese/nickel doped ferrite nano material, wherein the addition amount of the manganese/nickel doped ferrite nano material is 10-50%.
7. The method for preparing the electromagnetic shielding magnetic conductive polymer alloy according to claim 1 or 2, wherein the method comprises the following steps: the electromagnetic shielding magnetic material is subjected to surface modification, and is dispersed at normal temperature in a high-speed kneading mode, wherein the rotating speed is 2000-5000 r/min.
8. The method for preparing the electromagnetic shielding magnetic conductive polymer alloy according to claim 7, wherein the method comprises the following steps: the surface modifier comprises methyl silicone oil, polydimethylsiloxane and polycyclomethyl siloxane, and the dosage of the surface modifier is 0.1-3% of the mass of the electromagnetic shielding magnetic conducting material.
9. The method for preparing the electromagnetic shielding magnetic conductive polymer alloy according to claim 7, wherein the method comprises the following steps: the preparation of the electromagnetic shielding magnetic conductive polymer alloy comprises the following steps,
mixing the electromagnetic shielding and magnetic conductive nano material and resin powder through a premixer, and performing blending extrusion granulation through a double-screw extruder to prepare the electromagnetic shielding and magnetic conductive nano material; the mixing speed of the premixer is 200-600r/min, the working temperature is normal temperature, the double-screw extrusion processing temperature is 160-300 ℃, the working efficiency is 1-10 MHZ, and the electromagnetic shielding and magnetic conducting polymer alloy material is obtained through extrusion by a machine head, water cooling, short cutting and drying.
10. The product prepared by the preparation method of the electromagnetic shielding and magnetic conducting polymer alloy as claimed in any one of claims 1 to 9.
CN202111646248.1A 2021-12-30 2021-12-30 Preparation method of electromagnetic shielding magnetic-conducting polymer alloy and product thereof Pending CN114479435A (en)

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