CN115093639B - Surface finish improved shielding material, preparation method and semiconductive shielding product - Google Patents
Surface finish improved shielding material, preparation method and semiconductive shielding product Download PDFInfo
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- 229920001200 poly(ethylene-vinyl acetate) Polymers 0.000 claims description 7
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- QYMGIIIPAFAFRX-UHFFFAOYSA-N butyl prop-2-enoate;ethene Chemical compound C=C.CCCCOC(=O)C=C QYMGIIIPAFAFRX-UHFFFAOYSA-N 0.000 claims description 3
- 239000011259 mixed solution Substances 0.000 claims description 3
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- 239000003963 antioxidant agent Substances 0.000 description 8
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- DOIRQSBPFJWKBE-UHFFFAOYSA-N dibutyl phthalate Chemical compound CCCCOC(=O)C1=CC=CC=C1C(=O)OCCCC DOIRQSBPFJWKBE-UHFFFAOYSA-N 0.000 description 8
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- JKIJEFPNVSHHEI-UHFFFAOYSA-N Phenol, 2,4-bis(1,1-dimethylethyl)-, phosphite (3:1) Chemical compound CC(C)(C)C1=CC(C(C)(C)C)=CC=C1OP(OC=1C(=CC(=CC=1)C(C)(C)C)C(C)(C)C)OC1=CC=C(C(C)(C)C)C=C1C(C)(C)C JKIJEFPNVSHHEI-UHFFFAOYSA-N 0.000 description 4
- BGYHLZZASRKEJE-UHFFFAOYSA-N [3-[3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoyloxy]-2,2-bis[3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoyloxymethyl]propyl] 3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoate Chemical compound CC(C)(C)C1=C(O)C(C(C)(C)C)=CC(CCC(=O)OCC(COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)(COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)=C1 BGYHLZZASRKEJE-UHFFFAOYSA-N 0.000 description 4
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- DEKVAWHRMRNKMI-UHFFFAOYSA-N 1,2-bis(tert-butylperoxy)-3-propan-2-ylbenzene Chemical compound CC(C)C1=CC=CC(OOC(C)(C)C)=C1OOC(C)(C)C DEKVAWHRMRNKMI-UHFFFAOYSA-N 0.000 description 2
- XMNIXWIUMCBBBL-UHFFFAOYSA-N 2-(2-phenylpropan-2-ylperoxy)propan-2-ylbenzene Chemical compound C=1C=CC=CC=1C(C)(C)OOC(C)(C)C1=CC=CC=C1 XMNIXWIUMCBBBL-UHFFFAOYSA-N 0.000 description 2
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- XOOUIPVCVHRTMJ-UHFFFAOYSA-L zinc stearate Chemical compound [Zn+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O XOOUIPVCVHRTMJ-UHFFFAOYSA-L 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
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- FATBGEAMYMYZAF-UHFFFAOYSA-N oleicacidamide-heptaglycolether Natural products CCCCCCCCC=CCCCCCCCC(N)=O FATBGEAMYMYZAF-UHFFFAOYSA-N 0.000 description 1
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Classifications
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/04—Carbon
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/10—Metal compounds
- C08K3/14—Carbides
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/001—Conductive additives
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2203/00—Applications
- C08L2203/20—Applications use in electrical or conductive gadgets
- C08L2203/202—Applications use in electrical or conductive gadgets use in electrical wires or wirecoating
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Conductive Materials (AREA)
Abstract
The invention relates to a shielding material with improved surface finish, a preparation method and a semiconductive shielding product. The surface finish degree improved shielding material is mainly prepared from 55-65 parts by mass of matrix resin, 20-30 parts by mass of conductive carbon black, 1-10 parts by mass of Ti 3C2 MXene, 0.5-2 parts by mass of dispersing agent, 3-6 parts by mass of functional auxiliary agent and 0.9-2 parts by mass of cross-linking agent. The Ti 3C2 MXene surface has polar functional groups, has good compatibility with matrix resin, can improve the dispersibility of conductive carbon black in the matrix resin, reduce the bulges on the surface of the shielding material, improve the surface smoothness of the shielding material, and can also improve the mechanical property of the shielding material.
Description
Technical Field
The invention relates to the technical field of high-voltage cable materials, in particular to a shielding material with improved surface finish, a preparation method and a semiconductive shielding product.
Background
With the increasing demand of electricity at the user side, the power cable is developed towards a high transmission capacity and a longer transmission distance, and the voltage level of the cable is continuously improved. The semiconductive shielding layer is used as an important component of the high-voltage cable and is distributed on the inner side and the outer side of the insulating layer. The semi-conductive shielding layer is used for forming an equipotential body with the cable conductor core and the metal shielding layer, eliminating burrs or bulges on the surface of the metal conductor, uniformly distributing an electric field and inhibiting partial discharge. Typically, the semiconductive shield is made of a semiconductive shield. The semiconductive shielding material has a decisive influence on the performance of the semiconductive shielding layer. For example, the surface finish of the semiconductive shielding material has certain influence on the surface property, mechanical property and conductivity of the semiconductive shielding layer. Conventional semiconductive shields perform poorly in terms of surface finish.
Disclosure of Invention
Based on this, it is necessary to provide a surface finish-improved shielding material, and a method for producing the same and a semiconductive shielding article.
In order to solve the above technical problems, the technical solution of an embodiment of the present invention is as follows.
The shielding material with improved surface finish comprises the following raw materials in parts by weight:
In one embodiment, the preparation method of the Ti 3C2 MXene comprises the following steps: mixing Ti 3AlC2 precursor with hydrofluoric acid solution, and reacting at 20-50 deg.c for 40-50 hr.
In one embodiment, the hydrofluoric acid solution is a mixed solution of hydrochloric acid and lithium fluoride.
In one embodiment, the Ti 3AlC2 precursor is mixed with hydrofluoric acid solution and reacted for 40 to 50 hours at 20 to 50 ℃ and then comprises the following steps:
The mixture obtained by the reaction was centrifuged, and the upper liquid was dried.
The method for preparing a surface finish improvement shielding material according to any one of the above embodiments, comprising the steps of:
Mixing the conductive carbon black with the Ti 3C2 MXene to obtain a first mixture;
mixing the first mixture, the matrix resin, the dispersing agent and the functional auxiliary agent to obtain a second mixture;
extruding and granulating the second mixture to obtain cut granules;
mixing the chopped granules with the cross-linking agent to obtain a preform;
and heating the preform.
In one embodiment, mixing the conductive carbon black with the Ti 3C2 MXene to obtain a first mixture comprises the steps of:
Dispersing the Ti 3C2 Mxene in water to obtain Mxene dispersion;
mixing the Mxene dispersion with the conductive carbon black and then drying to obtain the first mixture.
In one embodiment, the stirring speed when mixing the first mixture, the matrix resin, the dispersant and the functional auxiliary agent is 150rpm to 200rpm.
In one embodiment, the second mixture is extruded at an extrusion temperature of 120 ℃ to 180 ℃.
In one embodiment, the temperature of the heating treatment is 50 ℃ to 70 ℃.
A semiconductive shield composition made from the stock of the surface finish-improving shield composition described in any one of the embodiments above.
The surface finish improved shielding material is mainly prepared from 55-65 parts by mass of matrix resin, 20-30 parts by mass of conductive carbon black, 1-10 parts by mass of Ti 3C2 MXene, 0.5-2 parts by mass of dispersing agent, 3-6 parts by mass of functional auxiliary agent and 0.9-2 parts by mass of cross-linking agent. The Ti 3C2 MXene surface has polar functional groups, has good compatibility with matrix resin, can improve the dispersibility of conductive carbon black in the matrix resin, reduce the bulges on the surface of the shielding material, improve the surface smoothness of the shielding material, and can also improve the mechanical property of the shielding material.
Further, the Ti 3C2 MXene has high specific surface area and diameter-thickness ratio, so that the conductive carbon black can be dispersed around the Ti 3C2 MXene or loaded on a sheet of the Ti 3C2 MXene, three-dimensional space contact between a two-dimensional material and a spherical material is realized, and further, bridging effect can be achieved in matrix resin, a stable conductive network is formed, and the conductive performance of the shielding material is improved.
Detailed Description
The following detailed description of the present invention will provide further details in order to make the above-mentioned objects, features and advantages of the present invention more comprehensible. In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present invention. The present invention may be embodied in many other forms than described herein and similarly modified by those skilled in the art without departing from the spirit of the invention, whereby the invention is not limited to the specific embodiments disclosed below.
The terms "first," "second," and the like, are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defining "a first" or "a second" may explicitly or implicitly include at least one such feature. In the description of the present invention, the meaning of "plurality" means at least two, for example, two, three, etc., unless specifically defined otherwise.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used herein in the description of the invention is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. The term "and/or" as used herein includes any and all combinations of one or more of the associated listed items.
An embodiment of the invention provides a shielding material with improved surface finish. The surface finish improvement type shielding material comprises the following components in parts by weight: 55 to 65 parts of matrix resin, 20 to 30 parts of conductive carbon black, 1 to 10 parts of Ti 3C2 MXene, 0.5 to 2 parts of dispersing agent, 3 to 6 parts of functional auxiliary agent and 0.9 to 2 parts of cross-linking agent. In the surface finish improvement type shielding material of the embodiment, the surface finish improvement type shielding material is mainly prepared from 55-65 parts by mass of matrix resin, 20-30 parts by mass of conductive carbon black, 1-10 parts by mass of Ti 3C2 MXene, 0.5-2 parts by mass of dispersing agent, 3-6 parts by mass of functional auxiliary agent and 0.9-2 parts by mass of cross-linking agent. The Ti 3C2 MXene surface has polar functional groups, has good compatibility with matrix resin, can improve the dispersibility of conductive carbon black in the matrix resin, reduce the bulges on the surface of the shielding material, improve the surface smoothness of the shielding material, and can also improve the mechanical property of the shielding material. Further, the Ti 3C2 MXene has high specific surface area and diameter-thickness ratio, so that the conductive carbon black can be dispersed around the Ti 3C2 MXene or loaded on a sheet of the Ti 3C2 MXene, three-dimensional space contact between a two-dimensional material and a spherical material is realized, and further, bridging effect can be achieved in matrix resin, a stable conductive network is formed, and the conductive performance of the shielding material is improved.
In one specific example, ti 3C2 MXene is a two-dimensional sheet structure. Alternatively, ti 3C2 MXene is a powder particle.
In a specific example, the preparation method of Ti 3C2 MXene comprises the following steps: mixing Ti 3AlC2 precursor with hydrofluoric acid solution, and reacting at 20-50 deg.c for 40-50 hr. Alternatively, the reaction temperature is 20 ℃, 25 ℃, 30 ℃, 35 ℃, 40 ℃, 45 ℃ or 50 ℃. The reaction time was 40h, 42h, 45h, 48h or 50h. It will be appreciated that the reaction is carried out in a water bath. It is also understood that agitation is maintained during the reaction. Further, after the reaction for 40 to 50 hours, the resulting mixture was subjected to centrifugation several times. For example, the centrifugation speed is 3000r/min to 4000r/min, and the time for each centrifugation is 5min to 10min. The times of centrifugation are 8-15 times.
In a specific example, the hydrofluoric acid solution is a mixed solution of hydrochloric acid and lithium fluoride. Optionally, the concentration of the hydrochloric acid is 20% -30%. In the preparation of hydrofluoric acid solution, lithium fluoride is added into hydrochloric acid, and then stirred and reacted for 8-12 h.
Further, the Ti 3AlC2 precursor is mixed with hydrofluoric acid solution and reacts for 40 to 50 hours at the temperature of 20 to 50 ℃ and then comprises the following steps: the mixture obtained by the reaction was centrifuged, and the upper liquid was dried. Optionally, transferring the mixture obtained by the reaction into a centrifuge tube, carrying out ultrasonic treatment for 1h by using a water bath, centrifuging at 3500r/min for 30min after the ultrasonic treatment is finished, collecting upper-layer liquid, repeating ultrasonic treatment, centrifuging, and collecting the upper-layer liquid. The upper liquid was then dried to give Ti 3C2 MXene. At this time, ti 3C2 MXene powder particles can be obtained.
In a specific example, the surface finish improvement type shielding material comprises the following components in parts by weight: 60 to 64 parts of matrix resin, 25 to 29 parts of conductive carbon black, 1 to 5 parts of Ti 3C2 MXene, 1 to 1.5 parts of dispersing agent, 3 to 5 parts of functional auxiliary agent and 1 to 2 parts of cross-linking agent.
Further, the mass ratio of the conductive carbon black to the Ti 3C2 MXene is 29:1-25:5. Preferably, the mass ratio of the conductive carbon black to the Ti 3C2 MXene is 26:4.
As an alternative example of the mass part of the matrix resin, the mass part of the matrix resin may be, but is not limited to, 55 parts, 56 parts, 57 parts, 58 parts, 59 parts, 60 parts, 61 parts, 62 parts, 63 parts, 64 parts, or 65 parts. It will be appreciated that the mass fraction of the matrix resin may be selected within the range of 55 parts to 65 parts as appropriate.
As an alternative example of the mass part of the conductive carbon black, the mass part of the conductive carbon black may be, but is not limited to, 20 parts, 21 parts, 22 parts, 23 parts, 24 parts, 25 parts, 26 parts, 27 parts, 28 parts, 29 parts, or 30 parts. It will be appreciated that the mass fraction of conductive carbon black may be selected within the range of 20 parts to 30 parts as appropriate.
As an alternative example of the parts by mass of Ti 3C2 MXene, the parts by mass of Ti 3C2 MXene may be, but are not limited to, 1 part, 2 parts, 3 parts, 4 parts, 5 parts, 6 parts, 7 parts, 8 parts, 9 parts, or 10 parts. It will be appreciated that the parts by weight of Ti 3C2 MXene may be selected in the range 1 part to 10 parts as appropriate.
As an alternative example of the mass part of the dispersant, the mass part of the dispersant may be, but is not limited to, 0.5 part, 0.8 part, 1 part, 1.1 part, 1.2 part, 1.4 part, 1.5 part, 1.7 part, 1.9 part, or 2 part. It will be appreciated that the mass fraction of dispersant may be selected in the range of 0.5 to 2 parts as appropriate.
As an alternative example of the parts by mass of the functional auxiliary, the parts by mass of the functional auxiliary may be, but are not limited to, 3 parts, 3.2 parts, 3.5 parts, 3.8 parts, 4 parts, 4.2 parts, 4.5 parts, 4.8 parts, 5 parts, 5.2 parts, 5.5 parts, 5.8 parts, or 6 parts. It is understood that the mass fraction of the functional auxiliary agent may be selected from the range of 3 to 6 parts.
As an alternative example of the parts by mass of the crosslinking agent, the parts by mass of the crosslinking agent may be, but is not limited to, 0.9 parts, 1 parts, 1.1 parts, 1.2 parts, 1.3 parts, 1.4 parts, 1.5 parts, 1.6 parts, 1.7 parts, 1.8 parts, 1.9 parts, or 2 parts. It will be appreciated that the cross-linking agent may be selected in a range of from 0.9 parts to 2 parts by mass as appropriate.
It will be appreciated that the surface finish improved shield is a surface finish improved high voltage cable semiconductive shield. That is, still another embodiment of the present invention provides a surface finish improved high voltage cable semiconductive shield composition. The surface finish improved high-voltage cable semiconductive shielding material comprises the following raw materials in parts by weight: 55 to 65 parts of matrix resin, 20 to 30 parts of conductive carbon black, 1 to 10 parts of Ti 3C2 MXene, 0.5 to 2 parts of dispersing agent, 3 to 6 parts of functional auxiliary agent and 0.9 to 2 parts of cross-linking agent.
Yet another embodiment of the present invention provides a surface finish improved shielding material. The surface finish improvement type shielding material is prepared from the following components in parts by weight: 55 to 65 parts of matrix resin, 20 to 30 parts of conductive carbon black, 1 to 10 parts of Ti 3C2 MXene, 0.5 to 2 parts of dispersing agent, 3 to 6 parts of functional auxiliary agent and 0.9 to 2 parts of cross-linking agent. In the example, the shielding material can achieve good surface finish, good electric conduction performance and good mechanical performance by matching 55-65 parts of matrix resin, 20-30 parts of conductive carbon black, 1-10 parts of Ti 3C2 MXene, 0.5-2 parts of dispersing agent, 3-6 parts of functional auxiliary agent and 0.9-2 parts of cross-linking agent.
In a specific example, as a choice of functional auxiliaries, the functional auxiliaries are made from components comprising, by mass: 1 to 2 parts of coupling agent, 1 to 3 parts of lubricant and 0.6 to 1 part of antioxidant. Optionally, the coupling agent is a silane coupling agent. The lubricant is at least one of zinc stearate and pentaerythritol. The antioxidant is at least one of antioxidant 1010 and antioxidant 168. Further alternatively, a silane coupling agent KH550. The antioxidant is formed by mixing an antioxidant 1010 and an antioxidant 168 according to the mass ratio of (1.5-2.5) to 1. Still further, the mass ratio of antioxidant 1010 to antioxidant 168 may be, but is not limited to, 1.8:1, 2:1, 2.2:1, 2.5:1. Optionally, the functional auxiliary agent is formed by mixing a coupling agent, a lubricant and an antioxidant.
It is understood that in the functional auxiliary agent, the mass part of the coupling agent may be, but is not limited to, 1 part, 1.2 parts, 1.5 parts, 1.8 parts, 2 parts, or the like. The lubricant may be, but is not limited to, 1 part, 1.2 parts, 1.5 parts, 1.8 parts, 2 parts, 2.2 parts, 2.5 parts, 2.8 parts, or 3 parts by mass. The antioxidant may be, but not limited to, 0.6 parts, 0.7 parts, 0.8 parts, 0.9 parts, 1 part, etc. It is also understood that the mass fraction of the coupling agent may be selected in the range of 1 to 2 parts, the mass fraction of the lubricant may be selected in the range of 1 to 3 parts, and the mass fraction of the antioxidant may be selected in the range of 0.6 to 1 part.
As an alternative example of the matrix resin, the matrix resin is at least one of ethylene-vinyl acetate copolymer (EVA), ethylene-butyl acrylate copolymer (EBA), and ethylene-ethyl acrylate copolymer (EEA). In preparing the semiconductive shielding material for the high-voltage cable, the shielding material for the crosslinked polyethylene insulated cable can adopt ethylene-vinyl acetate copolymer (EVA), ethylene-butyl acrylate copolymer (EBA) and ethylene-ethyl acrylate copolymer (EEA) as matrixes. However, when the ethylene-vinyl acetate copolymer (EVA) is applied to a shielding material for a cable with a voltage class of 110kV and above, a small amount of acidic substances can be released to corrode a copper conductor under high voltage, and the service life of the cable is reduced. Preferably, the matrix resin is an ethylene-ethyl acrylate copolymer (EEA).
As an alternative example of the conductive carbon black, the DBP (dibutyl phthalate) absorption value of the conductive carbon black is 120ml/100g to 200ml/170g. For example, the DBP absorption value of the conductive carbon black is 120ml/100g, 130ml/100g, 150ml/100g, 160ml/100g or 170ml/100g, etc. Further, the ash content of the conductive carbon black is less than or equal to 0.2 percent. Further, the ash content of the conductive carbon black is less than 0.2%, and further, the ash content of the conductive carbon black is less than 0.1%.
As an alternative example of the dispersant, the dispersant is at least one of Ethylene Bis Stearamide (EBS) and oleamide.
As an alternative example of the crosslinking agent, the crosslinking agent is at least one of bis-t-butylperoxyisopropyl benzene (BIPB) and dicumyl peroxide (DCP).
In another embodiment of the present invention, a method for preparing the surface finish improving shielding material is provided. The preparation method comprises the following steps: mixing conductive carbon black with Ti 3C2 MXene to obtain a first mixture; mixing the first mixture, matrix resin, a dispersing agent and a functional auxiliary agent to obtain a second mixture; extruding and granulating the second mixture to obtain granules; mixing the cut particles with a cross-linking agent to obtain a preform; and heating the preform. In the preparation method of the embodiment, the preparation method is simple and feasible and is suitable for popularization.
In a specific example, a conductive carbon black is mixed with Ti 3C2 MXene to obtain a first mixture, comprising the steps of: dispersing Ti 3C2 Mxene in water to obtain Mxene dispersion; the Mxene dispersion was mixed with conductive carbon black and then dried to obtain a first mixture. In this example, a first mixture was prepared by solution blending conductive carbon black and Ti 3C2 MXene. The Ti 3C2 MXene has good water dispersibility, conductive carbon black can be assisted to be dispersed in an aqueous solution to reduce conductive carbon black aggregation, so that the phenomenon that the conductive carbon black is easy to aggregate in matrix resin in the extrusion process is reduced, and the surface smoothness of the shielding material can be further improved. In this example, when the Mxene dispersion is mixed with the conductive carbon black, the water bath is sonicated for 1 to 5 hours, and then dried at 100 to 150 ℃ for 10 to 20 hours. Alternatively, the time of the water bath ultrasound is 1h, 2h, 3h, 4h or 5h. The drying temperature is 100deg.C, 110deg.C, 120deg.C, 130deg.C, 140 deg.C or 150deg.C. The drying time is 10h, 12h, 15h, 18h or 20h. Further alternatively, the mixing of the Mxene dispersion with the conductive carbon black is adding the conductive carbon black to the Mxene dispersion.
In another specific example, the conductive carbon black is mixed with Ti 3C2 MXene to obtain a first mixture, or the conductive carbon black and Ti 3C2 MXene powder particles are mixed solid-solid to obtain the first mixture.
In a specific example, the stirring speed at the time of mixing the first mixture, the matrix resin, the dispersant, and the functional auxiliary agent is 150rpm to 200rpm. Optionally, the stirring speed when mixing the first mixture, the matrix resin, the dispersant, the functional auxiliary agent is 150rpm, 160rpm, 170rpm, 180rpm, 190rpm, 200rpm, or the like. Optionally, the mixing time for mixing the first mixture, the matrix resin, the dispersant, the functional auxiliary agent is 8min, 10min, 15min or 20min, etc. It is understood that the stirring and mixing are performed in the mixer, and the speed, time and the like of the stirring and mixing can be conveniently controlled by setting the working parameters of the mixer.
In a specific example, the extrusion temperature at which the second mixture is extruded is 120 ℃ to 180 ℃. For example, the extrusion temperature is 130 ℃, 140 ℃, 150 ℃, 160 ℃, 170 ℃,180 ℃, or the like. Further, five-stage extrusion was employed, and the temperature of the five stages was 130℃and 140℃and 150℃and 160℃respectively. It is understood that extrusion is performed in an extruder, and that the host rotation speed of the extruder is controlled to 80rpm to 150rpm at the time of extrusion. For example, the host rotation speed of the extruder is controlled to 80rpm, 90rpm, 100rpm, 110rpm, 120rpm, 130rpm, 140rpm, or the like. Alternatively, the extrusion is performed in a twin screw extruder.
Further, before mixing the chopped pellets with the crosslinking agent, the method further comprises the steps of: and (3) preserving the temperature of the chopped granules at 60-80 ℃. Alternatively, the incubation temperature is 60 ℃, 65 ℃, 70 ℃, 75 ℃, 80 ℃, or the like. Further, the heat preservation time is 3-8 h. Optionally, the incubation time is 3h, 4h, 5h, 6h, 7h, 8h, or the like.
Still further, before mixing the chopped pellets with the crosslinking agent, the method further comprises the steps of: the crosslinking agent is subjected to grinding treatment. The grinding time is 8 min-20 min. Specifically, the grinding time is 8min, 10min, 15min or 20min, etc. It will be appreciated that the milling may be carried out in a mill.
In one specific example, the dicing is underwater dicing. It will be appreciated that after underwater pelletization, the pellets are dried to remove moisture and then incubated.
In a specific example, the temperature of the heat treatment is 50 to 70 ℃. Alternatively, the temperature of the heat treatment is 50 ℃, 55 ℃, 60 ℃, 65 ℃, or 70 ℃, etc. Further, the heating treatment time is 5-10 hours. Alternatively, the time of the heat treatment is 5h, 6h, 7h, 8h, 9h, 10h, or the like. By the heat treatment, the crosslinking agent can be sufficiently absorbed by the cut pellets to improve the performance of the surface finish-improved shielding material.
It will be appreciated that in preparing the surface finish improving type shielding material, the following steps are further included before mixing the conductive carbon black with the Ti 3C2 MXene: and drying the matrix resin, the conductive carbon black, the Ti 3C2 MXene, the dispersing agent, the functional auxiliary agent and the cross-linking agent to remove the moisture in the raw materials.
Yet another embodiment of the present invention provides a semiconductive shielding article. The semiconductive shielding product is made from raw materials comprising the surface finish improvement type shielding material. Alternatively, the semiconductive shield composition is extruded from a feedstock comprising the surface finish-improving shield composition described above. Further alternatively, the semiconductive shielding article is a semiconductive shielding can. Alternatively, the semiconductive shielding article is a high voltage cable semiconductive shielding article.
In a specific example, the semiconductive shielding article may further comprise an insulating material in the raw material from which the semiconductive shielding article is prepared. The semiconductive shielding product is produced by extrusion molding of a raw material including the above surface finish improving shielding material and insulating material.
The following are specific examples.
Example 1
The surface light cleanliness improving shielding material in the embodiment is prepared from the following raw materials in parts by weight: 63.5 parts of matrix resin, 29 parts of conductive carbon black, 1 part of Ti 3C2 MXene, 1 part of dispersing agent, 4.5 parts of functional auxiliary agent and 1 part of crosslinking agent. Wherein the matrix resin is ethylene-ethyl acrylate copolymer. The DBP absorption value of the conductive carbon black is 120-150 ml/100g, and the ash content of the conductive carbon black is less than 0.2%. The dispersing agent is ethylene bis stearamide. The cross-linking agent is bis-tert-butylperoxyisopropyl benzene (BIPB).
The functional auxiliary agent is prepared by mixing the following raw materials in parts by weight: 2 parts of coupling agent, 2 parts of lubricant and 0.5 part of antioxidant. Wherein the coupling agent is silane coupling agent KH550. The lubricant is zinc stearate. The antioxidant is formed by mixing an antioxidant 1010 and an antioxidant 168 according to a mass ratio of 2:1.
The preparation method of Ti 3C2 MXene in the embodiment comprises the following steps:
s101: 60ml of 20% hydrochloric acid was taken, 5g of lithium fluoride was added to the hydrochloric acid solution, and then the solution was put into a water bath for heating and stirring for 12 hours.
S102: 3g of Ti 3AlC2 precursor is taken, added into the solution obtained in S101, water-bath is carried out at 50 ℃, and after stirring is continued for 48 hours, centrifugation is carried out for 5min at 3500r/min, and 10 times are repeated.
S103: transferring the mixture obtained in the step S102 into a centrifuge tube, carrying out ultrasonic treatment for 1h by using a water bath, centrifuging at 3500r/min for 30min after the ultrasonic treatment is finished, collecting upper-layer liquid, repeating ultrasonic treatment, centrifuging, and collecting the upper-layer liquid. The upper liquid is then dried to give Ti 3C2 MXene powder particles.
The preparation method of the surface light cleanliness improvement type shielding material in the embodiment comprises the following steps:
S201: the base resin, conductive carbon black, ti 3C2 MXene powder particles, dispersant, functional auxiliary agent and cross-linking agent are dried at 60 ℃ for 24 hours to remove water.
S202: dispersing Ti 3C2 Mxene in 350mL distilled water, magnetically stirring for 1h, and rotating at 100r/min to obtain Mxene dispersion; conductive carbon black is added into Mxene dispersion liquid, water bath is carried out for 1.5 hours, and then the mixture is dried for 12 hours at 120 ℃ to obtain a first mixture.
S203: the first mixture, the matrix resin, the dispersant and the functional auxiliary agent were mixed for 10min at a stirring speed of 160rpm, to obtain a second mixture.
S204: and (3) carrying out melt extrusion on the second mixture in a double-screw extruder, wherein five-section extrusion is adopted, and the temperature of the five sections is 130 ℃,140 ℃,150 ℃, 160 ℃ and 150 ℃ respectively. The host rotation speed was 100rpm. After extrusion, granulating and drying to obtain the cut granules.
S205: drying the cut granules to remove water, and then preserving the temperature at 60 ℃ for 4 hours.
S206: the cross-linking agent was milled in a mill for 8min.
S207: mixing the cut pellets after heat preservation with the cross-linking agent after grinding for 10min to obtain a preform.
S208: the preform was heated at 60℃for 10h.
After heating, the surface finish-improved shielding material in this example was obtained.
Example 2
Compared with embodiment 1, this embodiment is different in that: the semiconductive shielding material for the high-voltage cable in the embodiment is prepared from the following raw materials in parts by weight: 63.5 parts of matrix resin, 28 parts of conductive carbon black, 2 parts of Ti 3C2 MXene, 1 part of dispersing agent, 4.5 parts of functional auxiliary agent and 1 part of cross-linking agent.
Example 3
Compared with embodiment 1, this embodiment is different in that: the semiconductive shielding material for the high-voltage cable in the embodiment is prepared from the following raw materials in parts by weight: 63.5 parts of matrix resin, 27 parts of conductive carbon black, 3 parts of Ti 3C2 MXene, 1 part of dispersing agent, 4.5 parts of functional auxiliary agent and 1 part of crosslinking agent.
Example 4
Compared with embodiment 1, this embodiment is different in that: the semiconductive shielding material for the high-voltage cable in the embodiment is prepared from the following raw materials in parts by weight: 63.5 parts of matrix resin, 26 parts of conductive carbon black, 4 parts of Ti 3C2 MXene, 1 part of dispersing agent, 4.5 parts of functional auxiliary agent and 1 part of crosslinking agent.
Comparative example 1
Compared with embodiment 1, this embodiment is different in that: the semiconductive shielding material for the high-voltage cable in the embodiment is prepared from the following raw materials in parts by weight: 63.5 parts of matrix resin, 30 parts of conductive carbon black, 0 part of Ti 3C2 MXene, 1 part of dispersing agent, 4.5 parts of functional auxiliary agent and 1 part of crosslinking agent.
Comparative example 2
Compared with embodiment 1, this embodiment is different in that: the semiconductive shielding material for the high-voltage cable in the embodiment is prepared from the following raw materials in parts by weight: 61.5 parts of matrix resin, 32 parts of conductive carbon black, 0 part of Ti 3C2 MXene, 1 part of dispersing agent, 4.5 parts of functional auxiliary agent and 1 part of crosslinking agent.
Comparative example 3
Compared with embodiment 1, this embodiment is different in that: the semiconductive shielding material for the high-voltage cable in the embodiment is prepared from the following raw materials in parts by weight: 58.5 parts of matrix resin, 35 parts of conductive carbon black, 0 part of Ti 3C2 MXene, 1 part of dispersing agent, 4.5 parts of functional auxiliary agent and 1 part of crosslinking agent.
Test case
The shields obtained in examples and comparative examples were each pressed to prepare test boards having a thickness of 1mm and a length and width of 10cm×10 cm. Then respectively testing tensile strength, elongation at break, normal-temperature volume resistivity and 90 ℃ volume resistivity of the test board; sheets having a length of 1m and a width of 0.02m were prepared by a single screw basis to observe the number of protrusions on the surface thereof. The test results are shown in Table 1.
TABLE 1
As can be seen from table 1, the surface finish of the shield in the examples is superior to that of the comparative examples. And in examples 1 to 4, the surface finish was gradually improved. This is probably due to the good water dispersibility of Ti 3C2 MXene, the auxiliary dispersion of the conductive carbon black in the aqueous solution reduces conductive carbon black agglomeration, reduces the agglomeration phenomenon occurring during extrusion, and improves the surface finish of the shielding material.
In examples 1 to 4, the Ti 3C2 MXene content was gradually increased, and the resistivity at 23℃was decreased from 17.3. Omega. Cm to 8.1. Omega. Cm, and the resistivity at 90℃was decreased from 224.8. Omega. Cm to 76.3. Omega. Cm. The resistivity is significantly improved. This is probably because the two-dimensional sheet-like Ti 3C2 MXene can form a bridging action between the conductive carbon black particles to form a stable conductive network. Comparative example 3 used 35 parts of conductive carbon black and example 1 had similar resistivity. The introduction of Ti 3C2 MXene from the side surface can effectively reduce the consumption of the conductive carbon black, so that the processing of the shielding material is easier.
Further, the mechanical properties of the shield in the examples increase with increasing Ti 3C2 MXene content, probably due to the two-dimensional flaky Ti 3C2 MXene having polar functional groups, such as: -OH, -F, -O, -Cl, which has better compatibility with polar matrix resin, thereby further improving the mechanical properties of the shielding material.
The technical features of the above-described embodiments may be arbitrarily combined, and all possible combinations of the technical features in the above-described embodiments are not described for brevity of description, however, as long as there is no contradiction between the combinations of the technical features, they should be considered as the scope of the description.
The above examples illustrate only a few embodiments of the invention, which are described in detail and are not to be construed as limiting the scope of the invention. It should be noted that it will be apparent to those skilled in the art that several variations and modifications can be made without departing from the spirit of the invention, which are all within the scope of the invention. The scope of the invention is, therefore, indicated by the appended claims, and the description may be intended to interpret the contents of the claims.
Claims (9)
1. The shielding material with the improved surface finish is characterized by comprising the following raw materials in parts by weight:
the matrix resin is at least one of ethylene-vinyl acetate copolymer, ethylene-butyl acrylate copolymer and ethylene-ethyl acrylate copolymer;
the preparation method of the surface finish improvement type shielding material comprises the following steps:
Mixing the conductive carbon black with the Ti 3C2 MXene to obtain a first mixture;
mixing the first mixture, the matrix resin, the dispersing agent and the functional auxiliary agent to obtain a second mixture;
extruding and granulating the second mixture to obtain cut granules;
mixing the chopped granules with the cross-linking agent to obtain a preform;
and heating the preform.
2. The surface finish improvement type shielding material according to claim 1, wherein the preparation method of the Ti 3C2 MXene comprises the steps of: mixing Ti 3AlC2 precursor with hydrofluoric acid solution, and reacting at 20-50 deg.c for 40-50 hr.
3. The surface finish improving shielding material according to claim 2, wherein the hydrofluoric acid solution is a mixed solution of hydrochloric acid and lithium fluoride.
4. The surface finish improvement shielding material according to any one of claims 2 to 3, wherein the Ti 3AlC2 precursor is mixed with a hydrofluoric acid solution, and the reaction is carried out at 20 ℃ to 50 ℃ for 40h to 50h, and then the method further comprises the steps of:
The mixture obtained by the reaction was centrifuged, and the upper liquid was dried.
5. The surface finish improving shielding material of claim 1, wherein mixing the conductive carbon black with the Ti 3C2 MXene to obtain a first mixture comprises the steps of:
Dispersing the Ti 3C2 Mxene in water to obtain Mxene dispersion;
mixing the Mxene dispersion with the conductive carbon black and then drying to obtain the first mixture.
6. The surface finish improving shielding material according to claim 1, wherein a stirring speed at the time of mixing the first mixture, the base resin, the dispersant, and the functional auxiliary agent is 150rpm to 200rpm.
7. The surface finish improving shielding material of claim 1, wherein the extrusion temperature at which the second mixture is extruded is 120 ℃ to 180 ℃.
8. The surface finish improvement shielding material according to any one of claims 5 to 7, wherein the temperature of the heat treatment is 50 ℃ to 70 ℃.
9. A semiconductive shielding article, characterized in that it is made from a raw material comprising the surface finish improving shielding material according to any one of claims 1 to 8.
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