CN112661908A - Antistatic resin for aluminum-plastic composite belt and preparation method thereof - Google Patents
Antistatic resin for aluminum-plastic composite belt and preparation method thereof Download PDFInfo
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- CN112661908A CN112661908A CN202011504292.4A CN202011504292A CN112661908A CN 112661908 A CN112661908 A CN 112661908A CN 202011504292 A CN202011504292 A CN 202011504292A CN 112661908 A CN112661908 A CN 112661908A
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- 239000002131 composite material Substances 0.000 title claims abstract description 54
- 229920003023 plastic Polymers 0.000 title claims abstract description 54
- 239000004033 plastic Substances 0.000 title claims abstract description 54
- 229920005989 resin Polymers 0.000 title claims abstract description 52
- 239000011347 resin Substances 0.000 title claims abstract description 52
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 239000002245 particle Substances 0.000 claims abstract description 85
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 59
- 239000004964 aerogel Substances 0.000 claims abstract description 33
- 239000000463 material Substances 0.000 claims abstract description 29
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 28
- 239000006185 dispersion Substances 0.000 claims abstract description 23
- JBKVHLHDHHXQEQ-UHFFFAOYSA-N epsilon-caprolactam Chemical compound O=C1CCCCCN1 JBKVHLHDHHXQEQ-UHFFFAOYSA-N 0.000 claims abstract description 16
- 229920001903 high density polyethylene Polymers 0.000 claims abstract description 14
- 239000004700 high-density polyethylene Substances 0.000 claims abstract description 14
- FPYJFEHAWHCUMM-UHFFFAOYSA-N maleic anhydride Chemical compound O=C1OC(=O)C=C1 FPYJFEHAWHCUMM-UHFFFAOYSA-N 0.000 claims abstract description 14
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 claims abstract description 8
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000005662 Paraffin oil Substances 0.000 claims abstract description 8
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 44
- 238000002156 mixing Methods 0.000 claims description 43
- 238000003756 stirring Methods 0.000 claims description 37
- 229910002804 graphite Inorganic materials 0.000 claims description 34
- 239000010439 graphite Substances 0.000 claims description 34
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 24
- 239000002244 precipitate Substances 0.000 claims description 20
- 239000005909 Kieselgur Substances 0.000 claims description 19
- 238000004321 preservation Methods 0.000 claims description 19
- 239000000203 mixture Substances 0.000 claims description 16
- 238000001816 cooling Methods 0.000 claims description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 12
- 238000001035 drying Methods 0.000 claims description 11
- 238000012986 modification Methods 0.000 claims description 11
- 230000004048 modification Effects 0.000 claims description 11
- 239000000725 suspension Substances 0.000 claims description 11
- 238000005406 washing Methods 0.000 claims description 11
- 238000001354 calcination Methods 0.000 claims description 10
- 238000000227 grinding Methods 0.000 claims description 10
- 239000011159 matrix material Substances 0.000 claims description 9
- 238000002791 soaking Methods 0.000 claims description 8
- 238000003837 high-temperature calcination Methods 0.000 claims description 7
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 7
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 7
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 7
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 5
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 5
- 239000011248 coating agent Substances 0.000 claims description 5
- 238000000576 coating method Methods 0.000 claims description 5
- 239000008367 deionised water Substances 0.000 claims description 5
- 229910021641 deionized water Inorganic materials 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 5
- 239000007788 liquid Substances 0.000 claims description 5
- 238000000034 method Methods 0.000 claims description 5
- 238000000465 moulding Methods 0.000 claims description 5
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 5
- 238000000926 separation method Methods 0.000 claims description 5
- 238000001132 ultrasonic dispersion Methods 0.000 claims description 5
- 238000005303 weighing Methods 0.000 claims description 5
- 239000003963 antioxidant agent Substances 0.000 claims 1
- 230000003078 antioxidant effect Effects 0.000 claims 1
- 230000005672 electromagnetic field Effects 0.000 abstract description 13
- 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 abstract description 5
- 239000000126 substance Substances 0.000 abstract description 2
- 239000000243 solution Substances 0.000 description 26
- 230000000052 comparative effect Effects 0.000 description 18
- 229960000892 attapulgite Drugs 0.000 description 13
- 238000006243 chemical reaction Methods 0.000 description 13
- 239000011259 mixed solution Substances 0.000 description 13
- 229910052625 palygorskite Inorganic materials 0.000 description 13
- 239000002216 antistatic agent Substances 0.000 description 12
- VWDWKYIASSYTQR-UHFFFAOYSA-N sodium nitrate Chemical compound [Na+].[O-][N+]([O-])=O VWDWKYIASSYTQR-UHFFFAOYSA-N 0.000 description 12
- -1 graphite alkene Chemical class 0.000 description 10
- 238000012360 testing method Methods 0.000 description 9
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 8
- 229910052782 aluminium Inorganic materials 0.000 description 8
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 6
- 239000012286 potassium permanganate Substances 0.000 description 6
- 235000010344 sodium nitrate Nutrition 0.000 description 6
- 239000004317 sodium nitrate Substances 0.000 description 6
- 230000000694 effects Effects 0.000 description 5
- 239000012298 atmosphere Substances 0.000 description 4
- 239000002041 carbon nanotube Substances 0.000 description 4
- 229910021393 carbon nanotube Inorganic materials 0.000 description 4
- 239000008187 granular material Substances 0.000 description 4
- 239000013307 optical fiber Substances 0.000 description 4
- 238000011056 performance test Methods 0.000 description 4
- 238000012545 processing Methods 0.000 description 4
- 238000007873 sieving Methods 0.000 description 4
- 238000009864 tensile test Methods 0.000 description 4
- 239000000853 adhesive Substances 0.000 description 3
- 230000001070 adhesive effect Effects 0.000 description 3
- 238000005253 cladding Methods 0.000 description 3
- 239000000155 melt Substances 0.000 description 3
- 239000003607 modifier Substances 0.000 description 3
- 239000011148 porous material Substances 0.000 description 3
- 239000004831 Hot glue Substances 0.000 description 2
- 238000005411 Van der Waals force Methods 0.000 description 2
- 229910021536 Zeolite Inorganic materials 0.000 description 2
- 230000009471 action Effects 0.000 description 2
- 150000008064 anhydrides Chemical group 0.000 description 2
- 238000004891 communication Methods 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 2
- 230000009881 electrostatic interaction Effects 0.000 description 2
- 238000001125 extrusion Methods 0.000 description 2
- 239000000835 fiber Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 229910044991 metal oxide Inorganic materials 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 238000012216 screening Methods 0.000 description 2
- 235000011149 sulphuric acid Nutrition 0.000 description 2
- 239000001117 sulphuric acid Substances 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- 239000010457 zeolite Substances 0.000 description 2
- 229910000831 Steel Inorganic materials 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
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- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
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- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
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- 230000005684 electric field Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 229920001179 medium density polyethylene Polymers 0.000 description 1
- 239000004701 medium-density polyethylene Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 239000012466 permeate Substances 0.000 description 1
- 238000005554 pickling Methods 0.000 description 1
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- 230000005476 size effect Effects 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 229920006352 transparent thermoplastic Polymers 0.000 description 1
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- Carbon And Carbon Compounds (AREA)
Abstract
The application relates to the field of electromagnetic shielding materials, and particularly discloses an antistatic resin for an aluminum-plastic composite belt and a preparation method thereof, wherein the antistatic resin for the aluminum-plastic composite belt comprises the following substances in parts by weight: 100-120 parts of high-density polyethylene, 1-2 parts of maleic anhydride, 0.5-1.0 part of antioxidant 1010, 0.5-1.0 part of acrylic acid, 0.05-0.10 part of caprolactam, 1-2 parts of paraffin oil and 3-5 parts of antistatic modified particles; the antistatic modified particles are graphene aerogel particles. According to the application, the graphene aerogel particles are adopted as the antistatic modified particles, so that the antistatic performance of the resin of the aluminum-plastic composite belt is effectively improved, and the dispersion performance of the added graphene is improved, so that the antistatic performance of the resin for the aluminum-plastic composite belt is improved under the condition that the mechanical strength of a resin part is not reduced, and the problem of poor external electromagnetic field interference resistance of the aluminum-plastic composite belt is solved.
Description
Technical Field
The application relates to the field of electromagnetic shielding materials, in particular to an antistatic resin for an aluminum-plastic composite belt and a preparation method thereof.
Background
In recent years, due to the rapid development of optical fiber cables, the usage amount is more and more, but because the communication optical cable is always in a humid environment, the aluminum tape is easily oxidized and corroded, the stability of optical fiber transmission signals can be greatly influenced, the service life is reduced due to the corrosion of the aluminum tape for a long time, the optical fiber communication cost is improved, and the aluminum-plastic composite tape is produced. The aluminum-plastic composite tape mainly takes an aluminum tape as a framework, the upper surface and the lower surface of the aluminum tape are respectively heated and laminated by using a hot melt adhesive of an aluminum-plastic pipe, and an outer layer of the aluminum tape is wrapped by common medium-density polyethylene, so that the waterproof and oxygen-insulating performance of the optical fiber cable can be greatly improved, and the aluminum-plastic composite tape has the characteristics of good shielding effect, convenience in transportation, convenience in processing and the like.
The hot melt adhesive for the aluminum-plastic composite strip is mainly bonded by high-density polyethylene on the outer layer and an aluminum strip or a steel strip on the inner layer, the bonding process is mainly characterized in that a three-layer co-extrusion composite film is thermally bonded with the aluminum strip, and then the compounded aluminum strip and an outer layer extrusion pipe are synchronously pulled and coiled.
In view of the above-mentioned related technologies, the inventor believes that the outer sheath material high density polyethylene used in the existing aluminum-plastic composite tape is a semi-transparent thermoplastic resin with high crystallinity and non-polarity, which is difficult to be bonded by an adhesive at normal temperature, and in the actual use process, when a large amount of adhesive is needed for bonding, the prepared aluminum-plastic composite tape has poor capability of resisting external electromagnetic field interference, radio frequency interference and electric field coupling because of the addition of large amount of adhesive and poor antistatic performance.
Disclosure of Invention
In order to overcome the defect that the prepared aluminum-plastic composite belt has poor external electromagnetic field interference resistance due to poor antistatic performance of the resin for the aluminum-plastic composite belt, the application provides the antistatic resin for the aluminum-plastic composite belt, and the following technical scheme is adopted:
the antistatic resin for the aluminum-plastic composite belt comprises the following substances in parts by weight: 100-120 parts of high-density polyethylene, 1-2 parts of maleic anhydride, 0.5-1.0 part of antioxidant 1010, 0.5-1.0 part of acrylic acid, 0.05-0.10 part of caprolactam, 1-2 parts of paraffin oil and 3-5 parts of antistatic modified particles; the antistatic modified particles are graphene aerogel particles.
By adopting the technical scheme, as the graphene aerogel particles are adopted as the antistatic modified particles, the graphene particles are effectively dispersed in the resin material and are distributed on the surface of the high-density polyethylene resin in a sheet form and connected to form a conductive path so as to be connected into a complete conductive film layer, the dissipation of the internal and surface charges of the resin is accelerated, and the antistatic property of the resin for the aluminum-plastic composite belt is effectively improved, on the basis, the aerogel structure is adopted for adding, the phenomena caused by strong pi-pi stacking and van der Waals force action between two-dimensional graphene sheets after the traditional graphene is added are improved, the dispersing property of the resin for the aluminum-plastic composite belt after the graphene is added is improved through the formed three-dimensional porous network structure, so the antistatic property of the resin for the aluminum-plastic composite belt is improved under the condition that the mechanical strength of a resin part is not reduced, thereby improving the problem that the aluminum-plastic composite belt has poor performance of resisting the interference of an external electromagnetic field.
Further, the antistatic modified particles also comprise diatomite particles for coating and modifying the graphene aerogel.
Through adopting above-mentioned technical scheme, because this application adopts diatomaceous earth to be the load base member of graphite aerogel, on the one hand, the base member through the screening is with graphite aerogel effective dispersion and improve the antistatic properties of resin, on the other hand, the positive charge on the diatomaceous earth particle surface that the cladding has the aerogel and the marginal a large amount of negative charges can produce weaker positive negative charge electrostatic interaction with the anhydride group on the maleic anhydride, form stronger hydrogen bond structure, thereby combine the effective grafting of high density polyethylene and maleic anhydride and form three-dimensional cross-linked structural morphology, thereby improve combined material's mechanical strength.
Further, the graphene aerogel coated and modified diatomite particles are prepared by the following preparation method: (1) according to the mass ratio of 1: 5-8: 20-25, adding graphite oxide particles and polyvinylpyrrolidone into deionized water, stirring, mixing and performing ultrasonic dispersion treatment to obtain a dispersion suspension; (2) dropwise adding the dispersion suspension into an ammonia water solution with the mass fraction of 10% according to the mass ratio of 1:4, placing at 85-95 ℃, continuously stirring and mixing for 1-2 h, standing and cooling to room temperature to obtain a dispersion modified gel solution; (3) according to the mass ratio of 1: and 10, adding the diatomite particles into the dispersion modified gel liquid, carrying out heat preservation and pressurization treatment, carrying out centrifugal separation to obtain a lower layer precipitate, placing the lower layer precipitate in a nitrogen atmosphere for heat preservation and calcination, standing and cooling to room temperature, and crushing and grinding to obtain the graphene aerogel coated modified diatomite particles.
By adopting the technical scheme, as the polyvinylpyrrolidone with good film-forming property and coating property and water are combined to form a dispersed gel system, the graphite oxide particles are subjected to dispersion treatment to form a graphene structure, so that the graphene structure is effectively dispersed and forms gel, and an effective load is formed on the surface of diatomite to form a good coating structure.
Further, the diatomite is diatomite particles subjected to high-temperature calcination modification treatment.
Through adopting above-mentioned technical scheme, because this application is modified through carrying out high temperature calcination to diatomaceous earth, having got rid of its inside loaded zeolite water, adsorbed water and crystal water, the needle bar form fibre group of unordered structure in the messenger attapulgite structure becomes loose inflation to the pore volume and the specific surface area of attapulgite have been improved, like this, when in follow-up with aerogel load to the attapulgite, can effectively improve the quality of the graphite alkene of attapulgite load, improve antistatic effect, thereby improved the not good problem of aluminium-plastic composite band anti external electromagnetic field interference performance.
Further, the high-temperature calcination modification treatment comprises the following modification steps: (1) soaking kieselguhr into sulfuric acid for 25-30 min, washing and drying to obtain acid-washed particles; (2) and (3) placing the acid-washed particles in a muffle furnace, heating, carrying out heat preservation and calcination treatment, standing, cooling to room temperature, collecting dried particles, crushing and grinding to obtain modified matrix particles.
Through adopting above-mentioned technical scheme, because this application is through with diatomaceous earth through sulphuric acid pickling, dissolve metallic oxide through sulphuric acid, reduce metallic oxide internal impurity to improve the inside hole through rate of diatomaceous earth, on this basis, through high temperature calcination processing, thereby effectively improve the structural properties of diatomaceous earth, do good foreshadowing for subsequent load modification.
Further, the heat preservation and pressurization treatment in the step (3) is heat preservation and pressurization treatment for 3-5 hours at the temperature of 55-60 ℃ and under the pressure of 3-5 MPa.
Through adopting above-mentioned technical scheme, this application is carrying out the in-process of complex to graphite alkene aquogel and diatomaceous earth, through pressurization processing, has improved graphite alkene aquogel at the inside permeability of diatomaceous earth, makes graphite alkene payload to the inside hole of diatomaceous earth, and this scheme can not only improve the diatomaceous earth to the load of aerogel, and the graphite alkene granule that permeates into in the diatomaceous earth simultaneously can provide good support and cladding effect to the diatomaceous earth, makes the resin material of preparation have good mechanical properties.
In a second aspect, the present application provides a method for preparing an antistatic resin for an aluminum-plastic composite tape, wherein the preparation method comprises the steps of: s1, preparing the components according to the formula, weighing paraffin oil, antistatic modified particles, caprolactam, acrylic acid and maleic anhydride, placing the weighed components in a stirring device, stirring and mixing the components, mixing the components with high-density polyethylene, placing the mixture in a high-speed stirrer, and stirring and mixing the components to obtain a mixed material; s2, placing the mixed material in an internal mixer, carrying out internal mixing treatment to obtain an internal mixed material, placing the internal mixed material in a hot press, and carrying out hot press molding to obtain the antistatic resin for the aluminum-plastic composite belt.
By adopting the technical scheme, because the antistatic modifier is added in the preparation process of the grafted resin, the modified antistatic modifier has better dispersibility and has a one-dimensional nanometer size effect in the melt grafting of maleic anhydride, the reaction rate of free radicals can be improved, so that the grafting rate of the maleic anhydride is improved, and on the other hand, the modified antistatic modifier has good special micropore and mesoporous structures and can adsorb the free radicals, so that the self-crosslinking degree of the resin is reduced, the mechanical property and the antistatic property of the prepared aluminum-plastic composite belt are effectively improved, and the problem of poor external electromagnetic field interference resistance of the aluminum-plastic composite belt is solved.
Further, the banburying treatment in the step S2 is banburying treatment at 175-185 ℃ and a rotor speed of 35-40 r/min for 5-10 min.
Through adopting above-mentioned technical scheme, this application is through optimizing the temperature and the rotational speed of banburying processing, under this temperature and rotational speed, the resin of mixing can effectively melt and form the melt structure, through the effective rotation of rotor, improve the misce bene performance between each component, simultaneously through the rotation of rotor under this temperature, carry out effectual shearing treatment to the melt structure, make each component molecular chain constantly slide each other and the looks friction, thereby form homogeneous system's crosslinked structure, the problem that the compound anti external electromagnetic field interference performance of aluminium-plastic composite belt is not good has been improved.
In summary, the present application includes at least one of the following beneficial technical effects:
firstly, this application adopts graphite alkene aerogel granule to be antistatic modification granule, through inside graphite alkene granule effective dispersion at resin material, distribute on high density polyethylene resin surface and form the electrically conductive route with the form of slice, make the antistatic properties of aluminium-plastic composite tape resin effectively improve, on this basis, this application adopts aerogel structure to add, lead to the phenomenon of reunion after improving traditional graphite alkene and adding, thereby under the condition that does not reduce resin mechanical strength, the resin antistatic performance for the aluminium-plastic composite tape has been improved, thereby the not good problem of the anti external electromagnetic field interference performance of aluminium-plastic composite tape has been improved.
Second, this application adopts diatomaceous earth to be graphite aerogel's load base member, on the one hand, the base member through the screening is with graphite aerogel effective dispersion and improve the antistatic properties of resin, on the other hand, the positive charge on the diatomaceous earth particle surface that the cladding has the aerogel and the abundant negative charge in edge can produce less strong positive negative charge electrostatic interaction with the anhydride group on the maleic anhydride, form stronger hydrogen bond structure, thereby combine the effective grafting of high density polyethylene and maleic anhydride and form three-dimensional cross-linked structural morphology, thereby improve combined material's mechanical strength.
Third, this application adopts and to calcine the modification through carrying out high temperature to diatomaceous earth, has improved the pore volume and the specific surface area of attapulgite, like this, when follow-up loading aerogel to attapulgite, can effectively improve the quality of the graphite alkene of attapulgite load, improves antistatic effect to the problem that the anti external electromagnetic field interference performance of aluminum-plastic composite tape is not good has been improved.
Detailed Description
The present application will be described in further detail with reference to examples.
In the examples of the present application, the following instruments and apparatuses are used, but not limited thereto:
a machine: a universal tensile testing machine (CMT 4204, Shenzhen Meister);
a universal tensile testing machine (CMT 4204, Shenzhen Meister);
a high-impedance instrument.
Examples
Preparation example 1
Taking 5g of crystalline flake graphite particles, 2.5g of sodium nitrate and 10mL of sulfuric acid with the mass fraction of 90%, stirring and mixing at 0 ℃ to obtain a mixed solution, then dropwise adding 10g of a potassium permanganate solution with the mass fraction of 1% into the mixed solution, collecting a reaction solution after dropwise adding is finished, adding the reaction solution into a hydrogen peroxide solution with the mass fraction of 5% according to the volume ratio of 1:10, stirring, mixing, standing, taking a lower-layer precipitate, washing and drying to obtain graphite oxide particles;
preparation example 2
Taking 6g of crystalline flake graphite particles, 2.7g of sodium nitrate and 12mL of sulfuric acid with the mass fraction of 90%, placing the mixture at 2 ℃, stirring and mixing to obtain a mixed solution, then taking 12g of potassium permanganate solution with the mass fraction of 1% dropwise into the mixed solution, collecting a reaction solution after the dropwise addition is finished, adding the reaction solution into a hydrogen peroxide solution with the mass fraction of 5% according to the volume ratio of 1:10, stirring, mixing, standing, taking a lower-layer precipitate, washing and drying to obtain graphite oxide particles;
preparation example 3
Taking 6g of crystalline flake graphite particles, 2.7g of sodium nitrate and 12mL of sulfuric acid with the mass fraction of 90%, placing the mixture at 2 ℃, stirring and mixing to obtain a mixed solution, then taking 12g of potassium permanganate solution with the mass fraction of 1% dropwise into the mixed solution, collecting a reaction solution after the dropwise addition is finished, adding the reaction solution into a hydrogen peroxide solution with the mass fraction of 5% according to the volume ratio of 1:10, stirring, mixing, standing, taking a lower-layer precipitate, washing and drying to obtain graphite oxide particles;
example 1
Taking 5g of crystalline flake graphite particles, 2.5g of sodium nitrate and 10mL of sulfuric acid with the mass fraction of 90%, stirring and mixing at 0 ℃ to obtain a mixed solution, then dropwise adding 10g of a potassium permanganate solution with the mass fraction of 1% into the mixed solution, collecting a reaction solution after dropwise adding is finished, adding the reaction solution into a hydrogen peroxide solution with the mass fraction of 5% according to the volume ratio of 1:10, stirring, mixing, standing, taking a lower-layer precipitate, washing and drying to obtain graphite oxide particles;
according to the mass ratio of 1: 5: 20, adding graphite oxide particles and polyvinylpyrrolidone into deionized water, stirring, mixing, performing ultrasonic dispersion treatment at 200W for 25min to obtain a dispersed suspension, placing the dispersed suspension at 85 ℃, dropwise adding the dispersed suspension into an ammonia water solution with the mass fraction of 10% according to the mass ratio of 1:4, continuously stirring and mixing for 1h, standing, and cooling to room temperature to obtain a dispersed modified gel solution;
soaking kieselguhr into sulfuric acid with the mass fraction of 90%, soaking for 25min, washing and drying to obtain acid-washed particles, placing the kieselguhr into a muffle furnace, heating to 450 ℃ at the speed of 5 ℃/min, carrying out heat preservation and calcination treatment, standing and cooling to room temperature, collecting the dried particles, crushing and grinding, and sieving with a 200-mesh sieve to obtain modified matrix particles;
according to the mass ratio of 1:10, adding the modified matrix particles into the dispersion modified gel liquid, carrying out heat preservation and pressurization treatment for 3h at the temperature of 55 ℃ under the pressure of 3MPa, then carrying out centrifugal separation for 10min at the speed of 2500r/min to obtain a lower layer precipitate, placing the lower layer precipitate into a tubular atmosphere furnace, carrying out heat preservation and calcination for 3h at the temperature of 125 ℃ under the nitrogen atmosphere, standing and cooling to room temperature, crushing and grinding the lower layer precipitate and the tubular atmosphere furnace, and sieving the calcined lower layer precipitate by a 500-mesh sieve;
weighing 1mL of paraffin oil, 3g of modified particles, 0.5g of antioxidant 1010, 0.05g of caprolactam, 0.5g of acrylic acid and 1g of maleic anhydride, placing the mixture in a stirring device, stirring and mixing, collecting a mixed material, mixing the mixed material with 100g of high-density polyethylene, placing the mixture in a high-speed stirrer, stirring and mixing, placing the mixture in an internal mixer, carrying out internal mixing treatment for 5min at the temperature of 175 ℃ and the rotor rotation speed of 35r/min to obtain an internal mixed material, placing the internal mixed material in a hot press, and carrying out hot press molding at the temperature of 10MPa and 165 ℃ to obtain the antistatic resin for the aluminum-plastic composite belt.
Example 2
Taking 6g of crystalline flake graphite particles, 2.7g of sodium nitrate and 12mL of sulfuric acid with the mass fraction of 90%, placing the mixture at 2 ℃, stirring and mixing to obtain a mixed solution, then taking 12g of potassium permanganate solution with the mass fraction of 1% dropwise into the mixed solution, collecting a reaction solution after the dropwise addition is finished, adding the reaction solution into a hydrogen peroxide solution with the mass fraction of 5% according to the volume ratio of 1:10, stirring, mixing, standing, taking a lower-layer precipitate, washing and drying to obtain graphite oxide particles;
according to the mass ratio of 1: 6: 22, adding graphite oxide particles and polyvinylpyrrolidone into deionized water, stirring, mixing, placing under 250W, performing ultrasonic dispersion treatment for 27min to obtain a dispersion suspension, placing at 90 ℃, dropwise adding the dispersion suspension into an ammonia water solution with the mass fraction of 10% according to the mass ratio of 1:4, continuing stirring and mixing for 1h, standing, and cooling to room temperature to obtain a dispersion modified gel solution;
soaking kieselguhr into sulfuric acid with the mass fraction of 90%, soaking for 27min, washing and drying to obtain acid-washed particles, placing the kieselguhr into a muffle furnace, heating to 475 ℃ at the speed of 5 ℃/min, carrying out heat preservation and calcination treatment, standing and cooling to room temperature, collecting the dried particles, crushing and grinding, and sieving with a 200-mesh sieve to obtain modified matrix particles;
according to the mass ratio of 1:10, adding the modified matrix particles into the dispersion modified gel liquid, carrying out heat preservation and pressurization treatment for 4 hours at the temperature of 57 ℃ under the pressure of 4MPa, then carrying out centrifugal separation for 12 minutes at the speed of 2750r/min to obtain a lower layer precipitate, placing the lower layer precipitate into a tubular atmosphere furnace, carrying out heat preservation and calcination for 4 hours at the temperature of 127 ℃ under the nitrogen atmosphere, standing and cooling to room temperature, crushing and grinding the lower layer precipitate and 500-mesh modified particles to obtain modified particles;
weighing 1mL of paraffin oil, 4g of modified particles, 0.8g of antioxidant 1010, 0.08g of caprolactam, 0.8g of acrylic acid and 2g of maleic anhydride, placing the mixture in a stirring device, stirring and mixing, collecting a mixed material, mixing the mixed material with 110g of high-density polyethylene, placing the mixture in a high-speed stirrer, stirring and mixing, placing the mixture in an internal mixer, carrying out internal mixing treatment for 7min at 180 ℃ and 37r/min of rotor rotation speed to obtain an internal mixed material, placing the internal mixed material in a hot press, and carrying out hot press molding at 12MPa and 173 ℃ to obtain the antistatic resin for the aluminum-plastic composite belt.
Example 3
Taking 8g of crystalline flake graphite particles, 3.0g of sodium nitrate and 15mL of sulfuric acid with the mass fraction of 90%, stirring and mixing at 5 ℃ to obtain a mixed solution, then taking 15g of potassium permanganate solution with the mass fraction of 1% and dropwise adding the mixed solution into the mixed solution, collecting a reaction solution after dropwise adding is finished, adding the reaction solution into a hydrogen peroxide solution with the mass fraction of 5% according to the volume ratio of 1:10, stirring, mixing, standing, taking a lower-layer precipitate, washing and drying to obtain graphite oxide particles;
according to the mass ratio of 1: 8: 25, adding graphite oxide particles and polyvinylpyrrolidone into deionized water, stirring, mixing, placing under 300W, performing ultrasonic dispersion treatment for 30min to obtain a dispersion suspension, placing at 95 ℃, dropwise adding the dispersion suspension into an ammonia water solution with the mass fraction of 10% according to the mass ratio of 1:4, continuing stirring and mixing for 2h, standing, and cooling to room temperature to obtain a dispersion modified gel solution;
soaking kieselguhr into sulfuric acid with the mass fraction of 90%, soaking for 30min, washing and drying to obtain acid-washed particles, placing the kieselguhr into a muffle furnace, heating to 500 ℃ at the speed of 5 ℃/min, carrying out heat preservation and calcination treatment, standing and cooling to room temperature, collecting the dried particles, crushing and grinding, and sieving with a 200-mesh sieve to obtain modified matrix particles;
according to the mass ratio of 1:10, adding the modified matrix particles into the dispersion modified gel liquid, carrying out heat preservation and pressurization treatment for 4 hours at the temperature of 57 ℃ under the pressure of 5MPa, then carrying out centrifugal separation for 15 minutes at the speed of 2750r/min to obtain a lower layer precipitate, placing the lower layer precipitate into a tubular atmosphere furnace, carrying out heat preservation and calcination for 4 hours at the temperature of 137 ℃ under the nitrogen atmosphere, standing and cooling to room temperature, crushing and grinding the lower layer precipitate and 500-mesh modified particles to obtain modified particles;
weighing 2mL of paraffin oil, 5g of modified particles, 4g of antioxidant 1010, 0.10g of caprolactam, 1.0g of acrylic acid and 2g of maleic anhydride, placing the mixture in a stirring device, stirring and mixing, collecting the mixture, mixing the mixture with 120g of high-density polyethylene, placing the mixture in a high-speed stirrer, stirring and mixing, placing the mixture in an internal mixer, carrying out internal mixing treatment for 10min at 185 ℃ and the rotor rotation speed of 40r/min to obtain an internal mixed material, placing the internal mixed material in a hot press, and carrying out hot press molding at 15MPa and 180 ℃ to obtain the antistatic resin for the aluminum-plastic composite belt.
Examples 4 to 6
In examples 4 to 6, the graphene aerogel particles were used as antistatic agents, and the conditions and component ratios were the same as in examples 4 to 6 corresponding to examples 1 to 3, respectively.
Examples 7 to 9
In the embodiments 7 to 9, the graphene aerogel particles are coated on the surface of the diatomite to serve as the antistatic agent, and the conditions and the component ratios are the same as those in the embodiments 7 to 9 corresponding to the embodiments 1 to 3, respectively.
Performance test
The mechanical properties and the antistatic properties of the antistatic resins for aluminum-plastic composite tapes prepared in examples 1 to 9 were measured.
Detection method/test method
Mechanical properties: a dumbbell-type spline is prepared according to the GB/T1040-2006 standard by using an universal tensile testing machine (CMT 4204, Shenzhen Meister), and the tensile strength of the material is tested at the tensile rate of 100mm/min according to the spline size (the width: 4 +/-0.05 mm, the thickness: 1.00 +/-0.05 mm and the original gauge length: 20 +/-0.05 mm).
Shear and peel strength testing: the peel and shear strength tests were carried out using a universal tensile tester (CMT 4204, Shenzhen Messtand) in accordance with GB/T8808-1998, with a tensile rate of 300 mm/min. The test conditions were carried out at ambient temperature (25 ℃).
Antistatic performance: surface resistivity is measured using a high impedance meter with reference to GB 1410-2006. The specific test results are shown in table 1 below:
TABLE 1 EXAMPLES 1 TO 9 TEST TABLE FOR PERFORMANCE
Referring to the comparison of the performance tests of table 1, it can be found that:
the performances of the aluminum-plastic composite belt are compared in the examples 1 to 3, and the antistatic performance and the mechanical performance of the antistatic agent are gradually increased along with the increase of the components of the antistatic agent in the examples 1 to 3, which shows that the antistatic performance of the resin for the aluminum-plastic composite belt is improved by effectively dispersing the graphene particles in the resin material, so that the problem of poor external electromagnetic field interference resistance of the aluminum-plastic composite belt is solved.
Comparing the performances of the embodiment 1 and the embodiments 4 to 6, because the graphene aerogel particles are used as the antistatic agent in the embodiments 4 to 6, and the antistatic performance and the tensile strength of the graphene aerogel particles are reduced, the application shows that the graphene oxide particles are dispersed to form a graphene structure by combining polyvinylpyrrolidone with good film forming performance and coating performance and forming a gel, so that the graphene oxide particles are effectively dispersed and formed into the gel, the antistatic performance of the resin for the aluminum-plastic composite belt is improved, and the problem of poor external electromagnetic field interference resistance of the aluminum-plastic composite belt is solved.
Comparing the performance of the embodiment 1 with that of the embodiments 7 to 9, the graphene aerogel particles are coated on the surface of the diatomite to serve as the antistatic agent in the embodiments 7 to 9, and the antistatic performance and the tensile strength of the diatomite are both slightly reduced, which indicates that the antistatic performance and the mechanical strength of the resin can be effectively improved by using the diatomite as the load matrix of the graphite aerogel.
Comparative example
Comparative examples 1 to 3
The comparative examples 1 to 3 were prepared using carbon nanotubes as antistatic agents, and the conditions and component ratios were the same as in comparative examples 1 to 3 corresponding to examples 1 to 3, respectively.
Comparative examples 4 to 6
In comparative examples 4 to 6, carbon nanotubes supported on attapulgite were used as antistatic agents, and the conditions and component ratios were the same as in comparative examples 4 to 6 corresponding to examples 1 to 3, respectively.
Comparative examples 7 to 9
In comparative examples 7 to 9, attapulgite was used instead of diatomaceous earth used in the present application to prepare antistatic agents, which were the same as in comparative examples 7 to 9 corresponding to examples 1 to 3, respectively, except for the same conditions and component ratios.
And respectively detecting the mechanical property and the antistatic property of the antistatic resin for the aluminum-plastic composite belt prepared in the comparative examples 1-9.
Detection method/test method
Mechanical properties: a dumbbell-type spline is prepared according to the GB/T1040-2006 standard by using an universal tensile testing machine (CMT 4204, Shenzhen Meister), and the tensile strength of the material is tested at the tensile rate of 100mm/min according to the spline size (the width: 4 +/-0.05 mm, the thickness: 1.00 +/-0.05 mm and the original gauge length: 20 +/-0.05 mm).
Shear and peel strength testing: the peel and shear strength tests were carried out using a universal tensile tester (CMT 4204, Shenzhen Messtand) in accordance with GB/T8808-1998, with a tensile rate of 300 mm/min. The test conditions were carried out at ambient temperature (25 ℃).
Antistatic performance: surface resistivity is measured using a high impedance meter with reference to GB 1410-2006. The specific test results are shown in table 2 below:
TABLE 2 comparative examples 1-9 Performance test Table
Referring to the comparison of the performance tests of table 2, it can be found that:
comparing the comparative examples 1-3 with the examples 1-3, the carbon nano tube is adopted as the antistatic agent in the comparative examples 1-3 for preparation, and the performance of the graphene aerogel particles is poorer than that of the examples 1-3, which shows that the graphene aerogel particles adopted in the application are antistatic modified particles, the phenomenon that agglomeration is caused by strong pi-pi stacking and van der waals force action between two-dimensional graphene sheet layers after the traditional graphene is added is improved, so that the antistatic performance of the resin for the aluminum-plastic composite belt is improved under the condition that the mechanical strength of a resin part is not reduced, and the problem that the external electromagnetic field interference resistance of the aluminum-plastic composite belt is poor is solved.
Comparing comparative examples 4-6 with examples 1-3, the carbon nano tube loaded on the attapulgite is adopted as the antistatic agent in the comparative examples 4-6, and the mechanical property and the antistatic property are obviously reduced, which shows that the diatomite is subjected to high-temperature calcination modification, zeolite water, adsorbed water and crystal water loaded in the diatomite are removed, and needle-rod-shaped fiber groups with disordered structures in the attapulgite structure become loose and expand, so that the pore volume and the specific surface area of the attapulgite are improved, and the problem of poor external electromagnetic field interference resistance of the aluminum-plastic composite belt is solved.
Compare this application comparative example 7 ~ 9 respectively with embodiment 1 ~ 3 in proper order, comparative example 7 ~ 9 adopt the attapulgite to replace the diatomaceous earth that this application adopted to prepare antistatic agent in the preparation process, and its mechanical properties and antistatic properties decline to some extent, this shows that this application adopts diatomaceous earth to be the load base member of graphite aerogel, and effective dispersion graphite alkene aerogel has improved the antistatic properties and the mechanical strength of resin.
The present embodiment is only for explaining the present application, and it is not limited to the present application, and those skilled in the art can make modifications of the present embodiment without inventive contribution as needed after reading the present specification, but all of them are protected by patent law within the scope of the claims of the present application.
Claims (8)
1. The antistatic resin for the aluminum-plastic composite belt is characterized by comprising the following components in parts by weight:
100-120 parts of high-density polyethylene;
1-2 parts of maleic anhydride;
10100.5-1.0 part of antioxidant;
0.5-1.0 part of acrylic acid;
0.05-0.10 part of caprolactam;
1-2 parts of paraffin oil;
3-5 parts of antistatic modified particles; the antistatic modified particles are graphene aerogel particles.
2. The antistatic resin for the aluminum-plastic composite belt as claimed in claim 1, wherein the antistatic modified particles further comprise diatomite particles for graphene aerogel coating modification.
3. The antistatic resin for the aluminum-plastic composite belt according to claim 2, wherein the graphene aerogel coated and modified diatomite particles are prepared by the following preparation method:
(1) according to the mass ratio of 1: 5-8: 20-25, adding graphite oxide particles and polyvinylpyrrolidone into deionized water, stirring, mixing and performing ultrasonic dispersion treatment to obtain a dispersion suspension;
(2) dropwise adding the dispersion suspension into an ammonia water solution with the mass fraction of 10% according to the mass ratio of 1:4, placing at 85-95 ℃, continuously stirring and mixing for 1-2 h, standing and cooling to room temperature to obtain a dispersion modified gel solution;
(3) according to the mass ratio of 1: and 10, adding the diatomite particles into the dispersion modified gel liquid, carrying out heat preservation and pressurization treatment, carrying out centrifugal separation to obtain a lower layer precipitate, placing the lower layer precipitate in a nitrogen atmosphere for heat preservation and calcination, standing and cooling to room temperature, and crushing and grinding to obtain the graphene aerogel coated modified diatomite particles.
4. The antistatic resin for aluminum-plastic composite belts as claimed in claim 2, wherein the diatomaceous earth is modified by high temperature calcination.
5. The antistatic resin for aluminum-plastic composite belts as claimed in claim 4, wherein the high-temperature calcination modification treatment comprises the following modification steps:
(1) soaking kieselguhr into sulfuric acid for 25-30 min, washing and drying to obtain acid-washed particles;
(2) and (3) placing the acid-washed particles in a muffle furnace, heating, carrying out heat preservation and calcination treatment, standing, cooling to room temperature, collecting dried particles, crushing and grinding to obtain modified matrix particles.
6. The antistatic resin for the aluminum-plastic composite belt as claimed in claim 3, wherein the heat-preservation pressure treatment in the step (3) is heat-preservation pressure treatment at 55-60 ℃ under 3-5 MPa for 3-5 h.
7. The preparation method of the antistatic resin for the aluminum-plastic composite belt according to any one of claims 1 to 6, wherein the preparation step comprises:
s1, preparing the components according to the formula, weighing paraffin oil, antistatic modified particles, caprolactam, acrylic acid and maleic anhydride, placing the weighed components in a stirring device, stirring and mixing the components, mixing the components with high-density polyethylene, placing the mixture in a high-speed stirrer, and stirring and mixing the components to obtain a mixed material;
s2, placing the mixed material in an internal mixer, carrying out internal mixing treatment to obtain an internal mixed material, placing the internal mixed material in a hot press, and carrying out hot press molding to obtain the antistatic resin for the aluminum-plastic composite belt.
8. The method of claim 7, wherein the banburying treatment in step S2 is carried out at 175-185 ℃ and 35-40 r/min of rotor speed for 5-10 min.
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Application publication date: 20210416 |