CN115584083B - Wave-absorbing polypropylene foaming bead and preparation method thereof - Google Patents
Wave-absorbing polypropylene foaming bead and preparation method thereof Download PDFInfo
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- CN115584083B CN115584083B CN202211312481.0A CN202211312481A CN115584083B CN 115584083 B CN115584083 B CN 115584083B CN 202211312481 A CN202211312481 A CN 202211312481A CN 115584083 B CN115584083 B CN 115584083B
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- -1 polypropylene Polymers 0.000 title claims abstract description 96
- 239000004743 Polypropylene Substances 0.000 title claims abstract description 95
- 229920001155 polypropylene Polymers 0.000 title claims abstract description 95
- 238000005187 foaming Methods 0.000 title claims abstract description 57
- 239000011324 bead Substances 0.000 title claims abstract description 55
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 239000002131 composite material Substances 0.000 claims abstract description 35
- 239000004594 Masterbatch (MB) Substances 0.000 claims abstract description 25
- 239000011347 resin Substances 0.000 claims abstract description 19
- 229920005989 resin Polymers 0.000 claims abstract description 19
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 claims abstract description 16
- 238000010521 absorption reaction Methods 0.000 claims abstract description 9
- 238000002156 mixing Methods 0.000 claims abstract description 6
- 239000012752 auxiliary agent Substances 0.000 claims description 34
- 239000000843 powder Substances 0.000 claims description 19
- 239000002270 dispersing agent Substances 0.000 claims description 11
- 239000000314 lubricant Substances 0.000 claims description 11
- 238000000034 method Methods 0.000 claims description 11
- 239000002667 nucleating agent Substances 0.000 claims description 11
- 239000004014 plasticizer Substances 0.000 claims description 11
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 10
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims description 9
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 8
- 239000002904 solvent Substances 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 7
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 6
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 6
- 150000001879 copper Chemical class 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 6
- 229910052786 argon Inorganic materials 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
- 229910052757 nitrogen Inorganic materials 0.000 claims description 5
- OZAIFHULBGXAKX-UHFFFAOYSA-N 2-(2-cyanopropan-2-yldiazenyl)-2-methylpropanenitrile Chemical compound N#CC(C)(C)N=NC(C)(C)C#N OZAIFHULBGXAKX-UHFFFAOYSA-N 0.000 claims description 4
- 239000004156 Azodicarbonamide Substances 0.000 claims description 4
- XOZUGNYVDXMRKW-AATRIKPKSA-N azodicarbonamide Chemical compound NC(=O)\N=N\C(N)=O XOZUGNYVDXMRKW-AATRIKPKSA-N 0.000 claims description 4
- 235000019399 azodicarbonamide Nutrition 0.000 claims description 4
- FLKPEMZONWLCSK-UHFFFAOYSA-N diethyl phthalate Chemical compound CCOC(=O)C1=CC=CC=C1C(=O)OCC FLKPEMZONWLCSK-UHFFFAOYSA-N 0.000 claims description 4
- VJHINFRRDQUWOJ-UHFFFAOYSA-N dioctyl sebacate Chemical compound CCCCC(CC)COC(=O)CCCCCCCCC(=O)OCC(CC)CCCC VJHINFRRDQUWOJ-UHFFFAOYSA-N 0.000 claims description 4
- FPAFDBFIGPHWGO-UHFFFAOYSA-N dioxosilane;oxomagnesium;hydrate Chemical compound O.[Mg]=O.[Mg]=O.[Mg]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O FPAFDBFIGPHWGO-UHFFFAOYSA-N 0.000 claims description 4
- 239000002994 raw material Substances 0.000 claims description 4
- 235000012239 silicon dioxide Nutrition 0.000 claims description 4
- 239000000377 silicon dioxide Substances 0.000 claims description 4
- WXMKPNITSTVMEF-UHFFFAOYSA-M sodium benzoate Chemical compound [Na+].[O-]C(=O)C1=CC=CC=C1 WXMKPNITSTVMEF-UHFFFAOYSA-M 0.000 claims description 4
- 239000004299 sodium benzoate Substances 0.000 claims description 4
- 235000010234 sodium benzoate Nutrition 0.000 claims description 4
- 239000001569 carbon dioxide Substances 0.000 claims description 3
- 229910002092 carbon dioxide Inorganic materials 0.000 claims description 3
- STXKJSYMVDTOSJ-UHFFFAOYSA-M chlorocopper hexahydrate Chemical compound [Cu]Cl.O.O.O.O.O.O STXKJSYMVDTOSJ-UHFFFAOYSA-M 0.000 claims description 3
- 238000001914 filtration Methods 0.000 claims description 3
- 239000007789 gas Substances 0.000 claims description 3
- 239000000155 melt Substances 0.000 claims description 3
- 238000004321 preservation Methods 0.000 claims description 3
- 238000001291 vacuum drying Methods 0.000 claims description 3
- PMDHMYFSRFZGIO-UHFFFAOYSA-N 1,4,7-trioxacyclotridecane-8,13-dione Chemical compound O=C1CCCCC(=O)OCCOCCO1 PMDHMYFSRFZGIO-UHFFFAOYSA-N 0.000 claims description 2
- ZFFMLCVRJBZUDZ-UHFFFAOYSA-N 2,3-dimethylbutane Chemical group CC(C)C(C)C ZFFMLCVRJBZUDZ-UHFFFAOYSA-N 0.000 claims description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 2
- ZJCCRDAZUWHFQH-UHFFFAOYSA-N Trimethylolpropane Chemical compound CCC(CO)(CO)CO ZJCCRDAZUWHFQH-UHFFFAOYSA-N 0.000 claims description 2
- JZCCFEFSEZPSOG-UHFFFAOYSA-L copper(II) sulfate pentahydrate Chemical compound O.O.O.O.O.[Cu+2].[O-]S([O-])(=O)=O JZCCFEFSEZPSOG-UHFFFAOYSA-L 0.000 claims description 2
- SXTLQDJHRPXDSB-UHFFFAOYSA-N copper;dinitrate;trihydrate Chemical compound O.O.O.[Cu+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O SXTLQDJHRPXDSB-UHFFFAOYSA-N 0.000 claims description 2
- 229940106012 diethylene glycol adipate Drugs 0.000 claims description 2
- 238000007599 discharging Methods 0.000 claims description 2
- 238000001125 extrusion Methods 0.000 claims description 2
- 239000011159 matrix material Substances 0.000 claims description 2
- 239000010445 mica Substances 0.000 claims description 2
- 229910052618 mica group Inorganic materials 0.000 claims description 2
- 238000006116 polymerization reaction Methods 0.000 claims description 2
- 230000000630 rising effect Effects 0.000 claims description 2
- 239000007787 solid Substances 0.000 claims description 2
- 230000002745 absorbent Effects 0.000 abstract description 13
- 239000002250 absorbent Substances 0.000 abstract description 13
- 239000010949 copper Substances 0.000 abstract description 9
- 239000011358 absorbing material Substances 0.000 abstract description 4
- 239000000805 composite resin Substances 0.000 abstract description 3
- 229910052982 molybdenum disulfide Inorganic materials 0.000 abstract description 3
- VYFYYTLLBUKUHU-UHFFFAOYSA-N dopamine Chemical compound NCCC1=CC=C(O)C(O)=C1 VYFYYTLLBUKUHU-UHFFFAOYSA-N 0.000 abstract 4
- 229960003638 dopamine Drugs 0.000 abstract 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 abstract 1
- 239000011248 coating agent Substances 0.000 abstract 1
- 238000000576 coating method Methods 0.000 abstract 1
- 229910052802 copper Inorganic materials 0.000 abstract 1
- 239000011858 nanopowder Substances 0.000 abstract 1
- 238000007747 plating Methods 0.000 abstract 1
- 239000000463 material Substances 0.000 description 14
- 230000000052 comparative effect Effects 0.000 description 8
- 238000012360 testing method Methods 0.000 description 7
- 230000001276 controlling effect Effects 0.000 description 5
- 239000000203 mixture Substances 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 238000005491 wire drawing Methods 0.000 description 3
- IAYPIBMASNFSPL-UHFFFAOYSA-N Ethylene oxide Chemical compound C1CO1 IAYPIBMASNFSPL-UHFFFAOYSA-N 0.000 description 2
- WNLRTRBMVRJNCN-UHFFFAOYSA-L adipate(2-) Chemical compound [O-]C(=O)CCCCC([O-])=O WNLRTRBMVRJNCN-UHFFFAOYSA-L 0.000 description 2
- 238000004891 communication Methods 0.000 description 2
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- VVWRJUBEIPHGQF-UHFFFAOYSA-N propan-2-yl n-propan-2-yloxycarbonyliminocarbamate Chemical compound CC(C)OC(=O)N=NC(=O)OC(C)C VVWRJUBEIPHGQF-UHFFFAOYSA-N 0.000 description 2
- CTENFNNZBMHDDG-UHFFFAOYSA-N Dopamine hydrochloride Chemical compound Cl.NCCC1=CC=C(O)C(O)=C1 CTENFNNZBMHDDG-UHFFFAOYSA-N 0.000 description 1
- PWKWDCOTNGQLID-UHFFFAOYSA-N [N].[Ar] Chemical compound [N].[Ar] PWKWDCOTNGQLID-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- AGXUVMPSUKZYDT-UHFFFAOYSA-L barium(2+);octadecanoate Chemical compound [Ba+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O AGXUVMPSUKZYDT-UHFFFAOYSA-L 0.000 description 1
- CJZGTCYPCWQAJB-UHFFFAOYSA-L calcium stearate Chemical compound [Ca+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O CJZGTCYPCWQAJB-UHFFFAOYSA-L 0.000 description 1
- 235000013539 calcium stearate Nutrition 0.000 description 1
- 239000008116 calcium stearate Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000007123 defense Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 229960001149 dopamine hydrochloride Drugs 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000006260 foam Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 238000000643 oven drying Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 238000009210 therapy by ultrasound Methods 0.000 description 1
- LENZDBCJOHFCAS-UHFFFAOYSA-N tris Chemical compound OCC(N)(CO)CO LENZDBCJOHFCAS-UHFFFAOYSA-N 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- XOOUIPVCVHRTMJ-UHFFFAOYSA-L zinc stearate Chemical compound [Zn+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O XOOUIPVCVHRTMJ-UHFFFAOYSA-L 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/04—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent
- C08J9/06—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a chemical blowing agent
- C08J9/10—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a chemical blowing agent developing nitrogen, the blowing agent being a compound containing a nitrogen-to-nitrogen bond
- C08J9/102—Azo-compounds
- C08J9/103—Azodicarbonamide
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/0095—Mixtures of at least two compounding ingredients belonging to different one-dot groups
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/04—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent
- C08J9/06—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a chemical blowing agent
- C08J9/10—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a chemical blowing agent developing nitrogen, the blowing agent being a compound containing a nitrogen-to-nitrogen bond
- C08J9/102—Azo-compounds
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
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- C09K3/00—Materials not provided for elsewhere
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- C08J2203/00—Foams characterized by the expanding agent
- C08J2203/04—N2 releasing, ex azodicarbonamide or nitroso compound
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- C08J2323/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
- C08J2323/02—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers not modified by chemical after treatment
- C08J2323/10—Homopolymers or copolymers of propene
- C08J2323/12—Polypropene
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Abstract
The invention discloses a wave-absorbing polypropylene foaming bead and a preparation method thereof. Firstly, coating molybdenum disulfide nano powder with dopamine, and then chemically plating metallic copper on a dopamine/molybdenum disulfide composite material to obtain a composite absorbent capable of realizing efficient microwave absorption; mixing and extruding the composite absorbent and polypropylene resin through a double-screw extruder to obtain composite resin master batch with wave absorbing performance; and foaming the composite master batch twice to obtain the wave-absorbing polypropylene foaming beads. The polypropylene composite beads subjected to secondary foaming not only have excellent microwave absorption performance, but also have lower bulk density, meet the new requirements of the novel wave-absorbing material on thinness, light weight, wide width and strong strength, and have wide application prospects in the novel composite material.
Description
Technical Field
The invention relates to a wave-absorbing polypropylene foaming bead and a preparation method thereof, belonging to the field of wave-absorbing materials.
Background
At present, the progress of electronic science and technology greatly changes the life of people, brings great pollution influence on the health while bringing convenience to the life of people, and electromagnetic pollution is already identified as the fourth pollution source in the world, so that the problem of electromagnetic pollution becomes a research hotspot in various countries in the world in recent years. However, with the progress of the electronic communication industry, the equipment is miniaturized and has a higher power, and the requirements for materials are also increasing. The wave absorbing material is also light, and the matching thickness is thinner, and the absorption bandwidth is wider.
The polypropylene resin has the characteristics of light weight, excellent acid and alkali resistance, high cost performance and the like, the weight of the foamed material obtained by foaming the polypropylene can be greatly reduced, the foamed polypropylene can be recycled, and the production efficiency is improved. Meanwhile, the hole structure in the foamed polypropylene can reflect electromagnetic waves incident into the material, so that the impedance matching degree of the material is improved, and the effect of absorbing electromagnetic waves in a broadband is achieved. However, development of efficient absorbent and matching degree of foamed polypropylene pore structure to electromagnetic wave still have some application problems, and on the basis of existing problems and challenges, the method has important practical significance for solving the problems of microscopic performance regulation of the absorbent and influence of foamed material pore structure to electromagnetic parameters.
Disclosure of Invention
The invention aims to provide a wave-absorbing polypropylene foaming bead and a preparation method thereof.
The wave-absorbing polypropylene foaming bead provided by the invention is prepared from the following raw materials in parts by mass:
60-70 parts of polypropylene resin, 25-30 parts of wave-absorbing powder and 10 parts of auxiliary agent;
the wave-absorbing powder is the chemically modified molybdenum disulfide provided by the invention.
In the wave-absorbing polypropylene foaming beads, the density of the polypropylene resin matrix is 0.85-0.95g/cm 3 The method comprises the steps of carrying out a first treatment on the surface of the Specifically 0.9g/cm 3 ；
The melt index is 90-100g/10min;
the auxiliary agent consists of a plasticizer, a nucleating agent, a foaming auxiliary agent and a lubricant;
each auxiliary agent accounts for 5% -35% of the total weight of the auxiliary agents;
specifically, the plasticizer accounts for 30% of the total weight of the auxiliary agent, the nucleating agent accounts for 30% of the total weight of the auxiliary agent, the foaming auxiliary agent accounts for 30% of the total weight of the auxiliary agent, and the lubricant accounts for 10% of the total weight of the auxiliary agent.
Specifically, the plasticizer is at least one selected from di (2-ethylhexyl) sebacate, di (2-ethyl) phthalate and diethylene glycol adipate;
the nucleating agent is at least one selected from talcum powder, silicon dioxide, mica and sodium benzoate;
the foaming auxiliary agent is at least one selected from azodicarbonamide, azodiisobutyronitrile and diisopropyl azodicarbonate;
the lubricant is at least one selected from the group consisting of trimethylolpropane and stearate; the stearate is specifically selected from at least one of zinc stearate, calcium stearate and barium stearate;
the wave-absorbing polypropylene foaming beads also contain a dispersing agent;
the mass ratio of the dispersing agent to the polypropylene composite master batch is 0.5-1:8-10; specifically 0.5:8.5;
the dispersant is specifically an adduct of an industrial alkyl phenol and ethylene oxide.
Specifically, the wave-absorbing polypropylene foaming beads are prepared from the following raw materials in parts by mass:
70 parts of polypropylene resin, 20 parts of wave-absorbing powder and 10 parts of auxiliary agent; or,
65 parts of polypropylene resin, 25 parts of wave-absorbing powder and 10 parts of auxiliary agent; or,
60 parts of polypropylene resin, 30 parts of wave-absorbing powder and 10 parts of auxiliary agent.
The auxiliary agent can be specifically composed of the following auxiliary agents:
auxiliary agent I: the weight content of the plasticizer of the di (2-ethylhexyl) sebacate is 30 percent, the weight content of the nucleating agent of the talcum powder is 30 percent, the weight content of the foaming auxiliary agent of the azodicarbonamide is 30 percent, and the weight content of the lubricant stearate is 10 percent;
auxiliary II: the weight content of plasticizer di (2-ethyl) phthalate is 30%, the weight content of nucleating agent silicon dioxide is 30%, the weight content of foaming auxiliary agent azodiisobutyronitrile is 30%, and the weight content of lubricant stearate is 10%;
auxiliary III: the weight content of the plasticizer diglycol adipate is 30%, the weight content of the nucleating agent sodium benzoate is 30%, the weight content of the foaming auxiliary diisopropyl azodicarboxylate is 30%, and the weight content of the lubricant stearate is 10%.
The chemically modified molybdenum disulfide is a product obtained according to the following steps:
copper salt and PDA/MoS 2 Dissolving in solvent, stirring, filtering, collecting solid, drying, and treating at high temperature.
Specifically, the copper salt is at least one selected from copper chloride hexahydrate, copper nitrate trihydrate and copper sulfate pentahydrate;
the solvent is at least one selected from deionized water, absolute ethyl alcohol and ethylene glycol;
the copper salt, PDA/MoS 2 The mass ratio of the solvent to the solvent is 1:2-4:15-17;
in the stirring step, the rotating speed is 150-400rpm; specifically, 200 rpm and 300rpm; the time is 4-8 hours; specifically 6 hours;
in the drying step, the drying mode is vacuum drying; the time is 8-14h; specifically, 12 hours;
in the high-temperature treatment step, the atmosphere is a mixed atmosphere consisting of nitrogen and argon; the flow rate ratio of the nitrogen to the argon is 1:2-4; the method specifically comprises the following steps of 1:3, a step of;
the temperature is 700-900 ℃; specifically 800 ℃; the time is 2-4h; specifically for 2 hours; the temperature rising rate from room temperature to high temperature treatment temperature is 2-3 ℃/min.
The application of the chemically modified molybdenum disulfide in wave absorption or wave absorption powder belongs to the protection scope of the invention.
The method for preparing the wave-absorbing polypropylene foaming beads provided by the invention comprises the following steps:
1) Mixing the polypropylene resin, the wave-absorbing powder and the auxiliary agent according to the mass ratio, and extruding to obtain polypropylene composite master batch;
2) Putting water, a dispersing agent and the polypropylene composite master batch into an autoclave, introducing carbon dioxide gas, heating the autoclave, controlling the temperature to 160-170 ℃ and the pressure to 1.5-2.0 MPa, and performing heat preservation and pressure maintaining for 3-10min (specifically, 5 min) and then performing pressure relief to obtain polypropylene primary foaming polymerization beads;
3) And adding the polypropylene primary foaming beads into an autoclave, introducing high-pressure air, keeping the pressure at 0.2-0.5MPa (specifically 0.4 MPa), maintaining the pressure for 8-12h, and then decompressing to obtain the wave-absorbing polypropylene foaming beads.
Step 1) of the above method, the aspect ratio of the twin-screw extruder used in the extrusion step was 20:1, the rotating speed is 60-120r/min;
the temperature of the twin-screw extruder from the feeding end to the discharging end is set to be 150-180 ℃ in a first zone, 160-230 ℃ in a second zone, 160-280 ℃ in a third zone, 170-290 ℃ in a fourth zone, 200-300 ℃ in a fifth zone, 200-330 ℃ in a sixth zone and 200-350 ℃ in a seventh zone;
specifically, the temperature is set as:
the first zone is 150 ℃, the second zone is 160 ℃, the third zone is 160 ℃, the fourth zone is 170 ℃, the fifth zone is 200 ℃, the sixth zone is 200 ℃, and the seventh zone is 200 ℃; or alternatively, the first and second heat exchangers may be,
the first zone 150 ℃, the second zone 170 ℃, the third zone 170 ℃, the fourth zone 175 ℃, the fifth zone 200 ℃, the sixth zone 200 ℃, and the seventh zone 205 ℃; or alternatively, the first and second heat exchangers may be,
the first zone 150 ℃, the second zone 170 ℃, the third zone 170 ℃, the fourth zone 180 ℃, the fifth zone 205 ℃, the sixth zone 210 ℃, and the seventh zone 210 ℃;
in the step 2), the mass ratio of water, the dispersing agent and the polypropylene composite master batch is 1:0.5-1:8-10; specifically 1:0.5:8.5.
In addition, the application of the wave-absorbing polypropylene foaming beads provided by the invention in microwave absorption and the application of the wave-absorbing polypropylene foaming beads in the preparation of microwave absorption products also belong to the protection scope of the invention.
The invention provides a wave-absorbing polypropylene foaming bead and a preparation method thereof, wherein a chemical combination method is utilized to develop and verify a high-efficiency microwave absorbent, and then the composite absorbent and polypropylene resin are mixed and extruded by a double-screw extruder to obtain a composite resin master batch with wave-absorbing performance; and foaming the composite master batch twice to obtain the wave-absorbing polypropylene foaming beads. The polypropylene composite beads subjected to secondary foaming not only have excellent microwave absorption performance, but also have lower bulk density, and have important application values in the fields of communication, vehicle-mounted radar and national defense.
Drawings
FIG. 1 shows the wave-absorbing properties of comparative examples 1-2 of examples 1-3.
Detailed Description
The invention will be further illustrated with reference to the following specific examples, but the invention is not limited to the following examples. The methods are conventional methods unless otherwise specified. The starting materials are available from published commercial sources unless otherwise specified.
The dispersant used in the examples below was an adduct of an industrial alkylphenol with ethylene oxide (product number NP-9, available from Henan Wakasi Biotechnology Co., ltd.).
Example 1
The example provides a wave-absorbing polypropylene foam bead, the raw material composition is that the density is 0.9g/cm 3 70 parts of polypropylene resin with the melt index of 100g/10min, 20 parts of wave-absorbing powder and 10 parts of auxiliary agent. Wherein the weight content of the plasticizer of the di (2-ethylhexyl) sebacate is 30 percent, the weight content of the nucleating agent of the talcum powder is 30 percent, the weight content of the foaming auxiliary agent of the azodicarbonamide is 30 percent, and the weight content of the lubricant of the stearate is 10 percent.
The wave-absorbing polypropylene foaming bead and the preparation method thereof comprise the following steps:
step one, PDA/MoS 2 Is prepared from the following steps:
according to parts by weight, dissolving 20 parts of commercial molybdenum disulfide nano particles by 70 parts of deionized water at a certain temperature, regulating the rotating speed of a stirrer to 150-400rpm, stirring for 15min, and carrying out ultrasonic treatment for 2h; after the dissolution is completed, 7 parts of dopamine hydrochloride and 3 parts of tris (hydroxymethyl) aminomethane are added into the mixture, and the mixture is stirred to disperse powder, and the pH value of the aqueous solution is kept to be about 8.5; stirring the solution for 8h, centrifugally washing the solution with deionized water for three times, and putting the solution into an ovenDrying overnight to obtain PDA/MoS 2 A powder;
step two, the wave-absorbing powder material provided by the invention is chemically modified molybdenum disulfide Cu/PDA/MoS 2 Is prepared from the following steps:
in parts by weight, 5 parts of copper chloride hexahydrate and 10 parts of PDA/MoS are used at a certain temperature 2 Dissolving in 85 parts deionized water, stirring at 150-400rpm (such as 300 rpm) for 6 hr, filtering at 60deg.C, vacuum drying for 12 hr, heating to 800deg.C at a heating rate of 2deg.C/min in a nitrogen-argon mixed atmosphere (flow rate ratio of nitrogen to argon is 1:3), and maintaining for 2 hr to obtain Cu/PDA/MoS 2 The composite absorbent is the chemically modified molybdenum disulfide provided by the invention;
step three, preparing polypropylene composite wave-absorbing master batch:
10 parts of auxiliary agent and 20 parts of Cu/PDA/MoS are added in parts by weight 2 Adding a composite absorbent (namely wave-absorbing powder-chemically modified molybdenum disulfide) and 70 parts of polypropylene resin into a mixer, and uniformly mixing to obtain a mixed material; adding the mixed materials into a double-screw extruder (length-diameter ratio is 20:1) for wiredrawing and granulating to obtain polypropylene composite wave-absorbing master batch, and controlling the temperature and screw rotating speed of each region, wherein the temperature of the first region is 150 ℃, the temperature of the second region is 160 ℃, the temperature of the third region is 160 ℃, the temperature of the fourth region is 170 ℃, the temperature of the fifth region is 200 ℃, the temperature of the sixth region is 200 ℃, the temperature of the seventh region is 200 ℃, and the screw rotating speed is 60-120r/min;
step four, preparing polypropylene primary foaming beads:
adding 10 parts of water, 5 parts of dispersing agent and 85 parts of polypropylene composite master batch obtained in the steps into an autoclave, introducing carbon dioxide gas, heating the autoclave, controlling the temperature to 160-170 ℃ and the pressure to 1.5-2.0 mpa, and releasing the pressure of the autoclave after heat preservation and pressure maintaining for 5min to obtain polypropylene primary foaming polymeric beads;
step five, preparing polypropylene secondary foaming beads:
adding the primary foaming beads obtained in the step four into a pressure kettle, introducing high-pressure air, keeping the pressure at 0.4Mpa, and performing pressure maintaining for 10 hours to obtain secondary foaming beads with lower density, namely the wave-absorbing polypropylene foaming beads provided by the invention.
Example 2
The embodiment provides a wave-absorbing polypropylene foaming bead, which comprises 65 parts of polypropylene resin, 25 parts of wave-absorbing powder and 10 parts of auxiliary agent. Wherein the weight content of plasticizer phthalic acid di (2-ethyl) ester is 30%, the weight content of nucleating agent silicon dioxide is 30%, the weight content of foaming auxiliary azodiisobutyronitrile is 30%, and the weight content of lubricant stearate is 10%.
The wave-absorbing polypropylene foaming bead and the preparation method thereof comprise the following steps:
step one, PDA/MoS 2 Is prepared from the following steps:
step one as in example 1
Step two, the wave-absorbing powder material provided by the invention is chemically modified molybdenum disulfide Cu/PDA/MoS 2 Is prepared from the following steps:
step two in example 1
Step three, preparing polypropylene composite wave-absorbing master batch:
10 parts of auxiliary agent and 25 parts of Cu/PDA/MoS are added in parts by weight 2 Adding a composite absorbent (namely wave-absorbing powder-chemically modified molybdenum disulfide) and 65 parts of polypropylene resin into a mixer, and uniformly mixing to obtain a mixed material; adding the mixed materials into a double-screw extruder for wiredrawing and granulating to obtain polypropylene composite wave-absorbing master batch, and controlling the temperature and screw rotating speed of each region, wherein the temperature of the first region is 150 ℃, the temperature of the second region is 170 ℃, the temperature of the third region is 170 ℃, the temperature of the fourth region is 175 ℃, the temperature of the fifth region is 200 ℃, the temperature of the sixth region is 200 ℃, the temperature of the seventh region is 205 ℃, and the screw rotating speed is 60-120r/min;
step four, preparing polypropylene primary foaming beads:
and in the same way as in the step four of the embodiment 1, only the polypropylene composite master batch obtained in the step three of the embodiment is replaced by the polypropylene composite master batch.
Step five, preparing polypropylene secondary foaming beads:
as in step five of example 1, only the polypropylene primary expanded beads were replaced with the polypropylene primary expanded beads obtained in step four of this example.
Example 3
The embodiment provides a wave-absorbing polypropylene foaming bead, which comprises 60 parts of polypropylene resin, 30 parts of wave-absorbing powder and 10 parts of auxiliary agent. Wherein the weight content of the plasticizer diglycol adipate is 30%, the weight content of the nucleating agent sodium benzoate is 30%, the weight content of the foaming auxiliary diisopropyl azodicarboxylate is 30%, and the weight content of the lubricant stearate is 10%.
The wave-absorbing polypropylene foaming bead and the preparation method thereof comprise the following steps:
step one, PDA/MoS 2 Is prepared from the following steps:
step one as in example 1
Step two, the wave-absorbing powder material provided by the invention is chemically modified molybdenum disulfide Cu/PDA/MoS 2 Is prepared from the following steps:
step two in example 1
Step three, preparing polypropylene composite wave-absorbing master batch:
10 parts of auxiliary agent and 30 parts of Cu/PDA/MoS are added in parts by weight 2 Adding a composite absorbent (namely wave-absorbing powder-chemically modified molybdenum disulfide) and 60 parts of polypropylene resin into a mixer, and uniformly mixing to obtain a mixed material; adding the mixed materials into a double-screw extruder for wiredrawing and granulating to obtain polypropylene composite wave-absorbing master batch, and controlling the temperature and screw rotating speed of each region, wherein the temperature of the first region is 150 ℃, the temperature of the second region is 170 ℃, the temperature of the third region is 170 ℃, the temperature of the fourth region is 180 ℃, the temperature of the fifth region is 205 ℃, the temperature of the sixth region is 210 ℃, the temperature of the seventh region is 210 ℃, and the screw rotating speed is 60-120r/min;
step four, preparing polypropylene primary foaming beads:
and in the same way as in the step four of the embodiment 1, only the polypropylene composite master batch obtained in the step three of the embodiment is replaced by the polypropylene composite master batch.
Step five, preparing polypropylene secondary foaming beads:
as in step five of example 1, only the polypropylene primary expanded beads were replaced with the polypropylene primary expanded beads obtained in step four of this example.
Comparative example 1
This comparative example provides a polypropylene expanded bead, which is substantially identical to the preparation method of example 2, except that: no added wave-absorbing powder material-chemical modified molybdenum disulfide Cu/PDA/MoS 2 A composite absorbent.
Comparative example 2
This comparative example provides a wave-absorbing polypropylene expanded bead, which is substantially identical to the preparation method of example 2, except that: there is no secondary foaming.
Performance testing
The beads prepared in examples 1-3 and comparative examples 1-2 were molded and foamed to prepare polypropylene foamed sheets. And (5) engraving the ring by using an engraving machine to obtain the coaxial ring for the wave-absorbing test. The test results of the wave absorbing performance by the coaxial method are shown in figure 1 and the test results of the mechanical performance are shown in table 1.
TABLE 1 mechanical Properties of examples 1-3 comparative examples 1-2
The invention provides a wave-absorbing polypropylene foaming bead and a preparation method thereof, which develop and verify a high-efficiency microwave absorbent through a chemical combination method, wherein the composite absorbent and polypropylene resin are mixed and extruded by a double-screw extruder to obtain a composite resin master batch with wave-absorbing performance; the composite master batch is foamed twice to obtain the wave-absorbing polypropylene foaming beads. Through the test of a vector network analyzer, the testing instrument is VNA, CETCCeYear3672B; the test frequency range is 2-18 GHz, and compared with comparative examples 1 and 2, the wave-absorbing performance of the embodiment is greatly improved, besides, the mechanical performance is improved, and the density reduction has important practical significance in the application of future wave-absorbing materials.
Claims (7)
1. The wave-absorbing polypropylene foaming beads are prepared from the following raw materials in parts by mass:
60-70 parts of polypropylene resin, 25-30 parts of wave-absorbing powder and 10 parts of auxiliary agent;
the wave-absorbing powder is chemically modified molybdenum disulfide;
the chemically modified molybdenum disulfide is a product obtained according to the following steps:
copper salt and PDA/MoS 2 Dissolving in solvent, stirring, filtering the obtained solution, collecting solid, drying, and treating at high temperature;
the density of the polypropylene resin matrix is 0.85-0.95g/cm 3 ；
The melt index is 90-100g/10min;
the copper salt is at least one selected from the group consisting of copper chloride hexahydrate, copper nitrate trihydrate and copper sulfate pentahydrate;
the solvent is at least one selected from deionized water, absolute ethyl alcohol and ethylene glycol;
the copper salt, PDA/MoS 2 The mass ratio of the solvent to the solvent is 1:2-4:15-17;
the auxiliary agent consists of a plasticizer, a nucleating agent, a foaming auxiliary agent and a lubricant;
in the high-temperature treatment step, the atmosphere is a mixed atmosphere consisting of nitrogen and argon; the flow rate ratio of the nitrogen to the argon is 1:2-4; the temperature is 700-900 ℃; the time is 2-4h; the temperature rising rate from room temperature to high temperature treatment temperature is 2-3 ℃/min;
the wave-absorbing polypropylene foaming beads also contain a dispersing agent.
2. The wave-absorbing polypropylene expanded beads according to claim 1, wherein:
each auxiliary agent accounts for 5% -35% of the total weight of the auxiliary agents;
the plasticizer is at least one selected from the group consisting of di (2-ethylhexyl) sebacate, di (2-ethyl) phthalate and diethylene glycol adipate;
the nucleating agent is at least one selected from talcum powder, silicon dioxide, mica and sodium benzoate;
the foaming auxiliary agent is at least one selected from azodicarbonamide, azodiisobutyronitrile and diisopropyl azodicarbonate;
the lubricant is at least one selected from the group consisting of trimethylolpropane and stearate;
the mass ratio of the dispersing agent to the polypropylene composite master batch is 0.5-1:8-10.
3. The wave-absorbing polypropylene expanded beads according to claim 1, wherein: in the stirring step, the rotating speed is 150-400rpm; the time is 4-8 hours;
in the drying step, the drying mode is vacuum drying; the time is 8-14h.
4. A method of preparing the wave-absorbing polypropylene expanded beads of any one of claims 1 to 3, comprising:
1) Mixing the polypropylene resin, the wave-absorbing powder and the auxiliary agent according to the mass ratio, and extruding to obtain polypropylene composite master batch;
2) Putting water, a dispersing agent and the polypropylene composite master batch into an autoclave, introducing carbon dioxide gas, heating the autoclave, controlling the temperature to 160-170 ℃ and the pressure to 1.5-2.0 MPa, and performing heat preservation and pressure maintaining for 3-10min, and then performing pressure relief to obtain polypropylene primary foaming polymerization beads;
3) And adding the polypropylene primary foaming beads into an autoclave, introducing high-pressure air, maintaining the pressure at 0.2-0.5MPa, and performing pressure maintaining for 8-12 hours, and then performing pressure relief to obtain the wave-absorbing polypropylene foaming beads.
5. The method according to claim 4, wherein: in the step 1) extrusion step, the length-diameter ratio of the twin-screw extruder used is 20:1, the rotating speed is 60-120r/min;
the temperature of the twin-screw extruder from the feeding end to the discharging end is set to be 150-180 ℃ in a first zone, 160-230 ℃ in a second zone, 160-280 ℃ in a third zone, 170-290 ℃ in a fourth zone, 200-300 ℃ in a fifth zone, 200-330 ℃ in a sixth zone and 200-350 ℃ in a seventh zone;
in the step 2), the mass ratio of water, the dispersing agent and the polypropylene composite master batch is 1:0.5-1:8-10.
6. Use of the wave-absorbing polypropylene expanded beads according to any one of claims 1 to 3 for microwave absorption.
7. Use of the wave-absorbing polypropylene expanded beads according to any one of claims 1 to 3 for the preparation of microwave absorbing products.
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