CN117024873A - Preparation method of modified polypropylene plastic - Google Patents
Preparation method of modified polypropylene plastic Download PDFInfo
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- CN117024873A CN117024873A CN202310707059.3A CN202310707059A CN117024873A CN 117024873 A CN117024873 A CN 117024873A CN 202310707059 A CN202310707059 A CN 202310707059A CN 117024873 A CN117024873 A CN 117024873A
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- polyether ketone
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- polypropylene
- modified
- modified polyether
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- -1 polypropylene Polymers 0.000 title claims abstract description 63
- 239000004743 Polypropylene Substances 0.000 title claims abstract description 62
- 229920001155 polypropylene Polymers 0.000 title claims abstract description 62
- 238000002360 preparation method Methods 0.000 title claims abstract description 32
- 239000004033 plastic Substances 0.000 title claims abstract description 13
- 229920001643 poly(ether ketone) Polymers 0.000 claims abstract description 62
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 58
- 239000002041 carbon nanotube Substances 0.000 claims abstract description 57
- 229910021393 carbon nanotube Inorganic materials 0.000 claims abstract description 57
- 238000002156 mixing Methods 0.000 claims abstract description 11
- 238000011065 in-situ storage Methods 0.000 claims abstract description 6
- 238000006116 polymerization reaction Methods 0.000 claims abstract description 6
- 239000006185 dispersion Substances 0.000 claims description 15
- 229930185605 Bisphenol Natural products 0.000 claims description 11
- 239000007788 liquid Substances 0.000 claims description 11
- 238000000034 method Methods 0.000 claims description 10
- IISBACLAFKSPIT-UHFFFAOYSA-N bisphenol A Chemical compound C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 claims description 9
- 239000002994 raw material Substances 0.000 claims description 9
- 239000003795 chemical substances by application Substances 0.000 claims description 5
- 239000003960 organic solvent Substances 0.000 claims description 5
- 238000006243 chemical reaction Methods 0.000 claims description 4
- 239000011261 inert gas Substances 0.000 claims description 4
- 238000007599 discharging Methods 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 3
- 239000002904 solvent Substances 0.000 claims description 3
- 238000003756 stirring Methods 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims description 3
- HKCNCNXZAZPKDZ-UHFFFAOYSA-N (4,4-difluorocyclohexa-1,5-dien-1-yl)-phenylmethanone Chemical compound C1=CC(F)(F)CC=C1C(=O)C1=CC=CC=C1 HKCNCNXZAZPKDZ-UHFFFAOYSA-N 0.000 claims description 2
- RXNYJUSEXLAVNQ-UHFFFAOYSA-N 4,4'-Dihydroxybenzophenone Chemical compound C1=CC(O)=CC=C1C(=O)C1=CC=C(O)C=C1 RXNYJUSEXLAVNQ-UHFFFAOYSA-N 0.000 claims description 2
- LSQARZALBDFYQZ-UHFFFAOYSA-N 4,4'-difluorobenzophenone Chemical compound C1=CC(F)=CC=C1C(=O)C1=CC=C(F)C=C1 LSQARZALBDFYQZ-UHFFFAOYSA-N 0.000 claims description 2
- 239000012298 atmosphere Substances 0.000 claims description 2
- 238000001816 cooling Methods 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 2
- 239000000463 material Substances 0.000 abstract description 8
- 239000011159 matrix material Substances 0.000 abstract description 6
- 239000011347 resin Substances 0.000 abstract description 6
- 229920005989 resin Polymers 0.000 abstract description 6
- 230000000052 comparative effect Effects 0.000 description 13
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 description 10
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 10
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 description 10
- 150000001875 compounds Chemical class 0.000 description 8
- 238000012986 modification Methods 0.000 description 6
- 230000004048 modification Effects 0.000 description 6
- 229910000027 potassium carbonate Inorganic materials 0.000 description 5
- 229910000029 sodium carbonate Inorganic materials 0.000 description 5
- KZTYYGOKRVBIMI-UHFFFAOYSA-N diphenyl sulfone Chemical compound C=1C=CC=CC=1S(=O)(=O)C1=CC=CC=C1 KZTYYGOKRVBIMI-UHFFFAOYSA-N 0.000 description 4
- NIHNNTQXNPWCJQ-UHFFFAOYSA-N fluorene Chemical compound C1=CC=C2CC3=CC=CC=C3C2=C1 NIHNNTQXNPWCJQ-UHFFFAOYSA-N 0.000 description 4
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 3
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 3
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 150000003839 salts Chemical class 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- MYRTYDVEIRVNKP-UHFFFAOYSA-N 1,2-Divinylbenzene Chemical compound C=CC1=CC=CC=C1C=C MYRTYDVEIRVNKP-UHFFFAOYSA-N 0.000 description 2
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 description 2
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 2
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 2
- BGYHLZZASRKEJE-UHFFFAOYSA-N [3-[3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoyloxy]-2,2-bis[3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoyloxymethyl]propyl] 3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoate Chemical compound CC(C)(C)C1=C(O)C(C(C)(C)C)=CC(CCC(=O)OCC(COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)(COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)=C1 BGYHLZZASRKEJE-UHFFFAOYSA-N 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- DOIRQSBPFJWKBE-UHFFFAOYSA-N dibutyl phthalate Chemical compound CCCCOC(=O)C1=CC=CC=C1C(=O)OCCCC DOIRQSBPFJWKBE-UHFFFAOYSA-N 0.000 description 2
- ZUOUZKKEUPVFJK-UHFFFAOYSA-N diphenyl Chemical compound C1=CC=CC=C1C1=CC=CC=C1 ZUOUZKKEUPVFJK-UHFFFAOYSA-N 0.000 description 2
- 238000001125 extrusion Methods 0.000 description 2
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 2
- 239000000155 melt Substances 0.000 description 2
- 239000002048 multi walled nanotube Substances 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 239000008096 xylene Substances 0.000 description 2
- 239000006057 Non-nutritive feed additive Substances 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- PYKYMHQGRFAEBM-UHFFFAOYSA-N anthraquinone Natural products CCC(=O)c1c(O)c2C(=O)C3C(C=CC=C3O)C(=O)c2cc1CC(=O)OC PYKYMHQGRFAEBM-UHFFFAOYSA-N 0.000 description 1
- 150000004056 anthraquinones Chemical class 0.000 description 1
- 230000000844 anti-bacterial effect Effects 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 239000012300 argon atmosphere Substances 0.000 description 1
- RWCCWEUUXYIKHB-UHFFFAOYSA-N benzophenone Chemical compound C=1C=CC=CC=1C(=O)C1=CC=CC=C1 RWCCWEUUXYIKHB-UHFFFAOYSA-N 0.000 description 1
- 235000010290 biphenyl Nutrition 0.000 description 1
- 239000004305 biphenyl Substances 0.000 description 1
- 229910000019 calcium carbonate Inorganic materials 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 239000011231 conductive filler Substances 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000005469 granulation Methods 0.000 description 1
- 230000003179 granulation Effects 0.000 description 1
- 229920006150 hyperbranched polyester Polymers 0.000 description 1
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 description 1
- 229910052808 lithium carbonate Inorganic materials 0.000 description 1
- 239000000314 lubricant Substances 0.000 description 1
- ZLNQQNXFFQJAID-UHFFFAOYSA-L magnesium carbonate Chemical compound [Mg+2].[O-]C([O-])=O ZLNQQNXFFQJAID-UHFFFAOYSA-L 0.000 description 1
- 239000001095 magnesium carbonate Substances 0.000 description 1
- 229910000021 magnesium carbonate Inorganic materials 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229910021392 nanocarbon Inorganic materials 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 239000008188 pellet Substances 0.000 description 1
- 229920006124 polyolefin elastomer Polymers 0.000 description 1
- 229920005629 polypropylene homopolymer Polymers 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 238000010992 reflux Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000002109 single walled nanotube Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229920001169 thermoplastic Polymers 0.000 description 1
- 239000004416 thermosoftening plastic Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
- C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L23/10—Homopolymers or copolymers of propene
- C08L23/12—Polypropene
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G65/00—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule
- C08G65/34—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from hydroxy compounds or their metallic derivatives
- C08G65/38—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from hydroxy compounds or their metallic derivatives derived from phenols
- C08G65/40—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from hydroxy compounds or their metallic derivatives derived from phenols from phenols (I) and other compounds (II), e.g. OH-Ar-OH + X-Ar-X, where X is halogen atom, i.e. leaving group
- C08G65/4012—Other compound (II) containing a ketone group, e.g. X-Ar-C(=O)-Ar-X for polyetherketones
Landscapes
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention provides a preparation method of modified polypropylene plastic, which is prepared by blending polypropylene and modified polyether ketone, wherein the modified polyether ketone is prepared by modifying carbon nano tubes in an in-situ polymerization mode. Therefore, the dispersibility of the carbon nano tube in the polypropylene matrix resin is improved, and the comprehensive performance of the prepared material is improved.
Description
Technical Field
The invention relates to a preparation method of modified polypropylene plastic, in particular to a preparation method of modified polypropylene plastic by nano carbon material.
Background
Polypropylene, which is a commonly used industrial plastic, has excellent properties such as high strength, high hardness, good impact resistance, strong corrosion resistance, good moldability, etc., and thus is widely used in various fields.
The carbon nano tube has excellent mechanical property and conductivity, can be added into polypropylene, and improves the performance of the polypropylene. The carbon nanotube directly modified polypropylene can improve the mechanical strength, conductivity, thermal stability and flame retardance of polypropylene, thereby expanding the application field of polypropylene. However, since the carbon nanotubes themselves are difficult to uniformly disperse in the polypropylene matrix, the performance improvement of the polypropylene by direct modification is limited.
The patent CN115850869A discloses a polypropylene modified thermoplastic shielding material and a preparation method thereof, wherein polypropylene, polyolefin elastomer and modified resin are used as matrixes, conductive filler, antioxidant, lubricant and processing aid are added for blending modification, and the added carbon nano tube is not further modified, but is directly added into the matrix resin for modification, so that various properties of the material are improved.
Patent CN114539667a discloses a durable antibacterial polypropylene composition, a preparation method and application thereof, and the patent promotes better dispersion of carbon nanotubes in a polypropylene matrix by grafting the carbon nanotubes on hyperbranched polyester, thereby improving the performance of polypropylene.
The prior art adds carbon nanotubes to polypropylene resin by different methods, but with different technical effects. The invention aims to provide a carbon nano tube modified polypropylene material which is different from the prior art and has good comprehensive performance.
Disclosure of Invention
The invention provides a preparation method of modified polypropylene plastic, which is prepared by blending polypropylene and modified polyether ketone, wherein the modified polyether ketone is prepared by modifying carbon nano tubes in an in-situ polymerization mode. Therefore, the dispersibility of the carbon nano tube in the polypropylene matrix resin is improved, and the comprehensive performance of the prepared material is improved.
The technical scheme provided by the invention is as follows:
the preparation method of the modified polypropylene plastic comprises the step of blending polypropylene and modified polyether ketone, wherein the modified polyether ketone is prepared in an in-situ polymerization mode by modifying carbon nano tubes.
The invention selects the carbon nano tube to modify the polypropylene, but if the carbon nano tube is directly added into the polypropylene, the prepared modified polypropylene plastic has poor performance due to poor dispersibility. The inventor finds that the carbon nano tube is added into the polyether ketone in an in-situ polymerization mode, so that the carbon nano tube is pre-dispersed in the polyether ketone; and then blending the prepared modified polyether ketone with polypropylene to obtain a modified polypropylene plastic with better performance than a sample obtained by directly modifying polypropylene by using the carbon nano tube.
It should be noted that, the modification of the polyetherketone by in-situ polymerization of the carbon nanotubes is already disclosed in the prior art, for example, a carbon nanotube/polyetherketone composite material disclosed in CN110183647a, and a preparation method and application thereof, but the blending modification of the carbon nanotube-modified polyetherketone and the polypropylene material as described in the present invention is not disclosed in the prior art.
The preparation raw materials of the modified polyether ketone comprise 4, 4-difluorobenzophenone, 4-dihydroxybenzophenone and carbon nanotubes.
The preparation method of the modified polyether ketone comprises the following steps:
adding the carbon nano tube and an organic solvent into a reactor to uniformly disperse, and obtaining a carbon nano tube dispersion liquid for standby;
and step two, adding a solvent, 4 '-dihydroxybenzophenone, 4' -difluorobenzophenone, a salifying agent and the carbon nanotube dispersion liquid into a reactor under the inert gas atmosphere, starting stirring, controlling the temperature of the reactor to be 170-310 ℃ for reaction for 2-6 hours, discharging, cooling, washing and drying to obtain the modified polyether ketone.
In a preferred embodiment of the present invention, in the second step of the preparation method of the modified polyether ketone, after the reaction raw materials are added into the reactor, the reaction system is sequentially reacted at 140 to 180 ℃ for 1 to 2 hours, at 210 to 230 ℃ for 2 to 3 hours, at 240 to 280 ℃ for 2 to 3 hours, and at 300 to 310 ℃ for 0.5 to 1 hour.
The inert gas may be selected from inert gases commonly used in the art, such as nitrogen, argon, etc., and such gases may be used alone or in combination.
The salt former may be selected from those commonly used in the art for preparing polyetherketones, such as potassium carbonate, sodium carbonate, calcium carbonate, magnesium carbonate, lithium carbonate, etc., and such salt formers may be used alone or in combination. In a preferred embodiment of the present invention, the salt former is potassium carbonate and sodium carbonate, wherein the molar ratio of potassium carbonate to sodium carbonate is 1:10.
the preparation method of the modified polyether ketone is not further limited, and the process steps, the raw material types, the dosage and the like can be adjusted according to the technical scheme commonly used in the field. For example, the organic solvent in the first step may be toluene, xylene, acetone, butanone, diethyl ether, chloroform, divinylbenzene, etc.; the solvent in the second step can be diphenyl sulfone, biphenyl, anthraquinone, dibutyl phthalate, silicon oil and the like.
In the preparation method of the modified polyether ketone, the first step is as follows: adding the carbon nano tube, 4' -diphenyl methylene bisphenol and an organic solvent into a reactor for uniform dispersion to obtain a carbon nano tube dispersion liquid for standby.
In the preparation method of the modified polyether ketone, a small amount of reactive compound can be selectively introduced to regulate and control the performance of the polyether ketone, and the modified polyether ketone and the carbon nano tube promote the dispersion thereof through the stacking effect. Such reactive compounds are preferably compounds having a hydroxyl group and a benzene ring structure, particularly compounds having a dihydroxyl group and a benzene ring structure, such as bisphenol fluorene and the like. When the reactive compound is simply applied to the preparation of the polyether ketone, only whether the chemical structure of the reactive compound is suitable for the synthesis of the polyether ketone is needed to be considered, but when the reactive compound is applied to the technical scheme of the invention, namely the carbon nanotube modified polypropylene, the influence on the polyether ketone is needed to be considered, and the situation of the material performance after the polyether ketone and the polypropylene are blended is also needed to be considered. According to the invention, 4' -dibenzylidene bisphenol is preferably used as a reactive compound to modify the polyether ketone, so that on one hand, the dispersibility of the carbon nano tube in the polyether ketone synthesis process can be promoted, the performance of the polyether ketone can be improved, and on the other hand, the modified polyether ketone prepared by the method has better compatibility when being blended with polypropylene, and the obtained modified polypropylene has more excellent performance.
In the preparation method of the modified polyether ketone, the molar ratio of the 4,4' -dibenzylidene bisphenol, the 4,4' -dihydroxybenzophenone and the 4,4' -difluorobenzophenone is 0.01-0.1: 0.9 to 0.99:1 to 1.2; preferably 0.1:0.9:1.05.
the mass ratio of the carbon nano tube to the 4,4' -dibenzylidene bisphenol is 0.1-1: 1, preferably 0.5 to 0.8:1.
in a preferred embodiment of the present invention, the modified polyetherketone is prepared by blending polypropylene in the form of small particles or powder after pulverization. The modified polyetherketone is preferably broken into a powder. In the melt blending process of the polyether ketone and the polypropylene, the polypropylene is matrix resin, and the processing temperature is more preferably set within the applicable range of the polypropylene, but the melt flow temperature of the polyether ketone is higher, so that the smaller the particle size of the polyether ketone is, the better the compatibility between the polyether ketone and the polypropylene is.
The carbon nanotubes may be selected from those commonly used in the art, preferably nonfunctionalized carbon nanotubes, i.e., multi-walled carbon nanotubes and/or single-walled carbon nanotubes. The functionalized carbon nanotubes, i.e. the carbon nanotubes are modified, and the structures of the carbon nanotubes are provided with active groups, such as hydroxyl groups, carboxyl groups and the like, so that the structures of the carbon nanotubes are damaged to a certain extent through modification, the strength of the carbon nanotubes is reduced, and the performance of the final material is possibly reduced.
The mass ratio of the polypropylene to the modified polyether ketone is 10:1 to 3.
The polypropylene may be selected from polypropylene commonly used in the art, such as homo-polypropylene, co-polypropylene, and the like.
The method for blending the polypropylene and the modified polyether ketone can adopt a technical scheme commonly used in the field. In a preferred embodiment of the present invention, the polypropylene and the modified polyether ketone are pre-mixed by a high-speed mixer and then blended by a twin-screw extruder, the rotation speed of the twin-screw extruder is 200-900 rpm, and the screw temperature is 180-230 ℃.
Detailed Description
The invention is further illustrated below in conjunction with specific examples. Unless specifically stated otherwise, the reagents, methods and apparatus employed in the present invention are those conventional in the art.
The raw materials adopted in the embodiment and the comparative example of the invention are as follows:
polypropylene, H309F, SK chemistry;
carbon nanotubes, XFM04, multiwall carbon nanotubes, jiangsu Xianfeng nanomaterials Co., ltd.
The preparation method of the carbon nanotube dispersion liquid 1 comprises the following steps: 17.62 parts by mass of carbon nano tube, 35.24 parts by mass of 4,4' -dibenzylidene bisphenol and 300 parts by mass of dimethylbenzene are added into a reactor, magnetically stirred and ultrasonically treated for 2 hours, and discharged for later use.
The preparation method of the carbon nano tube dispersion liquid 2 comprises the following steps: 28.19 parts by mass of carbon nano tube, 35.24 parts by mass of 4,4' -dibenzylidene bisphenol and 300 parts by mass of dimethylbenzene are added into a reactor, magnetically stirred and ultrasonically treated for 2 hours, and discharged for later use.
The preparation method of the carbon nano tube dispersion liquid 3 comprises the following steps: 28.03 parts by mass of carbon nano tube, 35.04 parts by mass of bisphenol fluorene and 300 parts by mass of xylene are added into a reactor, magnetically stirred and ultrasonically treated for 2 hours, and discharged for later use.
The preparation method of the carbon nanotube dispersion liquid 4 comprises the following steps: 28.19 parts by mass of carbon nano tube and 300 parts by mass of dimethylbenzene are added into a reactor, and the reactor is magnetically stirred and ultrasonically treated for 2 hours, and then the reactor is discharged for standby.
The salifying agent 1 adopts potassium carbonate and sodium carbonate with the mass of 1:10.
The salifying agent 2 adopts potassium carbonate and sodium carbonate with the mass of 1: 100.
The preparation method of the modified polyether ketone comprises the following steps: adding diphenyl sulfone, salifying agent, 4-di-light diphenyl ketone, 4' -difluoro diphenyl ketone and carbon nano tube dispersion liquid (if any) into a reactor under argon atmosphere, controlling the temperature of the reactor at 180 ℃, starting stirring, condensing and refluxing, reacting for 2 hours at 230 ℃, removing dimethylbenzene, reacting for 2 hours at 280 ℃, reacting for 0.5 hour at 310 ℃, discharging, crushing, washing and drying to obtain the modified polyether ketone.
The types and amounts of the respective raw materials of the modified polyether ketones used in the examples and comparative examples are shown in Table 1 in terms of relative parts by mass of the respective components.
TABLE 1 variety and amount of modified polyetherketone raw materials (parts by mass)
The preparation method of the modified polypropylene plastic samples of the examples and the comparative example 1 comprises the following steps: polypropylene, modified polyether ketone and antioxidant 1010 are mixed uniformly in advance by a high-speed mixer, extruded and granulated by a double-screw extruder under the condition that the screw rotating speed is 300rpm, and the screw temperature is 190 ℃, 200 ℃, 210 ℃, 220 ℃, 230 ℃, 220 ℃, 190 ℃, 185 ℃ and 180 ℃ from a feed inlet to a machine head section. Wherein the polypropylene is granular, and the modified polyether ketone is crushed into powder in advance.
The preparation method of the modified polypropylene plastic sample of comparative example 2 comprises the following steps: mixing polypropylene, carbon nanotube (the addition amount of carbon nanotube is 0.6% of polypropylene mass) and antioxidant 1010 uniformly in advance by a high-speed mixer, adding into a double-screw extruder for extrusion granulation, wherein the extrusion condition is that the screw rotation speed is 300rpm, and the screw temperature is 190 ℃, 200 ℃, 210 ℃, 220 ℃, 230 ℃, 220 ℃, 190 ℃, 185 ℃ and 180 ℃ from a feed inlet to a machine head section.
The amounts of polypropylene and modified polyetherketone used in examples and comparative example 1 are shown in Table 2, in relative parts by mass between the components.
Table 2 raw material amounts (parts by mass) of examples and comparative examples
| Category(s) | Example 1 | Example 2 | Example 3 | Example 4 | Example 5 | Comparative example 1 |
| Polypropylene | 10 | 10 | 10 | 10 | 10 | 10 |
| Modified polyetherketone 1 | 3 | |||||
| Modified polyetherketone 2 | 1 | |||||
| Modified polyetherketone 3 | 1 | |||||
| Modified polyetherketone 4 | 1 | |||||
| Modified polyetherketone 5 | 1 | |||||
| Modified polyetherketone 6 | 1 |
It is noted that comparative example 2 was not added with modified polyetherketone, but the polypropylene pellets used were subjected to the same processing steps for performance comparison.
The performance test is carried out on the samples of the examples and the comparative examples, the tensile strength test standard is ISO 527, the spline size is 130mm x 10mm x 0.8mm, and the tensile rate is 50mm/min; the impact strength test standard is ISO 179 test, cantilever beam, spline size 80mm 10mm 4mm, type A notch.
Table 3 results of the performance test of examples and comparative examples
The raw materials, the amounts, the process steps and the like which are not described in the examples and the comparative examples of the invention are all common in the field, and the non-described matters are consistent in the examples and the comparative examples, so that the examples and the comparative examples are not affected to be transversely compared, and the technical effects of the invention are not affected.
Claims (7)
1. The preparation method of the modified polypropylene plastic is characterized by comprising the step of blending polypropylene and modified polyether ketone, wherein the modified polyether ketone is prepared in an in-situ polymerization mode by modifying carbon nano tubes.
2. The preparation method according to claim 1, wherein the preparation raw material of the modified polyether ketone comprises 4, 4-difluorobenzophenone, 4-dihydroxybenzophenone, and carbon nanotubes.
3. The preparation method of the modified polyether ketone according to claim 2, wherein the preparation method comprises the following steps:
adding the carbon nano tube and an organic solvent into a reactor to uniformly disperse, and obtaining a carbon nano tube dispersion liquid for standby;
and step two, adding a solvent, 4 '-dihydroxybenzophenone, 4' -difluorobenzophenone, a salifying agent and the carbon nanotube dispersion liquid into a reactor under the inert gas atmosphere, starting stirring, controlling the temperature of the reactor to be 170-310 ℃ for reaction for 2-6 hours, discharging, cooling, washing and drying to obtain the modified polyether ketone.
4. The method according to claim 3, wherein in the method for producing the modified polyether ketone, the first step is: adding the carbon nano tube, 4' -diphenyl methylene bisphenol and an organic solvent into a reactor for uniform dispersion to obtain a carbon nano tube dispersion liquid for standby.
5. The method according to claim 4, wherein in the method for producing the modified polyether ketone, the molar ratio of the 4,4' -dibenzylidene bisphenol, the 4,4' -dihydroxybenzophenone, and the 4,4' -difluorobenzophenone is 0.01 to 0.1:0.9 to 0.99:1 to 1.2; preferably 0.1:0.9:1.05.
6. the preparation method according to claim 5, wherein the mass ratio of the carbon nanotubes to the 4,4' -dibenzylidene bisphenol is 0.1 to 1:1, preferably 0.5 to 0.8:1.
7. the preparation method according to any one of claims 1 to 6, wherein the mass ratio of the polypropylene to the modified polyether ketone is 10:1 to 3.
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