CN116970239A - Antistatic polypropylene film and preparation method and application thereof - Google Patents
Antistatic polypropylene film and preparation method and application thereof Download PDFInfo
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- CN116970239A CN116970239A CN202210422072.XA CN202210422072A CN116970239A CN 116970239 A CN116970239 A CN 116970239A CN 202210422072 A CN202210422072 A CN 202210422072A CN 116970239 A CN116970239 A CN 116970239A
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- polypropylene
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- -1 polypropylene Polymers 0.000 title claims abstract description 87
- 239000004743 Polypropylene Substances 0.000 title claims abstract description 84
- 229920001155 polypropylene Polymers 0.000 title claims abstract description 84
- 238000002360 preparation method Methods 0.000 title abstract description 12
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical class [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 119
- 239000012752 auxiliary agent Substances 0.000 claims abstract description 19
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 41
- 239000003963 antioxidant agent Substances 0.000 claims description 32
- 230000003078 antioxidant effect Effects 0.000 claims description 21
- 229910002092 carbon dioxide Inorganic materials 0.000 claims description 20
- 239000001569 carbon dioxide Substances 0.000 claims description 20
- 229910002804 graphite Inorganic materials 0.000 claims description 20
- 239000010439 graphite Substances 0.000 claims description 20
- 238000000034 method Methods 0.000 claims description 18
- 238000000227 grinding Methods 0.000 claims description 17
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 11
- 239000001257 hydrogen Substances 0.000 claims description 11
- 229910052739 hydrogen Inorganic materials 0.000 claims description 11
- 229910052760 oxygen Inorganic materials 0.000 claims description 11
- 239000001301 oxygen Substances 0.000 claims description 11
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 10
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 10
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 claims description 8
- 239000007822 coupling agent Substances 0.000 claims description 7
- 239000000463 material Substances 0.000 claims description 7
- 238000004806 packaging method and process Methods 0.000 claims description 7
- 229910019142 PO4 Inorganic materials 0.000 claims description 6
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 claims description 6
- JKIJEFPNVSHHEI-UHFFFAOYSA-N Phenol, 2,4-bis(1,1-dimethylethyl)-, phosphite (3:1) Chemical group CC(C)(C)C1=CC(C(C)(C)C)=CC=C1OP(OC=1C(=CC(=CC=1)C(C)(C)C)C(C)(C)C)OC1=CC=C(C(C)(C)C)C=C1C(C)(C)C JKIJEFPNVSHHEI-UHFFFAOYSA-N 0.000 claims description 6
- 239000010452 phosphate Substances 0.000 claims description 6
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims description 6
- 230000008569 process Effects 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- SOGAXMICEFXMKE-UHFFFAOYSA-N Butylmethacrylate Chemical compound CCCCOC(=O)C(C)=C SOGAXMICEFXMKE-UHFFFAOYSA-N 0.000 claims description 4
- NAQMVNRVTILPCV-UHFFFAOYSA-N hexane-1,6-diamine Chemical compound NCCCCCCN NAQMVNRVTILPCV-UHFFFAOYSA-N 0.000 claims description 4
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 150000007970 thio esters Chemical class 0.000 claims description 3
- VNQNXQYZMPJLQX-UHFFFAOYSA-N 1,3,5-tris[(3,5-ditert-butyl-4-hydroxyphenyl)methyl]-1,3,5-triazinane-2,4,6-trione Chemical compound CC(C)(C)C1=C(O)C(C(C)(C)C)=CC(CN2C(N(CC=3C=C(C(O)=C(C=3)C(C)(C)C)C(C)(C)C)C(=O)N(CC=3C=C(C(O)=C(C=3)C(C)(C)C)C(C)(C)C)C2=O)=O)=C1 VNQNXQYZMPJLQX-UHFFFAOYSA-N 0.000 claims description 2
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 claims description 2
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 2
- VVQNEPGJFQJSBK-UHFFFAOYSA-N Methyl methacrylate Chemical compound COC(=O)C(C)=C VVQNEPGJFQJSBK-UHFFFAOYSA-N 0.000 claims description 2
- BGHBLQKNCVRIKV-UHFFFAOYSA-N OP(O)OP(O)O.OCC(CO)(CO)CO.C(C)(C)(C)C1=C(C=CC(=C1)C(C)(C)C)O.C(C)(C)(C)C1=C(C=CC(=C1)C(C)(C)C)O Chemical compound OP(O)OP(O)O.OCC(CO)(CO)CO.C(C)(C)(C)C1=C(C=CC(=C1)C(C)(C)C)O.C(C)(C)(C)C1=C(C=CC(=C1)C(C)(C)C)O BGHBLQKNCVRIKV-UHFFFAOYSA-N 0.000 claims description 2
- VOZRXNHHFUQHIL-UHFFFAOYSA-N glycidyl methacrylate Chemical compound CC(=C)C(=O)OCC1CO1 VOZRXNHHFUQHIL-UHFFFAOYSA-N 0.000 claims description 2
- FPYJFEHAWHCUMM-UHFFFAOYSA-N maleic anhydride Chemical compound O=C1OC(=O)C=C1 FPYJFEHAWHCUMM-UHFFFAOYSA-N 0.000 claims description 2
- 229920001911 maleic anhydride grafted polypropylene Polymers 0.000 claims description 2
- 239000005022 packaging material Substances 0.000 claims description 2
- 239000002245 particle Substances 0.000 claims description 2
- WXZMFSXDPGVJKK-UHFFFAOYSA-N pentaerythritol Chemical compound OCC(CO)(CO)CO WXZMFSXDPGVJKK-UHFFFAOYSA-N 0.000 claims description 2
- XBDQKXXYIPTUBI-UHFFFAOYSA-M Propionate Chemical compound CCC([O-])=O XBDQKXXYIPTUBI-UHFFFAOYSA-M 0.000 claims 1
- 239000011159 matrix material Substances 0.000 abstract description 2
- 229910021389 graphene Inorganic materials 0.000 description 33
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 9
- 239000012535 impurity Substances 0.000 description 9
- 230000003068 static effect Effects 0.000 description 8
- 238000004833 X-ray photoelectron spectroscopy Methods 0.000 description 7
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- 239000000126 substance Substances 0.000 description 6
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- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 4
- BGYHLZZASRKEJE-UHFFFAOYSA-N [3-[3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoyloxy]-2,2-bis[3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoyloxymethyl]propyl] 3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoate Chemical compound CC(C)(C)C1=C(O)C(C(C)(C)C)=CC(CCC(=O)OCC(COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)(COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)=C1 BGYHLZZASRKEJE-UHFFFAOYSA-N 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
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- 238000004626 scanning electron microscopy Methods 0.000 description 4
- 238000007789 sealing Methods 0.000 description 4
- 238000010008 shearing Methods 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- 238000009825 accumulation Methods 0.000 description 3
- 239000002216 antistatic agent Substances 0.000 description 3
- 238000000498 ball milling Methods 0.000 description 3
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- 238000006243 chemical reaction Methods 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 125000000524 functional group Chemical group 0.000 description 3
- 238000012856 packing Methods 0.000 description 3
- 229920000642 polymer Polymers 0.000 description 3
- 229920005629 polypropylene homopolymer Polymers 0.000 description 3
- 238000012545 processing Methods 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 2
- 239000000428 dust Substances 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 230000003993 interaction Effects 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
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- 238000005086 pumping Methods 0.000 description 2
- 238000005070 sampling Methods 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- GHKOFFNLGXMVNJ-UHFFFAOYSA-N Didodecyl thiobispropanoate Chemical compound CCCCCCCCCCCCOC(=O)CCSCCC(=O)OCCCCCCCCCCCC GHKOFFNLGXMVNJ-UHFFFAOYSA-N 0.000 description 1
- OKOBUGCCXMIKDM-UHFFFAOYSA-N Irganox 1098 Chemical compound CC(C)(C)C1=C(O)C(C(C)(C)C)=CC(CCC(=O)NCCCCCCNC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)=C1 OKOBUGCCXMIKDM-UHFFFAOYSA-N 0.000 description 1
- XGULBQUJRQPLOG-OOOULUNWSA-N O([C@@H]1[C@@H](C)[C@H](O)CC(=O)O[C@@H]([C@H](/C=C(\C)/C=C/C(=O)[C@H](C)C[C@@H]1CC=O)COCC=1C=CC=CC=1)CC)[C@@H]1O[C@H](C)[C@@H](O)[C@H](N(C)C)[C@H]1O Chemical compound O([C@@H]1[C@@H](C)[C@H](O)CC(=O)O[C@@H]([C@H](/C=C(\C)/C=C/C(=O)[C@H](C)C[C@@H]1CC=O)COCC=1C=CC=CC=1)CC)[C@@H]1O[C@H](C)[C@@H](O)[C@H](N(C)C)[C@H]1O XGULBQUJRQPLOG-OOOULUNWSA-N 0.000 description 1
- 239000006096 absorbing agent Substances 0.000 description 1
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- 125000003277 amino group Chemical group 0.000 description 1
- 239000006229 carbon black Substances 0.000 description 1
- 235000011089 carbon dioxide Nutrition 0.000 description 1
- 235000009508 confectionery Nutrition 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- JBSLOWBPDRZSMB-FPLPWBNLSA-N dibutyl (z)-but-2-enedioate Chemical compound CCCCOC(=O)\C=C/C(=O)OCCCC JBSLOWBPDRZSMB-FPLPWBNLSA-N 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- PWWSSIYVTQUJQQ-UHFFFAOYSA-N distearyl thiodipropionate Chemical compound CCCCCCCCCCCCCCCCCCOC(=O)CCSCCC(=O)OCCCCCCCCCCCCCCCCCC PWWSSIYVTQUJQQ-UHFFFAOYSA-N 0.000 description 1
- 238000010292 electrical insulation Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 230000005674 electromagnetic induction Effects 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 125000003700 epoxy group Chemical group 0.000 description 1
- 238000001125 extrusion Methods 0.000 description 1
- 239000003063 flame retardant Substances 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 238000007306 functionalization reaction Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000003801 milling Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000002667 nucleating agent Substances 0.000 description 1
- SSDSCDGVMJFTEQ-UHFFFAOYSA-N octadecyl 3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoate Chemical compound CCCCCCCCCCCCCCCCCCOC(=O)CCC1=CC(C(C)(C)C)=C(O)C(C(C)(C)C)=C1 SSDSCDGVMJFTEQ-UHFFFAOYSA-N 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000012858 packaging process Methods 0.000 description 1
- NFHFRUOZVGFOOS-UHFFFAOYSA-N palladium;triphenylphosphane Chemical compound [Pd].C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1.C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1.C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1.C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1 NFHFRUOZVGFOOS-UHFFFAOYSA-N 0.000 description 1
- 229920006255 plastic film Polymers 0.000 description 1
- 239000002985 plastic film Substances 0.000 description 1
- 229920006254 polymer film Polymers 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 102220040412 rs587778307 Human genes 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000006557 surface reaction Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 238000004506 ultrasonic cleaning Methods 0.000 description 1
Classifications
-
- 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
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B65—CONVEYING; PACKING; STORING; HANDLING THIN OR FILAMENTARY MATERIAL
- B65D—CONTAINERS FOR STORAGE OR TRANSPORT OF ARTICLES OR MATERIALS, e.g. BAGS, BARRELS, BOTTLES, BOXES, CANS, CARTONS, CRATES, DRUMS, JARS, TANKS, HOPPERS, FORWARDING CONTAINERS; ACCESSORIES, CLOSURES, OR FITTINGS THEREFOR; PACKAGING ELEMENTS; PACKAGES
- B65D65/00—Wrappers or flexible covers; Packaging materials of special type or form
- B65D65/38—Packaging materials of special type or form
-
- 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
- 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
-
- 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
- C08J2451/00—Characterised by the use of graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Derivatives of such polymers
- C08J2451/06—Characterised by the use of graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Derivatives of such polymers grafted on to homopolymers or copolymers of aliphatic hydrocarbons containing only one carbon-to-carbon double bond
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/017—Additives being an antistatic agent
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/04—Carbon
- C08K3/042—Graphene or derivatives, e.g. graphene oxides
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
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- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Mechanical Engineering (AREA)
- Manufacture Of Macromolecular Shaped Articles (AREA)
Abstract
The invention belongs to the field of polypropylene films, and relates to an antistatic polypropylene film, and a preparation method and application thereof. The polypropylene film comprises polypropylene, edge modified graphene and an auxiliary agent, wherein the content of the edge modified graphene is 0.05-5 parts by weight and the content of the auxiliary agent is 0.1-20 parts by weight based on 100 parts by weight of polypropylene; the auxiliary agent comprises a compatilizer. The edge modified graphene used in the invention can react with groups in the compatilizer, so that the compatibility of the matrix and the edge modified graphene is improved, the edge modified graphene can be more effectively dispersed in polypropylene, and the prepared antistatic polypropylene film has good antistatic performance and mechanical property.
Description
Technical Field
The invention belongs to the field of polypropylene films, and particularly relates to an antistatic polypropylene film, a preparation method of the antistatic polypropylene film and application of the antistatic polypropylene film.
Background
The polypropylene molecule is completely nonpolar, has high electrical insulation and has surface resistivity of 10 14 -10 17 Omega, volume resistivity 10 15 -10 18 The static charge accumulation is easy to generate in omega/cm, the static charge is hard to disappear by conduction due to the reason of friction and the like in the production or processing process of the polypropylene film, the problems are brought to the production, processing and application of the film, and when a human body contacts with a product with the static charge, the feeling of electric shock is also generated. For example, when a film is used for packaging powdery commodities, the sealing strength is greatly reduced due to electrostatic dust collection of a heat sealing surface, and the commodities can be seriously damaged in the process of storage and transportation; when the film is printed, the ink transfer is possibly influenced by the electrostatic dust collection effect of the film, and uneven inking and the like are caused to cause the defect of printed patterns; in the packaging process of the high-speed packaging production line, static electricity can influence the cutting, conveying, folding and the like of the film; particularly, with the rapid development of IT industry, various sensitive electronic components, instruments and meters and the like are also packaged by a large amount of plastic films, the films can generate static accumulation due to electromagnetic induction and friction, and the static accumulation can generate static attraction or repulsion and spark discharge phenomena, so that the packaged commodity is destroyed due to high-voltage discharge generated by the static accumulationEven fire can occur under dry storage conditions. The antistatic polypropylene film is applied in powder packing, food packing, candy packing and other fields, and after the 80 th century, the antistatic polypropylene film and product are developed fast in electromechanical product, instrument and meter part, electronic component, large scale integrated circuit, circuit board and other fields, and the requirement and use amount are increased fast.
The graphene has excellent conductivity, and when added in a small amount, the polymer has good antistatic performance. However, due to the inert surface of graphene, the graphene lacks effective chemical bond or hydrogen bond connection with polymer molecules, and surface functionalization treatment is often required. Functionalized graphene refers to the introduction of functional groups, such as carboxyl groups, amine groups, epoxy groups, on the surface or edge of graphene through chemical reaction. The main purpose of introducing functional groups is to increase the polarity of graphene or provide chemical reaction sites, enhancing the interaction between graphene and other materials. However, the active groups are introduced and the conjugated system on the surface of the graphene is destroyed, so that the good conductivity of the graphene is certainly weakened, and the more the modification groups are introduced, the larger the loss of the electronic conductivity of the graphene is. If the functional groups are only introduced at the edges of the graphene, the conjugated system on the surface of the graphene is not destroyed, so that the basic performance of the graphene is ensured. Thus, active groups are introduced and the performance of the graphene can be ensured. However, such selectively modified graphene is difficult to prepare. At present, few application documents are reported. The method of ball milling graphite and dry ice in US 2013/0018204 A1 can be used for modifying carboxyl at the edge of a graphite sheet, firstly preparing graphite with the carboxyl modified at the edge, and dispersing the graphite with the carboxyl modified at the edge in water after introducing enough carboxyl to obtain the graphene with the carboxyl modified at the edge. In the method, enough strong polar groups (i.e. modified edge carboxyl groups) are required to be introduced, and water is required to be added to peel off graphite into graphene, and the obtained graphene has a nano-scale size and is easy to agglomerate when being blended with a polymer, so that the antistatic effect is affected.
Disclosure of Invention
The invention aims to solve the problems of poor antistatic performance, high antistatic agent addition amount, destroyed structure after graphene functionalization and the like of a polypropylene material in the prior art, and provides a novel antistatic polypropylene film, and a preparation method and application of the antistatic polypropylene film. The antistatic polypropylene film provided by the invention uses a polypropylene material as a base resin, uses edge modified graphene as a long-acting antistatic agent, and simultaneously adds a compatilizer. The antistatic polypropylene film has good antistatic property and mechanical property.
The first aspect of the invention provides an antistatic polypropylene film, which comprises polypropylene, edge modified graphene and an auxiliary agent, wherein the content of the edge modified graphene is 0.05-5 parts by weight, preferably 0.1-2 parts by weight, and the content of the auxiliary agent is 0.1-20 parts by weight, preferably 0.5-15 parts by weight, based on 100 parts by weight of polypropylene; the auxiliary agent comprises a compatilizer;
the edge-modified graphene has the following characteristics:
the average sheet diameter is 2-30 μm, preferably 5-15 μm; and/or
Average aspect ratio of 600-10000:1, preferably 1200-4500:1, more preferably 1500-3800:1, a step of; and/or
The conductivity is 200-800S/m, preferably 300-600S/m; and/or
In the edge modified graphene, the oxygen content calculated by oxygen element is 3-30at%, preferably 5-18at%; the hydrogen content is 1 to 10at%, preferably 3 to 8at%, in terms of hydrogen element.
The second aspect of the invention provides a preparation method of the antistatic polypropylene film, which comprises the steps of mixing polypropylene, edge modified graphene and an auxiliary agent, granulating, casting and stretching to form a film.
A third aspect of the present invention provides the use of the above antistatic polypropylene film in the field of packaging materials.
The edge modified graphene used in the invention can react with groups in the compatilizer, so that the compatibility of the matrix and the edge modified graphene is improved, the edge modified graphene can be more effectively dispersed in polypropylene, and the prepared antistatic polypropylene film has good antistatic performance and mechanical property.
Additional features and advantages of the invention will be set forth in the detailed description which follows.
Detailed Description
The following describes specific embodiments of the present invention in detail. It should be understood that the detailed description and specific examples, while indicating and illustrating the invention, are not intended to limit the invention.
The invention provides an antistatic polypropylene film which comprises polypropylene, edge modified graphene and an auxiliary agent, wherein the content of the edge modified graphene is 0.05-5 parts by weight, preferably 0.1-2 parts by weight, and the content of the auxiliary agent is 0.1-20 parts by weight, preferably 0.5-15 parts by weight, based on 100 parts by weight of polypropylene; the auxiliary agent comprises a compatilizer;
the edge-modified graphene has the following characteristics:
the average sheet diameter is 2-30 μm, preferably 5-15 μm; and/or
Average aspect ratio of 600-10000:1, preferably 1200-4500:1, more preferably 1500-3800:1, a step of; and/or
The conductivity is 200-800S/m, preferably 300-600S/m; and/or
In the edge modified graphene, the oxygen content calculated by oxygen element is 3-30at%, preferably 5-18at%; the hydrogen content is 1 to 10at%, preferably 3 to 8at%, in terms of hydrogen element.
The edge modified graphene has the sheet diameter size of micron level, has adjustable aspect ratio and content of carbon and oxygen elements, has higher conductivity, can be obviously different from the existing nanoscale graphene (such as US 20130018204), and can overcome the problem that the nanoscale graphene is easy to aggregate.
In the present invention, the "aspect ratio" refers to the ratio of the long side (sheet diameter) to the thickness of graphene.
According to the present invention, preferably, the edge-modified graphene is prepared by grinding graphite by a grinding disc under supercritical carbon dioxide.
Under the condition of supercritical carbon dioxide, the property of the carbon dioxide is greatly changed, the density is close to that of liquid, the viscosity is close to that of gas, and the diffusion coefficient is 100 times that of liquid. The inventor of the present invention has found that in this state, carbon dioxide is intercalated into the graphite flake layers, pi-pi interaction between the graphite flake layers is reduced, and graphite is exfoliated into graphene after it is sheared by the grinding disc; meanwhile, graphite or graphene is crushed by the shearing action of the grinding disc, the newly generated high-activity edge reacts with carbon dioxide, and as a result, carboxyl groups are modified at the edge of the graphene. Compared with the common ball milling method, the method can prepare the graphene with carboxylated edges without grinding graphite to be particularly fine, and the common ball milling method has to grind the graphite to the nano-scale, otherwise, the graphene cannot be prepared.
The edge modified graphene provided by the invention is prepared by a method comprising the following steps: the graphite powder is milled in a high pressure millstone kettle in the presence of supercritical carbon dioxide.
According to a specific embodiment of the invention, the edge-modified graphene is prepared by a method comprising the following steps:
step S1, adding purified or unpurified graphite powder into a high-pressure millstone kettle;
step S2, introducing carbon dioxide into a high-pressure millstone kettle, and enabling the carbon dioxide to be in a supercritical state to form a material containing graphite powder and supercritical carbon dioxide;
and step S3, grinding the material containing graphite powder and supercritical carbon dioxide.
According to some embodiments of the invention, the graphite powder is selected from the group consisting of crystalline flake graphite powder and expanded graphite powder, preferably the graphite powder has a particle size of 10-80 mesh, preferably 20-60 mesh.
According to some embodiments of the present invention, the graphite powder is preferably subjected to a purification treatment in advance, such as by ultrasonic cleaning and/or chemical treatment, to remove impurities, such as impurity substances and impurity elements, prior to grinding.
According to some embodiments of the invention, in step S2, carbon dioxide is brought into a supercritical state by bringing the temperature inside the tank to over 32.26 ℃ and the pressure to over 72.9 atm.
According to some embodiments of the invention, in step S3, after finishing the grinding, the pressure in the high-pressure millstone kettle is rapidly reduced; preferably, the pressure in the autoclave is reduced to below 1atm in 5-20 seconds.
According to some embodiments of the invention, the temperature in the autoclave is 35-200 ℃, preferably 35-100 ℃, more preferably 35-70 ℃. According to some embodiments of the invention, the pressure in the autoclave is 75-165atm, preferably 75-165atm, more preferably 75-125atm. According to some embodiments of the invention, the stirring speed in the high-pressure millstone kettle is 500-10000r/min, preferably 500-5000r/min. According to some embodiments of the invention, the milling time is from 6 to 48 hours.
Through the setting of the specific grinding conditions, the prepared edge modified graphene can meet the structural and performance characteristics.
In the invention, the graphite and the supercritical carbon dioxide can be fully mixed by adopting a high-pressure millstone kettle, and the graphite is ground and peeled off. According to a preferred embodiment of the invention, the high-pressure millstone kettle is a self-circulation millstone device used in a high-pressure environment.
The edge modified graphene used in the invention has carboxyl modified groups, the sheet integrity is good, a good conductive network is easy to form, supercritical carbon dioxide is used as a solvent in the preparation of the graphene, and the preparation method is green and environment-friendly and has low production cost; meanwhile, the method has the advantages of short reaction period, simple process and the like.
Due to the characteristics, compared with the existing graphene antistatic agent, the edge modified graphene adopted by the invention can achieve more excellent antistatic effect under the condition of less addition.
According to a preferred embodiment of the present invention, the compatibilizer is a polypropylene graft, preferably a polypropylene polar graft, more preferably at least one of maleic anhydride grafted polypropylene (PP-g-MAH), styrene grafted polypropylene (PP-g-St), maleic anhydride/styrene grafted polypropylene (PP-g-MAH-St), glycidyl methacrylate grafted polypropylene (PP-g-GMA), dibutyl maleate grafted polypropylene (PP-g-DBM), acrylic acid grafted polypropylene (PP-g-AA), methyl methacrylate grafted polypropylene (PP-g-MMA), butyl methacrylate grafted polypropylene (PP-g-BMA); the graft ratio of the polypropylene graft is preferably 0.5 to 6wt%, more preferably 1 to 3wt%.
According to the present invention, the content of the compatibilizer is preferably 0.5 to 10 parts by weight based on 100 parts by weight of polypropylene.
According to some embodiments of the invention, the auxiliary agent comprises a coupling agent, preferably a silane coupling agent and/or a titanate coupling agent; the coupling agent is contained in an amount of 0.1 to 2 parts by weight based on 100 parts by weight of polypropylene. The silane coupling agents include, but are not limited to, KH570, KH792, DL602, KH550. The titanate coupling agents include, but are not limited to TMC-201, TMC101, TMC105.
In the present invention, an antioxidant is preferably further contained in order to improve the oxidation resistance of the antistatic film during processing. The antioxidant may be any of various antioxidants commonly used in the art, and is not particularly limited.
The antioxidant can be at least one selected from hindered phenol antioxidants, phosphate antioxidants and thioester antioxidants.
The hindered phenol antioxidant may be at least one selected from pentaerythritol tetrakis [ beta- (3, 5-di-t-butyl-4-hydroxyphenyl) propionate (antioxidant 1010), N-stearyl beta- (3, 5-di-t-butyl-4-hydroxyphenyl) propionate (antioxidant 1076), N' -bis- (3, 5-di-t-butyl-4-hydroxyphenyl) propionyl) hexamethylenediamine (antioxidant 1098) and 1,3, 5-tris (3, 5-di-t-butyl-4-hydroxybenzyl) isocyanuric acid (antioxidant 3114).
The phosphate antioxidant may be selected from tris (2, 4-di-tert-butylphenol) phosphite (antioxidant 168) and/or bis (2, 4-di-tert-butylphenol) pentaerythritol diphosphite (antioxidant 626).
The thioester antioxidant can be DLTP or DSTP.
Preferably, the antioxidant is a mixture of hindered phenol antioxidants and phosphate antioxidants, and the weight ratio of the hindered phenol antioxidants to the phosphate antioxidants is 1: (1 to 8), preferably 1: (1 to 6), more preferably 1: (1-4).
According to the present invention, the antioxidant is preferably contained in an amount of 0.1 to 0.8 parts by weight, preferably 0.2 to 0.4 parts by weight, based on 100 parts by weight of polypropylene.
According to the invention, other auxiliary agents commonly used in the art, such as nucleating agents, flame retardants, ultraviolet absorbers and the like, can be added according to actual needs, and the dosage is also conventional.
The invention also provides a preparation method of the antistatic polypropylene film, which comprises the steps of mixing polypropylene, edge modified graphene and an auxiliary agent, granulating and preparing a film.
The method of forming the pellets into a polymer film may be performed with reference to the prior art, and for example, the pellets may be processed by an extrusion casting method or processed by a biaxially stretching method, thereby producing the antistatic film of the present invention.
The antistatic film is mainly used in the packaging field with antistatic requirements, such as the battery packaging field or the electronic product packaging field.
The present invention will be further described with reference to examples, but the scope of the present invention is not limited to these examples.
The test method and the equipment used in the test are as follows:
(1) The average sheet diameter and aspect ratio of the graphene were determined by Scanning Electron Microscopy (SEM), available from FEI company under the model XL-30.
(2) The oxygen and hydrogen content was measured using XPS equipment available from Thermo Fisher Scientific under the model ESCALAB250.
(3) Determination of the conductivity of edge modified graphene powder resistivity conductivity tester, available from Ningborrelike West instruments Inc., model FT-300, was used as described in DB 13/T2768.3-2018.
(4) The tensile strength, elongation at break and tensile modulus of elasticity of the film were measured according to the methods specified in GB/T1040.3-2006.
(5) Film surface resistivity was measured by a Keithley 6517B Electrometer.
Example 1
Ultrasonically cleaning 100g of 32-mesh flake graphite powder (1 time of water cleaning and 2 times of ethanol cleaning) to remove impurity substances and impurity elements, placing the flake graphite in a high-pressure millstone kettle, sealing the high-pressure millstone kettle, heating the high-pressure millstone kettle to 40 ℃, and pumping CO 2 And (3) raising the pressure in the high-pressure millstone kettle to 85atm at the rotating speed of 500r/min, grinding and stripping graphite by utilizing the shearing force generated by the millstone, reducing the pressure to 1atm within 10s after stirring for 24h, and sampling from the high-pressure millstone kettle to obtain the edge modified graphene G1. The graphene has an average sheet diameter of 12.6 μm, an average thickness of 3.4nm, and an average aspect ratio of 3706, as analyzed by Scanning Electron Microscopy (SEM): 1, X-ray photoelectron spectroscopy (XPS) characterization, oxygen content of 5.60at%, hydrogen content of 3.22at%, conductivity of 506S/m.
The polypropylene (homo-polypropylene T30S, shanghai petrochemical), the PP-G-MAH (self-made, the grafting rate is 2.3 wt%), the edge modified graphene G1, the silane coupling agent KH550 and the antioxidant (the antioxidant 1010 is compounded with the antioxidant 168 in a weight ratio of 1:1) are premixed according to a proportion, wherein the addition amount of the PP-G-MAH is 5 parts by weight, the addition amount of the G1 is 1 part by weight, the addition amount of the silane coupling agent is 0.5 part by weight and the addition amount of the antioxidant is 0.3 part by weight based on 100 parts by weight of the polypropylene. After premixing, granulating, casting and biaxially stretching according to a conventional film preparation method to obtain the antistatic polypropylene film, wherein the thickness of the film is 20.1 mu m, and the mechanical properties and the electrical properties are shown in Table 1.
Example 2
Ultrasonically cleaning 100g of 32-mesh flake graphite powder (1 time of water cleaning and 2 times of ethanol cleaning) to remove impurity substances and impurity elements, placing the flake graphite in a high-pressure millstone kettle, sealing the high-pressure millstone kettle, heating the high-pressure millstone kettle to 70 ℃, and pumping CO 2 The pressure in the high-pressure millstone kettle is increased to 125atm, the rotating speed is 1000r/min, graphite is ground and peeled off by utilizing the shearing force generated by the millstone, the pressure is reduced to 1atm within 10 seconds after stirring for 24 hours, and the pressure is increased to the pressure of the graphiteSampling in the autoclave disc to obtain the edge modified graphene G2. The graphene has an average sheet diameter of 6.2 μm, an average thickness of 2.9nm, and an average aspect ratio of 2138 as analyzed by Scanning Electron Microscopy (SEM): 1, X-ray photoelectron spectroscopy (XPS) characterization, oxygen content 13.40at%, hydrogen content 7.3at% and conductivity 339S/m.
Polypropylene (homo-polypropylene FA03, china petrochemical), PP-G-St (self-made, grafting rate is 2.1 wt%), edge modified graphene G2, a silane coupling agent KH550 and an antioxidant (the antioxidant 1010 is compounded with the antioxidant 168, and the weight ratio is 1:1) are premixed according to a proportion, wherein the addition amount of the PP-G-St is 5 parts by weight, the addition amount of the G2 is 0.5 part by weight, the addition amount of the silane coupling agent is 0.5 part by weight and the addition amount of the antioxidant is 0.3 part by weight based on 100 parts by weight of polypropylene. After premixing, granulating, casting and biaxially stretching according to a conventional film preparation method to obtain the antistatic polypropylene film, wherein the thickness of the film is 20.3 mu m, and the mechanical properties and the electrical properties are shown in Table 1.
Example 3
40g of 32-mesh expanded graphite powder is ultrasonically cleaned (water-cleaned for 1 time and ethanol-cleaned for 2 times) to remove impurity substances and impurity elements, then the expanded graphite powder is placed in a high-pressure millstone kettle, the high-pressure millstone kettle is sealed, then the high-pressure millstone kettle is heated to 40 ℃, and CO is pumped in 2 And (3) raising the pressure in the high-pressure millstone kettle to 85atm at the rotating speed of 500r/min, grinding and stripping graphite by utilizing the shearing force generated by the millstone, reducing the pressure to 1atm within 10s after stirring for 48h, and sampling from the high-pressure millstone kettle to obtain the edge modified graphene G3. The graphene has an average sheet diameter of 9.6 μm, an average thickness of 3.2nm, and an average aspect ratio of 3000, as analyzed by Scanning Electron Microscopy (SEM): 1, X-ray photoelectron spectroscopy (XPS) characterization, oxygen content of 7.83at%, hydrogen content of 3.23at% and conductivity of 425S/m.
Polypropylene (homo-polypropylene F300M, petrochemical name), PP-G-AA (self-made, grafting rate is 1.8 wt%), edge modified graphene G3, a silane coupling agent KH550 and an antioxidant (the antioxidant 1010 is compounded with the antioxidant 168, 1:1 weight ratio) are premixed according to a proportion, wherein the addition amount of the PP-G-AA is 8 weight parts, the addition amount of the G3 is 1.5 weight parts, the addition amount of the silane coupling agent is 0.5 weight part and the addition amount of the antioxidant is 0.3 weight part based on 100 weight parts of polypropylene. After premixing, granulating, casting and biaxially stretching according to a conventional film preparation method to obtain the antistatic polypropylene film, wherein the thickness of the film is 20.1 mu m, and the mechanical properties and the electrical properties are shown in Table 1.
Example 4
The difference is that no silane coupling agent was added, and the surface conductivity and mechanical properties of the obtained film are shown in Table 1.
Comparative example 1
The difference from example 1 is that the edge-modified graphene was replaced with an equal weight of chemically exfoliated graphene (purchased from nanjibin nanotechnology limited), and the surface conductivity and mechanical properties of the resulting film are listed in table 1.
Comparative example 2
The difference in example 1 is that no grafted polypropylene is added and the surface conductivity and mechanical properties of the resulting film are shown in Table 1.
Comparative example 3
The difference from example 1 is that an equal weight of carbon black is used instead of edge modified graphene and the surface conductivity and mechanical properties of the resulting film are listed in table 1.
TABLE 1 mechanical and electrical Property results
The foregoing description of embodiments of the invention has been presented for purposes of illustration and description, and is not intended to be exhaustive or limited to the embodiments disclosed. Many modifications and variations will be apparent to those of ordinary skill in the art without departing from the scope and spirit of the various embodiments described.
The endpoints and any values of the ranges disclosed herein are not limited to the precise range or value, and are understood to encompass values approaching those ranges or values. For numerical ranges, one or more new numerical ranges may be found between the endpoints of each range, between the endpoint of each range and the individual point value, and between the individual point value, in combination with each other, and are to be considered as specifically disclosed herein.
Claims (10)
1. The antistatic polypropylene film is characterized by comprising polypropylene, edge modified graphene and an auxiliary agent, wherein the content of the edge modified graphene is 0.05-5 parts by weight, preferably 0.1-2 parts by weight, and the content of the auxiliary agent is 0.1-20 parts by weight, preferably 0.5-15 parts by weight, based on 100 parts by weight of polypropylene; the auxiliary agent comprises a compatilizer;
the edge-modified graphene has the following characteristics:
the average sheet diameter is 2-30 μm, preferably 5-15 μm; and/or
Average aspect ratio of 600-10000:1, preferably 1200-4500:1, more preferably 1500-3800:1, a step of; and/or
The conductivity is 200-800S/m, preferably 300-600S/m; and/or
In the edge modified graphene, the oxygen content calculated by oxygen element is 3-30at%, preferably 5-18at%; the hydrogen content is 1 to 10at%, preferably 3 to 8at%, in terms of hydrogen element.
2. The antistatic polypropylene film according to claim 1, wherein the edge modified graphene is prepared by grinding graphite by a grinding disc under supercritical carbon dioxide; preferably, the edge-modified graphene is prepared by a method comprising the steps of: grinding graphite powder in a high-pressure millstone kettle in the presence of supercritical carbon dioxide;
the graphite powder is preferably selected from flake graphite powder and/or expanded graphite powder, more preferably the particle size of the graphite powder is 10-80 mesh, preferably 20-60 mesh.
3. The antistatic polypropylene film according to claim 2 wherein said edge modified graphene is made by a process comprising the steps of:
step S1, adding purified or unpurified graphite powder into a high-pressure millstone kettle;
step S2, introducing carbon dioxide into a high-pressure millstone kettle, and enabling the carbon dioxide to be in a supercritical state to form a material containing graphite powder and supercritical carbon dioxide;
step S3, grinding a material containing graphite powder and supercritical carbon dioxide;
preferably, in step S2, carbon dioxide is brought into a supercritical state by bringing the temperature in the tank to over 32.26 ℃ and the pressure to over 72.9 atm;
preferably, in step S3, after finishing the grinding, the pressure in the high-pressure millstone kettle is rapidly reduced; preferably, the pressure in the high-pressure millstone kettle is reduced to below 1atm in 5-20 seconds;
preferably, the temperature in the high-pressure millstone kettle is 35-200 ℃, preferably 35-100 ℃, more preferably 35-70 ℃; the pressure is 75 to 165atm, preferably 75 to 150atm, more preferably 75 to 125atm; the stirring speed is 500-10000r/min, preferably 500-5000r/min; the grinding time is 6-48 hours.
4. An antistatic polypropylene film according to any one of claims 1 to 3 wherein said compatibilizer is a polypropylene graft, preferably a polypropylene polar graft, more preferably at least one of maleic anhydride grafted polypropylene, styrene grafted polypropylene, maleic anhydride/styrene grafted polypropylene, glycidyl methacrylate grafted polypropylene, dibutyl maleate grafted polypropylene, acrylic acid grafted polypropylene, methyl methacrylate grafted polypropylene, butyl methacrylate grafted polypropylene; the graft ratio of the polypropylene graft is preferably 0.5 to 6wt%, more preferably 1 to 3wt%.
5. An antistatic polypropylene film according to any one of claims 1 to 3 wherein said compatibilizer is present in an amount of 0.5 to 10 parts by weight based on 100 parts by weight of polypropylene.
6. An antistatic polypropylene film according to any one of claims 1 to 3 wherein said auxiliary agent comprises a coupling agent, preferably a silane coupling agent and/or a titanate coupling agent; the coupling agent is contained in an amount of 0.1 to 2 parts by weight based on 100 parts by weight of polypropylene.
7. An antistatic polypropylene film according to any one of claims 1 to 3 wherein said auxiliary agent comprises an antioxidant; the antioxidant is contained in an amount of 0.1 to 0.8 parts by weight, preferably 0.2 to 0.4 parts by weight, based on 100 parts by weight of polypropylene.
8. The antistatic polypropylene film according to claim 7, wherein said antioxidant is selected from at least one of hindered phenol type antioxidants, phosphate type antioxidants and thioester type antioxidants;
the hindered phenol antioxidant is preferably at least one of pentaerythritol tetra [ beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate ], N-stearyl beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate, N' -bis- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionyl) hexamethylenediamine and 1,3, 5-tris (3, 5-di-tert-butyl-4-hydroxybenzyl) isocyanurate;
the phosphate antioxidant is preferably tris (2, 4-di-tert-butylphenol) phosphite and/or bis (2, 4-di-tert-butylphenol) pentaerythritol diphosphite.
9. The process for producing an antistatic polypropylene film as claimed in any one of claims 1 to 8, comprising mixing polypropylene, edge-modified graphene and an auxiliary agent, granulating, and producing a film.
10. Use of an antistatic polypropylene film according to any one of claims 1 to 8 in the field of packaging materials, preferably in the field of battery packaging or in the field of electronic product packaging.
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