CN111269493A - Graphene oxide/zinc oxide antistatic polypropylene cast film - Google Patents
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- 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
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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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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
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- C08K2003/2296—Oxides; Hydroxides of metals of zinc
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- 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
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- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/04—Carbon
- C08K3/042—Graphene or derivatives, e.g. graphene oxides
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/08—Ingredients agglomerated by treatment with a binding agent
Abstract
The invention discloses a graphene oxide/zinc oxide antistatic polypropylene cast film and a preparation method thereof, and belongs to the technical field of materials. The raw materials of the graphene oxide/zinc oxide antistatic polypropylene cast film are calculated according to parts by weight; 100 parts of polypropylene resin; 5-15 parts of antistatic master batch; the antistatic master batch is prepared from polypropylene resin, a composite antistatic agent OA/GO-g-ZnO and EVA resin. The composite antistatic agent OA/GO-g-ZnO used in the antistatic master batch combines the antistatic performance of graphene oxide and oleic acid, zinc oxide uniformly grows on the graphene oxide modified by oleic acid functionalization, and agglomeration of the zinc oxide is avoided, so that the obtained polypropylene casting film has a good antistatic effect.
Description
Technical Field
The invention belongs to the technical field of materials, and particularly relates to a graphene oxide/zinc oxide antistatic polypropylene cast film and a preparation method thereof.
Background
Polypropylene (PP) is a semicrystalline polymer, has high rigidity, excellent mechanical properties, good heat resistance and chemical resistance, has properties of no toxicity, easy recovery and the like, and is environment-friendly, so that the polypropylene (PP) is widely concerned by researchers at home and abroad in recent years. However, PP is a highly insulating material and has a volume resistivity of generally 1016～1018Omega. m, surface resistivity of 1016～1017Omega, PP cannot transfer generated static charges due to high surface resistivity and volume resistivity, and serious dangers such as dust collection, discharge, breakdown, even combustion or explosion can be brought after the static charges on the surface are accumulated to a certain degree, so that the application range of PP is greatly limited, and the PP can only be applied to the insulation field in industry or life.
At present, in order to eliminate the static charge accumulated on the surface of the PP, the main methods are as follows: conductive carbon black or a surfactant antistatic agent is added. Surfactants antistatic agents are small molecules with a hydrophilic-lipophilic group structure, and can be classified into anionic, cationic and nonionic types according to their surface activities. After processing and forming, the micromolecules continuously migrate to the surface of the material, and the lipophilic group of the micromolecules faces to the inside of the resin; the hydrophilic groups are arranged towards one side of the air to absorb moisture in the air, and a continuous and uniform conductive layer is formed on the surface of the material to achieve the antistatic effect.
The metal oxide filled antistatic material is one new product developed in recent years and has performance slightly inferior to that of metal filled material but high cost performance. At present, titanium oxide, zinc oxide and the like are successfully applied, wherein tin oxide with good cost performance is also used, the color is light, the particle size is small (less than 0.1 pm), and the requirements of transparency and static electricity prevention can be met.
Graphene is a polymer made of carbon atoms in sp2The honeycomb plane film formed by the hybridization mode is a quasi-two-dimensional material with the thickness of only one atomic layer.Graphene is currently the thinnest and hardest nanomaterial in the world, and is almost completely transparent, absorbing only 2.3% of light; the heat conductivity coefficient is as high as 5300W/m.K, higher than that of carbon nano tube and diamond, and its electron mobility is over 15000cm at normal temp2The resistivity of the material is only about 10-6 omega cm and lower than that of copper or silver, and the material is the material with the minimum resistivity in the world at present. Since the greatest characteristic of graphene is high conductivity, graphene can be used as an excellent antistatic material to improve the antistatic property of a high polymer material.
Disclosure of Invention
The invention aims to provide a graphene oxide/zinc oxide antistatic polypropylene cast film and a preparation method thereof.
In order to achieve the purpose, the invention adopts the following technical scheme:
a graphene oxide/zinc oxide antistatic polypropylene cast film comprises the following raw materials in parts by weight: 100 parts of polypropylene resin, antistatic master batch: 5-15 parts.
Wherein the polypropylene resin has a Melt Flow Rate (MFR) of 6-12g/min, a molecular weight of 10-50 ten thousand, and a relative density of 0.9-0.91g/cm3。
The antistatic master batch is prepared by adding polypropylene resin, composite antistatic agent OA/GO-g-ZnO and EVA resin into a high-speed mixer according to the mass ratio of 5:2:3, uniformly stirring at a high speed of 300r/min at 60 ℃, pumping into a dehumidifying dryer, drying for 4-6h at 50-60 ℃, and extruding and granulating at 190 ℃ to obtain the antistatic master batch.
The preparation method of the composite antistatic agent OA/GO-g-ZnO comprises the following steps:
1) dissolving graphene oxide and polypropylene pyrrolidone in DMF (dimethyl formamide) according to the mass ratio of 1:3, and carrying out condensation reaction at 60 ℃ for 1h in the presence of triethylamine to obtain polypropylene pyrrolidone functionalized modified graphene oxide;
2) ultrasonically dispersing the obtained graphene oxide functionalized and modified by the polypropylene pyrrolidone in oleic acid, performing reflux reaction at 200 ℃ for 10 hours, centrifuging, washing with DMF (dimethyl formamide), and performing centrifugal separation to obtain OA/GO modified by the oil acid functionalization;
3) under magnetic stirring, rapidly adding 0.2mol/L sodium hydroxide solution into 0.1mol/L zinc chloride solution (the molar ratio of zinc chloride to sodium hydroxide in the mixed solution is 1: 2), then adding the OA/GO modified by the oleic acid functionalization prepared in the step 2) at normal temperature, continuing to stir strongly for 3h, centrifuging, washing the product with deionized water and absolute ethyl alcohol in sequence, drying at 70 ℃, and calcining at 200 ℃ for 2h to obtain the OA/GO-g-ZnO composite antistatic agent of the oleic acid functionalized graphene oxide loaded zinc oxide; the mass ratio of OA/GO to ZnO in the obtained composite antistatic agent is 1: 5.
The preparation method of the graphene oxide/zinc oxide antistatic polypropylene cast film comprises the steps of putting polypropylene resin and antistatic master batches into a stirrer in proportion, stirring at a high speed of 300r/min at 60 ℃ to enable the polypropylene resin and the antistatic master batches to be uniform, and then carrying out extrusion casting, cooling, trimming, pressurizing and rolling to obtain a finished product.
The casting is direct casting, the casting roller is a chromium-plated steel roller, the thickness of the chromium-plated layer is 0.01-0.015 mm, the diameter of the steel roller is 500mm, and the height of the steel roller is 0.20-0.25 mm; the temperature of the steel roller is set to be 35-40 ℃.
The pressurization rolling is carried out on a 60-65A liquid silica gel rubber roll, and the pressurization pressure is 5-8 Kgf.
The invention has the following remarkable advantages:
(1) the OA/GO modified graphene oxide with the oil acid function in the composite antistatic agent combines the antistatic performance of the graphene oxide and the oleic acid, and zinc oxide uniformly grows on the OA/GO modified graphene oxide to prevent the zinc oxide from aggregating, so that the obtained polypropylene casting film combines three antistatic materials to show a good antistatic effect.
(2) The composite antistatic agent OA/GO-g-ZnO has good compatibility and dispersibility with PP, the antistatic agent is not easy to migrate, the material can have good antistatic performance under the condition of small amount of addition, the possibility of agglomeration of high molecular materials in the raw materials can be reduced due to the small amount of the antistatic agent, and the quality of products can be guaranteed.
Drawings
Fig. 1 is an XRD comparison graph of oleic acid functionalized graphene oxide and pure graphene oxide obtained in the process of preparing the composite antistatic agent according to the present invention.
FIG. 2 is a SEM comparison of OA/GO-g-ZnO (a) and OA/GO, which are composite antistatic agents prepared in example 1, and a commercially available nano zinc oxide mixture (b). As can be seen from the figure, the agglomeration phenomenon of the nano zinc oxide in the material obtained by mixing OA/GO and the commercially available nano zinc oxide is serious.
FIG. 3 is a SEM comparison of the cast polypropylene film (a) prepared in example 1 and the cast polypropylene film (b) prepared in comparative example. As can be seen from the figure, the film surface prepared by directly using the antistatic master batch prepared by ZnO is rough because ZnO is not uniformly dispersed in the film.
Detailed Description
In order to make the present invention more comprehensible, the technical solutions of the present invention are further described below with reference to specific embodiments, but the present invention is not limited thereto.
The polypropylene resin has Melt Flow Rate (MFR) of 6-12g/min, molecular weight of 10-50 ten thousand, and is colorless, odorless, nontoxic, combustible particles with relative density of 0.9-0.91g/cm3High transparency and good heat resistance.
Example 1
100 parts by weight of polypropylene resin and 5 parts by weight of antistatic master batch are put into a stirrer, stirred at a high speed of 300r/min at 60 ℃ to be uniform, and then subjected to extrusion casting, cooling, edge cutting, pressurization and rolling to obtain a finished product.
The preparation method of the antistatic master batch comprises the steps of adding polypropylene resin, composite antistatic agent OA/GO-g-ZnO and EVA resin into a high-speed mixer according to the mass ratio of 5:2:3, stirring at a high speed of 300r/min at 60 ℃ to enable the mixture to be uniform, pumping the mixture into a dehumidification dryer, drying at 50-60 ℃ for 4-6 hours, and extruding and granulating at 190 ℃ to obtain the antistatic master batch.
The preparation method of the composite antistatic agent OA/GO-g-ZnO comprises the steps of dissolving 150g of graphene oxide and 450g of polypropylene pyrrolidone in 50mL of DMF, and carrying out condensation reaction at 60 ℃ for 1h in the presence of 0.5mL of triethylamine to obtain the graphene oxide functionally modified by the polypropylene pyrrolidone; ultrasonically dispersing the obtained graphene oxide functionalized and modified by the polypropylene pyrrolidone in 50mL of oleic acid, carrying out reflux reaction at 200 ℃ for 10 hours, centrifuging, washing with DMF (dimethyl formamide), and then carrying out centrifugal separation to obtain OA/GO modified by the oil acid functionalization; under magnetic stirring, quickly adding 100mL and 0.2mol/L sodium hydroxide solution into 100mL and 0.1mol/L zinc chloride solution, then adding the OA/GO (mass ratio of OA/GO to ZnO) of the oleic acid functionalized modified graphene prepared in the step 2) at normal temperature, strongly stirring for 3h, centrifuging, washing the product with deionized water and absolute ethyl alcohol in sequence, drying at 70 ℃, and calcining for 2h at 200 ℃ to obtain the OA/GO-g-ZnO composite antistatic agent with the oleic acid functionalized graphene oxide supported zinc oxide, wherein the mass ratio of OA/GO to ZnO is 1: 5.
The casting is direct casting, the casting roller is a chromium-plated steel roller, the thickness of the chromium-plated layer is 0.01-0.015 mm, the diameter of the steel roller is 500mm, and the height of the steel roller is 0.20-0.25 mm; the temperature of the steel roller is set to be 35-40 ℃.
The pressurization rolling is carried out on a 60-65A liquid silica gel rubber roll, and the pressurization pressure is 5 Kgf.
Example 2
100 parts by weight of polypropylene resin and 10 parts by weight of antistatic master batch are put into a stirrer, stirred at a high speed of 300r/min at 60 ℃ to be uniform, and then subjected to extrusion casting, cooling, edge cutting, pressurization and rolling to obtain a finished product.
The preparation method of the antistatic master batch comprises the steps of adding polypropylene resin, composite antistatic agent OA/GO-g-ZnO and EVA resin into a high-speed mixer according to the mass ratio of 5:2:3, stirring at a high speed of 300r/min at 60 ℃ to enable the mixture to be uniform, pumping the mixture into a dehumidification dryer, drying at 50-60 ℃ for 4-6 hours, and extruding and granulating at 190 ℃ to obtain the antistatic master batch.
The preparation method of the composite antistatic agent OA/GO-g-ZnO comprises the steps of dissolving 150g of graphene oxide and 450g of polypropylene pyrrolidone in 50mL of DMF, and carrying out condensation reaction at 60 ℃ for 1h in the presence of 0.5mL of triethylamine to obtain the graphene oxide functionally modified by the polypropylene pyrrolidone; ultrasonically dispersing the obtained graphene oxide functionalized and modified by the polypropylene pyrrolidone in 50mL of oleic acid, carrying out reflux reaction at 200 ℃ for 10 hours, centrifuging, washing with DMF (dimethyl formamide), and then carrying out centrifugal separation to obtain OA/GO modified by the oil acid functionalization; under magnetic stirring, quickly adding 100mL and 0.2mol/L sodium hydroxide solution into 100mL and 0.1mol/L zinc chloride solution, then adding the oleic acid functionalized modified graphene OA/GO prepared in the step 2) at normal temperature, strongly stirring for 3h, centrifuging, washing the product with deionized water and absolute ethyl alcohol in sequence, drying at 70 ℃, and calcining at 200 ℃ for 2h to obtain the composite antistatic agent OA/GO-g-ZnO with the oleic acid functionalized graphene oxide carrying zinc oxide, wherein the mass ratio of OA/GO to ZnO is 1: 5.
The casting is direct casting, the casting roller is a chromium-plated steel roller, the thickness of the chromium-plated layer is 0.01-0.015 mm, the diameter of the steel roller is 500mm, and the height of the steel roller is 0.20-0.25 mm; the temperature of the steel roller is set to be 35-40 ℃.
The pressurization rolling is carried out on a 60-65A liquid silica gel rubber roll, and the pressurization pressure is 5 Kgf.
Example 3
100 parts by weight of polypropylene resin and 15 parts by weight of antistatic master batch are put into a stirrer, stirred at a high speed of 300r/min at 60 ℃ to be uniform, and then subjected to extrusion casting, cooling, edge cutting, pressurization and rolling to obtain a finished product.
The preparation method of the antistatic master batch comprises the steps of adding polypropylene resin, composite antistatic agent OA/GO-g-ZnO and EVA resin into a high-speed mixer according to the mass ratio of 5:2:3, stirring at a high speed of 300r/min at 60 ℃ to enable the mixture to be uniform, pumping the mixture into a dehumidification dryer, drying at 50-60 ℃ for 4-6 hours, and extruding and granulating at 190 ℃ to obtain the antistatic master batch.
The preparation method of the composite antistatic agent OA/GO-g-ZnO comprises the steps of dissolving 150g of graphene oxide and 450g of polypropylene pyrrolidone in 50mL of DMF, and carrying out condensation reaction at 60 ℃ for 1h in the presence of 0.5mL of triethylamine to obtain the graphene oxide functionally modified by the polypropylene pyrrolidone; ultrasonically dispersing the obtained graphene oxide functionalized and modified by the polypropylene pyrrolidone in 50mL of oleic acid, carrying out reflux reaction at 200 ℃ for 10 hours, centrifuging, washing with DMF (dimethyl formamide), and then carrying out centrifugal separation to obtain OA/GO modified by the oil acid functionalization; under magnetic stirring, quickly adding 100mL and 0.2mol/L sodium hydroxide solution into 100mL and 0.1mol/L zinc chloride solution, then adding the oleic acid functionalized modified graphene OA/GO prepared in the step 2) at normal temperature, strongly stirring for 3h, centrifuging, washing the product with deionized water and absolute ethyl alcohol in sequence, drying at 70 ℃, and calcining at 200 ℃ for 2h to obtain the composite antistatic agent OA/GO-g-ZnO with the oleic acid functionalized graphene oxide carrying zinc oxide, wherein the mass ratio of OA/GO to ZnO is 1: 5.
The casting is direct casting, the casting roller is a chromium-plated steel roller, the thickness of the chromium-plated layer is 0.01-0.015 mm, the diameter of the steel roller is 500mm, and the height of the steel roller is 0.20-0.25 mm; the temperature of the steel roller is set to be 35-40 ℃.
The pressurization rolling is carried out on a 60-65A liquid silica gel rubber roll, and the pressurization pressure is 5 Kgf.
Comparative example
100 parts by weight of polypropylene resin and 5 parts by weight of antistatic master batch are put into a stirrer, stirred at a high speed of 300r/min at 60 ℃ to be uniform, and then subjected to extrusion casting, cooling, edge cutting, pressurization and rolling to obtain a finished product.
The preparation method of the antistatic master batch comprises the steps of adding polypropylene resin, composite antistatic agent OA/GO, commercially available nano zinc oxide and EVA resin into a high-speed mixer according to the mass ratio of 15:1:5:9, stirring at a high speed of 300r/min at 60 ℃ to enable the mixture to be uniform, pumping the mixture into a dehumidification dryer, drying at 50-60 ℃ for 4-6 hours, and extruding and granulating at 190 ℃ to obtain the antistatic master batch.
The preparation method of the composite antistatic agent OA/GO comprises the steps of dissolving 150g of graphene oxide and 450g of polypropylene pyrrolidone in 50mL of DMF, and carrying out condensation reaction at 60 ℃ for 1h in the presence of 0.5mL of triethylamine to obtain the graphene oxide functionally modified by the polypropylene pyrrolidone; ultrasonically dispersing the obtained graphene oxide functionalized and modified by the polypropylene pyrrolidone in 50mL of oleic acid, carrying out reflux reaction at 200 ℃ for 10 hours, centrifuging, washing with DMF, and then carrying out centrifugal separation to obtain the oleic acid functionalized and modified graphene OA/GO.
The casting is direct casting, the casting roller is a chromium-plated steel roller, the thickness of the chromium-plated layer is 0.01-0.015 mm, the diameter of the steel roller is 500mm, and the height of the steel roller is 0.20-0.25 mm; the temperature of the steel roller is set to be 35-40 ℃.
The pressurization rolling is carried out on a 60-65A liquid silica gel rubber roll, and the pressurization pressure is 5 Kgf.
The mechanical properties of the obtained film material were tested according to the GB44552006 standard, and the results are shown in Table 1.
TABLE 1
The surface resistivity of the obtained membrane material is tested according to GB/T1410-2006, and the result is shown in Table 2.
TABLE 2
The above description is only a preferred embodiment of the present invention, and all equivalent changes and modifications made in accordance with the claims of the present invention should be covered by the present invention.
Claims (8)
1. The utility model provides an antistatic polypropylene curtain coating film of oxidation graphite alkene/zinc oxide which characterized in that: the raw materials comprise the following components in parts by weight: 100 parts of polypropylene resin, antistatic master batch: 5-15 parts.
2. The graphene oxide/zinc oxide antistatic polypropylene cast film according to claim 1, characterized in that: the melt flow rate of the polypropylene resin is 6-12g/min, the molecular weight is 10-50 ten thousand, and the relative density is 0.9-0.91g/cm3。
3. The graphene oxide/zinc oxide antistatic polypropylene cast film according to claim 1, characterized in that: the antistatic master batch is prepared by adding polypropylene resin, composite antistatic agent OA/GO-g-ZnO and EVA resin into a high-speed mixer according to the mass ratio of 5:2:3, uniformly stirring at a high speed of 300r/min at 60 ℃, pumping into a dehumidifying dryer, drying for 4-6h at 50-60 ℃, and extruding and granulating at 190 ℃ to obtain the antistatic master batch.
4. The graphene oxide/zinc oxide antistatic polypropylene cast film according to claim 3, wherein: the preparation method of the composite antistatic agent OA/GO-g-ZnO comprises the following steps:
1) dissolving graphene oxide and polypropylene pyrrolidone in DMF (dimethyl formamide) according to the mass ratio of 1:3, and carrying out condensation reaction at 60 ℃ for 1h in the presence of triethylamine to obtain polypropylene pyrrolidone functionalized modified graphene oxide;
2) ultrasonically dispersing the obtained graphene oxide functionalized and modified by the polypropylene pyrrolidone in oleic acid, performing reflux reaction at 200 ℃ for 10 hours, centrifuging, washing with DMF (dimethyl formamide), and performing centrifugal separation to obtain OA/GO modified by the oil acid functionalization;
3) rapidly adding a sodium hydroxide solution into a zinc chloride solution under magnetic stirring, then adding the oleic acid functionalized modified graphene OA/GO prepared in the step 2) at normal temperature, continuously and intensively stirring for 3h, centrifuging, washing a product by deionized water and absolute ethyl alcohol in sequence, drying at 70 ℃, and calcining at 200 ℃ for 2h to obtain an oleic acid functionalized graphene oxide zinc oxide-loaded composite antistatic agent OA/GO-g-ZnO;
the mass ratio of OA/GO to ZnO in the obtained composite antistatic agent is 1: 5.
5. The graphene oxide/zinc oxide antistatic polypropylene cast film according to claim 4, wherein: the concentration of the zinc chloride solution in the step 3) is 0.1mol/L, the concentration of the sodium hydroxide solution is 0.2mol/L, and the molar ratio of the zinc chloride to the sodium hydroxide is 1: 2.
6. The graphene oxide/zinc oxide antistatic polypropylene cast film according to claim 1, characterized in that: the preparation method of the graphene oxide/zinc oxide antistatic polypropylene cast film comprises the steps of putting polypropylene resin and antistatic master batches into a stirrer in proportion, stirring at a high speed of 300r/min at 60 ℃ to enable the polypropylene resin and the antistatic master batches to be uniform, and then carrying out extrusion casting, cooling, trimming, pressurizing and rolling to obtain a finished product.
7. The graphene oxide/zinc oxide antistatic polypropylene cast film according to claim 6, wherein: the casting is direct casting, the casting roller is a chromium-plated steel roller, the thickness of the chromium-plated layer is 0.01-0.015 mm, the diameter of the steel roller is 500mm, and the height of the steel roller is 0.20-0.25 mm; the temperature of the steel roller is set to be 35-40 ℃.
8. The graphene oxide/zinc oxide antistatic polypropylene cast film according to claim 7, wherein: the pressurization rolling is carried out on a 60-65A liquid silica gel rubber roll, and the pressurization pressure is 5-8 Kgf.
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| CN114456478A (en) * | 2022-02-21 | 2022-05-10 | 山东星达新材料有限公司 | Antistatic master batch for plastics and plastic film containing antistatic master batch |
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| CN111676085A (en) * | 2020-06-30 | 2020-09-18 | 佛山市南海区里水镇经济促进局 | Graphene lubricating oil for robot and preparation method and application thereof |
| CN114456478A (en) * | 2022-02-21 | 2022-05-10 | 山东星达新材料有限公司 | Antistatic master batch for plastics and plastic film containing antistatic master batch |
| CN114456478B (en) * | 2022-02-21 | 2024-03-08 | 山东星达新材料有限公司 | Antistatic master batch for plastics and plastic film containing same |
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