CN115433408A - Graphene-polypropylene composite antibacterial master batch and preparation method and application thereof - Google Patents
Graphene-polypropylene composite antibacterial master batch and preparation method and application thereof Download PDFInfo
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- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/20—Compounding polymers with additives, e.g. colouring
- C08J3/22—Compounding polymers with additives, e.g. colouring using masterbatch techniques
- C08J3/226—Compounding polymers with additives, e.g. colouring using masterbatch techniques using a polymer as a carrier
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2423/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
- C08J2423/02—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
- C08J2423/10—Homopolymers or copolymers of propene
- C08J2423/12—Polypropene
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2479/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing nitrogen with or without oxygen, or carbon only, not provided for in groups C08J2461/00 - C08J2477/00
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- 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
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- 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
- C08K5/00—Use of organic ingredients
- C08K5/16—Nitrogen-containing compounds
- C08K5/29—Compounds containing one or more carbon-to-nitrogen double bonds
- C08K5/31—Guanidine; Derivatives thereof
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- 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
- C08K9/04—Ingredients treated with organic substances
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- 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
- C08K9/12—Adsorbed ingredients, e.g. ingredients on carriers
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Abstract
The invention discloses a graphene-polypropylene composite antibacterial master batch and a preparation method and application thereof. The preparation method comprises the following steps: s1: grafting a hydrophobic molecule chain segment on graphene oxide; s2: and (3) premixing, extruding, granulating and compounding the graphene oxide grafted on the hydrophobic molecular chain section, the antibacterial agent and the polypropylene to obtain the graphene-polypropylene composite antibacterial master batch with two phases being completely compatible. Graphene oxide with hydrophobic molecular chain segments grafted on the surface is used for losing the hydrophilicity of GO, meanwhile, the compatibility of Modified Graphene Oxide (MGO) and organic polymer base materials such as PP and the like is enhanced, the interfacial energy of a composite system is reduced due to the interaction between the surface modified graphene oxide filler and the polypropylene base materials, and the graphene-polypropylene composite antibacterial master batch with two phases which are completely compatible can be obtained through simple extrusion, granulation, melting and compounding. The film and the non-woven fabric produced by the composite master batch prepared by the invention have the excellent characteristics of high mechanical strength, antibiosis and the like without subsequent treatment.
Description
Technical Field
The invention relates to the technical field of composite materials, and particularly relates to a graphene-polypropylene composite antibacterial master batch and a preparation method and application thereof.
Background
In recent years, in the field of graphene-polypropylene antibacterial materials, prepared graphene slurry is mainly fixed on the surface of polypropylene through impregnation, spraying and other modes to prepare a graphene-polypropylene antibacterial functional material, or modified graphene is premixed with polypropylene and extruded for granulation, for example, chinese patent with application number CN112175286B discloses a graphene-polypropylene composite master batch and a preparation method and application thereof, and the preparation method comprises the following steps: adding a dimethylbenzene solution containing a compatilizer into the graphene dispersion liquid, stirring, mixing and irradiating to obtain compatilizer grafted graphene particles; and premixing the graphene particles grafted by the compatilizer and polypropylene, and extruding and granulating to obtain the graphene-polypropylene composite master batch. However, the method has complex steps, organic solvents exist in the graphene modification preparation process, certain pollution is caused to the environment, the antibacterial capacity of the graphene is not enough, and the application of the graphene in the actual life is limited.
Disclosure of Invention
The invention aims to provide a graphene-polypropylene composite antibacterial master batch, and a preparation method and application thereof, aiming at the defects in the prior art.
The preparation method of the graphene-polypropylene composite antibacterial master batch comprises the following steps:
s1: grafting hydrophobic molecule chain segments on the graphene oxide;
s2: and (3) premixing, extruding, granulating and compounding the graphene oxide grafted on the hydrophobic molecular chain section, the antibacterial agent and the polypropylene to obtain the graphene-polypropylene composite antibacterial master batch with two phases being completely compatible.
Further, the specific process of step S1 is: dropwise adding a surface modifier into a freshly prepared graphene oxide dispersion liquid under constant-temperature stirring, carrying out electrostatic assembly on the modifier and rich oxygen-containing groups on the surface of graphene oxide to form a graphene oxide flocculating solution with the surface subjected to hydrophobic modification, repeatedly washing, and carrying out freeze drying to obtain the graphene oxide structure with the surface grafted with hydrophobic molecular chain segments.
Further, in step S1, the graphene oxide dispersion liquid is an aqueous graphene oxide dispersion liquid prepared by an improved hummers method, and the graphene oxide content is 0.1-10mg/ml.
Further, in step S1, the surfactant is an amphoteric surfactant, and specifically is one or more of lauramidopropyl amine oxide, octadecyl dihydroxyethyl amine oxide, or tetradecyl dihydroxyethyl amine oxide.
Further, in the step S1, the modification of the graphene oxide is carried out at a stirring speed of 250-550rpm, a constant temperature of 30-60 ℃ and a mass ratio of the graphene oxide to the surfactant of 0.5-2.
Further, in step S2, the antibacterial agent is one or more of polyhexamethylene biguanide hydrochloride, polyhexamethylene biguanide hydrochloride or guanidine phosphate.
Further, in the step S1, the mass ratio of the graphene oxide, the antibacterial agent and the polypropylene is 0.5-3.
Further, in step S1, the premixing time is 6-12min, and the extrusion temperature is 180-210 ℃.
The graphene-polypropylene composite master batch prepared by the preparation method is provided.
The graphene-polypropylene composite master batch is applied to preparing films and non-woven fabrics.
According to the invention, the Graphene Oxide (GO) is subjected to surface modification by using the amphoteric surface modifier, and the specific functional group of the surface modifier reacts with oxygen-containing functional groups such as carboxyl on GO, so that the hydrophilicity of GO is lost, and meanwhile, the compatibility of the Modified Graphene Oxide (MGO) and organic polymer base materials such as PP is enhanced, so that the organic polymer material has better mechanical properties. Meanwhile, GO is an ideal carrier of antibacterial active substances due to the special two-dimensional porous structure of GO. The antimicrobial agent containing guanidine has the advantages of excellent antimicrobial performance, good biocompatibility and the like, oxygen-containing functional groups in the modified graphene oxide, particularly hydroxyl groups and imino groups in guanidine salt are combined through weak interaction, the combining capacity of the oxygen-containing functional groups and the imino groups is guaranteed, the guanidine salt can be well loaded on a two-dimensional structure of the modified graphene oxide and has nonspecific action with bacteria, the bacteria cannot generate drug resistance, and the defect of insufficient GO bacteriostatic ability is overcome.
The product prepared from the graphene-polypropylene composite antibacterial master batch prepared by the melt compounding method has good mechanical properties and excellent antibacterial properties. Meanwhile, the modifier and rich oxygen-containing groups on the surface of the graphene oxide are assembled through static electricity to form graphene oxide flocculation liquid with the surface subjected to hydrophobic modification, and the graphene oxide structure with the surface grafted with hydrophobic molecule chain segments is obtained through repeated washing and freeze drying; the graphene oxide with the surface grafted with the hydrophobic molecular chain segment is premixed with the antibacterial agent and the polypropylene, so that the interfacial energy of a composite system is reduced due to the interaction between the surface modified graphene oxide filler and the polypropylene base material, and the graphene-polypropylene composite antibacterial master batch with two phases which are completely compatible can be obtained through simple extrusion, granulation, melting and compounding.
The film and the non-woven fabric produced by the composite master batch prepared by the invention have the excellent characteristics of high mechanical strength, antibiosis and the like without subsequent treatment.
Detailed Description
The following are specific examples of the present invention and further describe the technical solutions of the present invention, but the present invention is not limited to these examples.
< example 1>
The embodiment relates to a preparation method of a graphene-polypropylene composite antibacterial master batch, which specifically comprises the following steps:
preparing a graphene oxide aqueous solution by using an improved Hummers method, wherein the content of graphene oxide is 4mg/ml; and dropwise adding a surfactant lauramide propyl amine oxide at 50 ℃, washing, and freeze-drying to obtain the modified graphene oxide particles. And (3) taking the modified graphene oxide particles, premixing the modified graphene oxide particles with polyhexamethylene guanidine hydrochloride and polypropylene polymer, and extruding and granulating to obtain the graphene-polypropylene composite master batch. The mass ratio of the graphene oxide to the polyhexamethylene guanidine hydrochloride to the polypropylene is 0.5.
< example 2>
The embodiment relates to a preparation method of a graphene-polypropylene composite antibacterial master batch, which specifically comprises the following steps:
preparing a graphene oxide aqueous solution by using an improved Hummers method, wherein the content of graphene oxide is 8mg/ml; and dropwise adding a surfactant lauramide propyl amine oxide at the temperature of 30 ℃, washing, and freeze-drying to obtain the modified graphene oxide particles. And (3) taking the modified graphene oxide particles, premixing the modified graphene oxide particles with polyhexamethylene guanidine hydrochloride and polypropylene macromolecules, and extruding and granulating to obtain the graphene-polypropylene composite master batch. The mass ratio of the graphene oxide to the polyhexamethylene guanidine hydrochloride to the polypropylene is 1.5.
< example 3>
The embodiment relates to a preparation method of a graphene-polypropylene composite antibacterial master batch, which specifically comprises the following steps:
preparing a graphene oxide aqueous solution by using an improved Hummers method, wherein the content of graphene oxide is 4mg/ml; and dropwise adding surfactant tetradecyl dihydroxyethyl amine oxide at 50 ℃, washing, and freeze-drying to obtain the modified graphene oxide particles. And (3) taking the modified graphene oxide particles, premixing the modified graphene oxide particles with polyhexamethylene guanidine hydrochloride and polypropylene polymer, and extruding and granulating to obtain the graphene-polypropylene composite master batch. The mass ratio of the graphene oxide to the polyhexamethylene guanidine hydrochloride to the polypropylene is 2.
< example 4>
The embodiment relates to a preparation method of a graphene-polypropylene composite antibacterial master batch, which specifically comprises the following steps:
preparing a graphene oxide aqueous solution by using an improved Hummers method, wherein the content of graphene oxide is 10mg/ml; and dropwise adding surfactant tetradecyl dihydroxyethyl amine oxide and lauramidopropyl amine oxide at 60 ℃, washing, and freeze-drying to obtain the modified graphene oxide particles. And (3) taking the modified graphene oxide particles, premixing the modified graphene oxide particles with guanidine phosphate and polypropylene macromolecules, and extruding and granulating to obtain the graphene-polypropylene composite master batch. The mass ratio of the graphene oxide to the guanidine phosphate to the polypropylene is 0.5.
< comparative example 1>
The embodiment relates to a preparation method of a graphene-polypropylene composite material, which specifically comprises the following steps:
the embodiment relates to a preparation method of a graphene-polypropylene composite material, which is the same as the embodiment 1 except that directly freeze-dried graphene oxide is adopted and an antibacterial agent is not added.
< comparative example 2>
The embodiment relates to a preparation method of a graphene-polypropylene composite material, which specifically comprises the following steps:
the embodiment relates to a preparation method of a graphene-polypropylene composite material, which is the same as the embodiment 1 except that an antibacterial agent is not adopted for compounding.
< comparative example 3>
The embodiment relates to a preparation method of a graphene-polypropylene composite material, which specifically comprises the following steps:
the present example relates to a method for preparing a graphene-polypropylene composite material, which is the same as example 1, except that unmodified graphene oxide directly lyophilized is used, but an antibacterial agent is added.
< comparative example 4>
The embodiment relates to a preparation method of a graphene-polypropylene composite material, which specifically comprises the following steps:
the embodiment relates to a preparation method of a graphene-polypropylene composite material, which is the same as the embodiment 1 except that the antibacterial agent is bacterial cellulose without a guanidino functional group.
The standard sample strips prepared from the graphene-polypropylene composite materials of the embodiments 1 to 4 and the graphene-polypropylene composite materials prepared from the comparative examples 1 to 4 are tested for antibacterial performance, elongation at break and tensile strength, the method of WS/T650-2019 is adopted for the antibacterial performance test, the method of GB-T1040.1-2018 is adopted for the elongation at break test and the tensile strength test standards, and the test results are shown in the following table.
As can be seen from the above table, the antibacterial performance, the elongation at break and the tensile strength of the standard sample strips prepared from the graphene-polypropylene composite materials of examples 1 to 4 are improved significantly compared to the standard sample strips of comparative examples 1 to 4. The surfactant is attached to the surface of the graphene, so that the compatibility of the graphene in a matrix is improved, an interface layer is formed between the graphene reinforced material and the matrix, the interface layer can transfer stress, the composite strength is improved by utilizing the synergistic effect of the interface layer and the matrix, and the performance of the composite material is improved. The addition of the graphene and the antibacterial agent endows the polypropylene with functionality, and the antibacterial performance, the elongation at break, the tensile strength and other performances of the composite material are remarkably improved.
The above is not relevant and is applicable to the prior art.
While certain specific embodiments of the present invention have been described in detail by way of illustration, it will be understood by those skilled in the art that the foregoing is illustrative only and is not limiting of the scope of the invention, as various modifications or additions may be made to the specific embodiments described and substituted in a similar manner by those skilled in the art without departing from the scope of the invention as defined in the appending claims. It should be understood by those skilled in the art that any modifications, equivalents, improvements and the like made to the above embodiments in accordance with the technical spirit of the present invention are included in the scope of the present invention.
Claims (10)
1. A preparation method of a graphene-polypropylene composite antibacterial master batch is characterized by comprising the following steps:
s1: grafting hydrophobic molecule chain segments on the graphene oxide;
s2: and (3) premixing, extruding, granulating and compounding the graphene oxide grafted on the hydrophobic molecular chain section, the antibacterial agent and the polypropylene to obtain the graphene-polypropylene composite antibacterial master batch with two phases being completely compatible.
2. The preparation method of the graphene-polypropylene composite antibacterial master batch as claimed in claim 1, wherein the specific process of the step S1 is as follows: dropwise adding a surface modifier into a freshly prepared graphene oxide dispersion liquid under constant-temperature stirring, carrying out electrostatic assembly on the modifier and rich oxygen-containing groups on the surface of graphene oxide to form a graphene oxide flocculating solution with the surface subjected to hydrophobic modification, repeatedly washing, and carrying out freeze drying to obtain the graphene oxide structure with the surface grafted with hydrophobic molecular chain segments.
3. The method for preparing the graphene-polypropylene composite antibacterial master batch as claimed in claim 2, wherein in the step S1, the graphene oxide dispersion liquid is a graphene oxide aqueous dispersion liquid prepared by a modified hummers method, and the content of graphene oxide is 0.1-10mg/ml.
4. The preparation method of the graphene-polypropylene composite antibacterial master batch as claimed in claim 2, wherein in the step S1, the surfactant is an amphoteric surfactant, and is specifically one or more of lauramidopropyl amine oxide, octadecyl dihydroxyethyl amine oxide or tetradecyl dihydroxyethyl amine oxide.
5. The preparation method of the graphene-polypropylene composite antibacterial master batch as claimed in claim 2, wherein in the step S1, the modification of the graphene oxide is carried out at a stirring speed of 250-550rpm, a constant temperature of 30-60 ℃ and a mass ratio of the graphene oxide to the surfactant of 0.5-2.
6. The method for preparing the graphene-polypropylene composite antibacterial master batch as claimed in claim 2, wherein in the step S2, the antibacterial agent is one or more of polyhexamethylene biguanide hydrochloride, polyhexamethylene biguanide hydrochloride or guanidine phosphate.
7. The preparation method of the graphene-polypropylene composite antibacterial master batch as claimed in claim 1, wherein in the step S1, the mass ratio of the graphene oxide to the antibacterial agent to the polypropylene is 0.5-3.
8. The preparation method of the graphene-polypropylene composite antibacterial master batch as claimed in claim 1, wherein in the step S1, the premixing time is 6-12min, and the extrusion temperature is 180-210 ℃.
9. A graphene-polypropylene composite masterbatch prepared by the preparation method of any one of claims 1 to 8.
10. Use of the graphene-polypropylene composite masterbatch according to claim 9 for the preparation of films and non-woven fabrics.
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