CN107793640A - Activeness and quietness antibacterial polypropylene material and its preparation method and application - Google Patents

Activeness and quietness antibacterial polypropylene material and its preparation method and application Download PDF

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Publication number
CN107793640A
CN107793640A CN201711056533.1A CN201711056533A CN107793640A CN 107793640 A CN107793640 A CN 107793640A CN 201711056533 A CN201711056533 A CN 201711056533A CN 107793640 A CN107793640 A CN 107793640A
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temperature
area
polypropylene
molecular weight
quietness
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何丹农
林琳
陈超
金彩虹
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Shanghai National Engineering Research Center for Nanotechnology Co Ltd
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Shanghai National Engineering Research Center for Nanotechnology Co Ltd
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    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
    • C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
    • C08L23/10—Homopolymers or copolymers of propene
    • C08L23/12—Polypropene
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
    • B29B9/00—Making granules
    • B29B9/02—Making granules by dividing preformed material
    • B29B9/06—Making granules by dividing preformed material in the form of filamentary material, e.g. combined with extrusion
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
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    • C08J3/20—Compounding polymers with additives, e.g. colouring
    • C08J3/22—Compounding polymers with additives, e.g. colouring using masterbatch techniques
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    • C08L23/10—Homopolymers or copolymers of propene
    • C08L23/14—Copolymers of propene
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C2948/00—Indexing scheme relating to extrusion moulding
    • B29C2948/92—Measuring, controlling or regulating
    • B29C2948/92504—Controlled parameter
    • B29C2948/92514—Pressure
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C2948/00—Indexing scheme relating to extrusion moulding
    • B29C2948/92—Measuring, controlling or regulating
    • B29C2948/92504—Controlled parameter
    • B29C2948/9258—Velocity
    • B29C2948/9259—Angular velocity
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C2948/00—Indexing scheme relating to extrusion moulding
    • B29C2948/92—Measuring, controlling or regulating
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    • B29C2948/92704—Temperature
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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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    • 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
    • C08J2323/14—Copolymers of propene
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    • 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
    • C08J2423/04—Homopolymers or copolymers of ethene
    • C08J2423/06—Polyethene
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    • 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
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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
    • C08K3/22—Oxides; Hydroxides of metals
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Abstract

The present invention relates to a kind of activeness and quietness antibacterial polypropylene material and its preparation method and application, it is made up of following raw materials by weight：Polypropylene 54~87.7%；Inorganic antiseptic 0.5~5%；Ultra-high molecular weight polyethylene master batch 10~30%；Graft polypropylene 1~8%；Stabilizer 0.2~1%；Dispersant 0.2~1%；Antioxidant 0.4~1%.The present invention is standby into master batch by ultrahigh molecular weight polyethylene, and high-intensity high-tenacity and high anti-microbial property PP composite material is made in the inorganic antiseptic for being then modified surface, polypropylene, ultra-high molecular weight polyethylene master batch, graft polypropylene and other auxiliary agent mixed at high speed extrusion.The present invention is while ensureing that addition inorganic antiseptic assigns polypropylene excellent antibacterial activity, by adding organic overlength chain macromolecule activeness and quietness polypropylene.Therefore, the PP composite material that prepared by the present invention not only shows excellent anti-microbial property, and with prominent mechanical characteristic.

Description

Activeness and quietness antibacterial polypropylene material and its preparation method and application
Technical field
The present invention relates to a kind of activeness and quietness antibacterial polypropylene material and its preparation method and application, belong to high polymer material Technical field.
Background technology
Data shows the various surface of plastic products contamination touched in daily life and grows a variety of germs.Such as hotel Bacterium on restaurant's toilet seat has Escherichia coli, staphylococcus aureus, White staphylococcus, hay bacillus, tetrads etc., bacterium Fall number up to 40；The clump count of public telephone microphone is up to 50；Hospital, hotel door handle clump count even up to more than 200. With the raising of people's living standard, everybody is to health and healthy requirement also more and more higher.Since the nineties, with day This has carried out antibacterial for the developed country of representative in household electrical appliance, packaging for foodstuff, toy for children, kitchen and sanitary bath equipment etc. Research, exploitation and the production work of material, to reduce because of the bacterium infection occurred using plastic products.
Polypropylene, because density is small, price is low and good processing characteristics, is widely used in house as a kind of non-toxic plastic Each field such as electrical appliance.But polypropylene is easily polluted as other plastics by various harmful bacterias, in the case of being adapted to, it is more easy to Bacterial growth.Polyacrylic anti-microbial property is generally improved using addition antiseptic now.Currently used plastic antimicrobial agent can It is divided into organic antibacterial agent and inorganic antiseptic, organic antibacterial agent mainly has ethers, phenol, biphenyl ethers, quaternary ammonium salt etc., its Feature is that sterilization speed is fast, but the antibacterial term of validity is short, heat resistance is poor.Inorganic antiseptic be mainly silver, zinc, titanium plasma and its Compound, it is characterized in heat-resist, safe, antibacterial term of validity length etc..Such as Chinese patent CN101089038A is disclosed Nano Silver addition polypropylene obtains a kind of antibiotic rate and is more than 99% PP composite material；Chinese patent CN1699459A is disclosed A kind of silver-carrying nano oxide antibacterial polypropylene water-feeding pipes and preparation method thereof.Above-mentioned patent is related to Nano Silver, load silver is received Application of the rice oxide antiseptic in polypropylene, and obtain certain achievement.But silver-series antibacterial agent is there is also many shortcomings, such as easy Discoloration, poor heat resistance, manufacture are difficult, and in the plastic using complex process etc., noble metal toxic is also disputable in addition.In machinery Aspect of performance, polypropylene cause material under low temperature or high strain rate, because the impact energy of absorption has little time to transmit in time Impact resistance ability, notch sensitivity are strong, impact strength is low, so as to greatly limit polypropylene as engineering material and structural wood The application of material.To optimize Properties of Polypropylene, further expand its application, all carry out substantial amounts of polypropylene enhancing both at home and abroad The research and development of toughening modifying, certain achievement is achieved in terms of multiphase copolymer and blending and modifying.Such as Chinese patent CN201110308569.0 discloses one kind and utilizes rubber sulfonation flexibilized polypropylene material；Chinese patent CN201010214965.2 One kind is disclosed using butadiene-styrene rubber toughening modifying polypropylene material and preparation method thereof；Japanese Patent Laid-Open 6-190991 is public A kind of high density polyethylene (HDPE)/polypropylene bonding composite is opened；United States Patent (USP) US20020010241A1 discloses one kind by gathering The polyolefin composition of propylene and ultra-high molecular weight polyethylene composition.Although above-mentioned patent report is polypropylene toughness-increasing modified, It is not relate to study of both Mechanical Properties of PP and antibacterial in disclosed research.
The content of the invention
For overcome the deficiencies in the prior art, present invention aims at：A kind of activeness and quietness antibacterial polypropylene material is provided.Should While material use addition inorganic antiseptic assigns polypropylene excellent anti-microbial property, improved by adding super long chain macromolecule Polyacrylic tensile strength and notch impact strength.
It is still another object of the present invention to provide the preparation method of the said goods.
A further object of the present invention is the application for providing the said goods.
The object of the invention is realized by following proposal：A kind of activeness and quietness antibacterial polypropylene material, polypropylene, inorganic antibacterial Agent, ultra-high molecular weight polyethylene master batch, graft polypropylene, dispersant, the proportioning of stabilizer and antioxidant percentage It is as follows：
Polypropylene 54~87.7%；
Inorganic antiseptic 0.5~5%；
Ultra-high molecular weight polyethylene master batch 10~30%；
Graft polypropylene 1~8%；
Dispersant 0.2~1%；
Stabilizer 0.2~1%；
Antioxidant 0.4~1%.
On the basis of such scheme, described polypropylene is a kind of or their combination in homopolymerization and COPP Thing, its melt index are 1~25g/10min；Described antiseptic is nano inorganic antibacterial, composite hybridization nano inorganic antimicrobial agent In one or more；Graft polypropylene is maleic anhydride inoculated polypropylene or glycidyl methacrylate graft polypropylene In one kind or their compositions.
On the basis of such scheme, described dispersant is ethylene group bis-stearamides, glyceryl monostearate, three tristearin One or more in acid glyceride；Described stabilizer be organic tin in dibutyl tin laurate, dibutyitin maleate, One or more in dibutyltin mercaptide.
On the basis of such scheme, described antioxidant includes primary antioxidant and auxiliary anti-oxidant, and primary antioxidant is hindered phenol With the one or more in sulphur ester antioxidant, auxiliary anti-oxidant is the one or more in phosphorite kind antioxidant；For Increase the affinity of inorganic antiseptic and fluoropolymer resin, the inorganic antiseptic being modified using coupling agent surface, wherein coupling agent For silane coupler, titanate coupling agent, aluminate coupling agent one or more.
On the basis of such scheme, described ultra-high molecular weight polyethylene master batch is by following substances in percentage by weight group Into：
Ultra-high molecular weight polyethylene 30~50%；
LLDPE 30~40%；
Inorganic particle 10~15%；
Compatilizer 10~15%.
On the basis of such scheme, the molecular weight of described ultra-high molecular weight polyethylene is 150~5,000,000；Described line Property low density polyethylene (LDPE) density is 0.92g/cm3, melt index 24g/10min.
Described inorganic particle is in calcium carbonate, talcum powder, carbon fiber, glass fibre, silica, potassium titanate crystal whisker It is one or more of；Described compatilizer is atoleine, and molecular weight is 100~200 g/mol.
The present invention provides the preparation method of any activeness and quietness antibacterial polypropylene material as described above, is squeezed by twin-screw Go out machine by polypropylene, inorganic antiseptic, ultra-high molecular weight polyethylene master batch, graft polypropylene, dispersant, stabilizer and antioxidant Cooling granulation after melting extrusion, is made activeness and quietness antibacterial polypropylene material, and step is as follows：
（1）First at a certain temperature, using coupling agent to inorganic antiseptic carry out surface modification, surface modification temperature be 60~ 70oC, coupling agent dosage are 0.5~2%；
（2）Polypropylene, inorganic antiseptic, ultra-high molecular weight polyethylene master batch, graft polypropylene, scattered is weighed by weight ratio Agent, stabilizer and antioxidant mix 15~20 minutes in super mixer；
（3）Mixed raw material is added in double screw extruder, the cooling granulation after melting extrusion, expressing technique is：One area Temperature 180~190oC, two area's temperature 180~190oC, three area's temperature 190~200oC, four area's temperature 190~200oC, five area's temperature Degree 190~200oC, six area's temperature 200~210oC, seven area's temperature 200~210oC, eight area's temperature 210~220oC, nine area's temperature 210~220oC, head temperature 200~210oC, 200~250 revs/min of screw speed, 18~25MPa of pressure.
On the basis of such scheme, described ultra-high molecular weight polyethylene master batch preparation process is as follows：By what is necessarily matched Ultra-high molecular weight polyethylene, LLDPE, inorganic particle and compatilizer are well mixed in super mixer, then It is through double screw extruder extruding pelletization, expressing technique by mixture：One area's temperature 190~200oC, two area's temperature 190~ 200oC, three area's temperature 200~210oC, four area's temperature 200~210oC, five area's temperature 200~210oC, six area's temperature 210~ 220oC, seven area's temperature 210~220oC, eight area's temperature 215~225oC, nine area's temperature 215~225oC, head temperature 200~ 220oC, screw speed 200~250 turns/min, 20~25MPa of melt pressure.
The present invention provides a kind of application of activeness and quietness antibacterial polypropylene material as material for car interior trim parts.
In polypropylene toughness-increasing modified research, the most frequently used toughening methods are exactly that flexible polymer is introduced in plastic substrate Thing, when system is by external impacts, a large amount of punchings are absorbed by the crazing and shear yielding that trigger flexible polymer surrounding matrix Energy is hit, so as to improve the toughness of matrix.But this method has fatal weakness, although that is, the toughness of polypropylene matrix improves , but often result in the reduction of tensile strength and hardness；On the other hand, for the Pp System of addition inorganic antiseptic, draw Enter flexible polymer to be easy to form clad in inorganic antiseptic particle surface, reduce the antimicrobial efficiency of inorganic antiseptic.Cause This, simply adds flexible polymer in inorganic antiseptic/Pp System, although improving to a certain extent polyacrylic Toughness, but largely using the antimicrobial efficiency of sacrificial inorganic antiseptic as cost.Therefore, ensureing that inorganic antiseptic is excellent While different anti-microbial property, how to improve Mechanical Properties of PP is one of difficult point of antibacterial polypropylene material research.
Many researchers use introduces super long chain macromolecule in polypropylene matrix, utilizes overlength strand shape in the base Into the skeleton structure of physical entanglement, when material is acted on by external force, the skeleton of this entanglement absorbs and transmits impact in matrix Can, to play a part of activeness and quietness.For example, using the high PE modified polypropylene of molecular weight, make itself and polypropylene melt Melt blending and form linear interpenetrating networks or physical cross-linked network, when material under external force, large deformation occurs for network, absorbs outer Boundary's energy, play the effect of activeness and quietness.But ultra-high molecular weight polyethylene molecular weight is very long, mutually tangle each other, even if More than melting temperature, the state of elastomer is also kept without mobility.
The present invention uses LLDPE as carrier, and the alkane for adding certain low molecule amount gathers with super high molecular weight Ethene melt blending generates the ultra-high molecular weight polyethylene master batch of low viscosity；Using nano zine oxide or titanium dioxide as inorganic Antiseptic, then polypropylene, ultra-high molecular weight polyethylene master batch, inorganic antiseptic, graft polypropylene and other auxiliary agents are passed through Double screw extruder melt blending is extruded to obtain activeness and quietness antibacterial polypropylene material.For preparing activeness and quietness antibacterial polypropylene The requirement of material, the present invention have the property that：（1）Nano zine oxide or titanium dioxide are selected as inorganic antiseptic；（2）Choosing The ultra-high molecular weight polyethylene with overlength strand is selected as organic filler, and carrier is used as by the use of LLDPE The ultra-high molecular weight polyethylene master batch of generation low viscosity is extruded with ultra-high molecular weight polyethylene melt blending；（3）Effectively improving On the premise of polypropylene antibacterial activity and mechanical strength, as far as possible using a small amount of inorganic antiseptic and ultra-high molecular weight polyethylene Master batch.
Compared with existing antibacterial polypropylene material, the present invention has the following effects that：The polypropylene material that the present invention is prepared Expect antibacterial more rapidly, it is more longlasting, safer；Simultaneously material is improved present invention uses super long chain macromolecule as filler Mechanical property, widened the application of antibacterial polypropylene material.
Brief description of the drawings
Fig. 1 is the TEM pictures of KH550 modified nano zinc oxide powders in embodiment 1；
Fig. 2 is the polypropylene impact fracture surface SEM photograph of embodiment 3.
Embodiment
Following embodiment is the further explanation to the present invention, and the present invention is not limited to following examples and reality Applying method.
Embodiment 1
1) surface modification of inorganic antiseptics
60 are heated to by decentralized medium of ethanoloC, add Silane coupling agent KH550 and disperse 5min, then add inorganic antiseptic Zinc oxide disperses 30min, and drying, grinding, sieving obtain modified zinc oxide, and wherein KH550 dosages are 0.5%.Fig. 1 is embodiment 1 The TEM pictures of middle KH550 modified nano zinc oxides powder.
2) preparation of ultra-high molecular weight polyethylenes master batch
By 30% ultra-high molecular weight polyethylene, 40% LLDPE, 15% calcium carbonate, 15% atoleine in mixed at high speed It is well mixed in device.Mixture is standby through double screw extruder extruding pelletization, and wherein ultra-high molecular weight polyethylene molecular weight is 150 Ten thousand, expressing technique is：One area's temperature 190oC, two area's temperature 190oC, three area's temperature 200oC, four area's temperature 200oC, five area's temperature 200oC, six area's temperature 210oC, seven area's temperature 210oC, eight area's temperature 215oC, nine area's temperature 215oC, head temperature 200oC, spiral shell Bar rotating speed 200 turns/min, melt pressure 20MPa.
3) preparation of activeness and quietness antibacterial polypropylene material
87.7% HOPP, 0.5% modified zinc oxide, 10% ultra-high molecular weight polyethylene master batch, the grafting of 1% maleic anhydride is poly- Propylene, 0.2% glyceryl monostearate, 0.2% dibutyl tin laurate, each 0.2% primary antioxidant 3114 and auxiliary anti-oxidant 168 exist It is well mixed in super mixer, then extrudes mixture through double screw extruder to obtain activeness and quietness antibacterial polypropylene material Material.Wherein polypropylene melt index is 1g/10min, and expressing technique is：One area's temperature 180oC, two area's temperature 180oC, three area's temperature Degree 190oC, four area's temperature 190oC, five area's temperature 190oC, six area's temperature 200oC, seven area's temperature 200oC, eight area's temperature 210oC, Nine area's temperature 210oC, head temperature 200oC, screw speed 200 turns/min, melt pressure 18MPa.
Embodiment 2
1) surface modification of inorganic antiseptics
60 are heated to by decentralized medium of ethanoloC, add Silane coupling agent KH550 and disperse 5min, then add inorganic antiseptic Zinc oxide disperses 30min, and drying, grinding, sieving obtain modified zinc oxide, and wherein KH550 dosages are 0.5%.
2) preparation of ultra-high molecular weight polyethylenes master batch
By 50% ultra-high molecular weight polyethylene, 30% LLDPE, 10% calcium carbonate, 10% atoleine in mixed at high speed It is well mixed in device.Mixture is standby through double screw extruder extruding pelletization, and wherein ultra-high molecular weight polyethylene molecular weight is 150 Ten thousand, expressing technique is：One area's temperature 200oC, two area's temperature 200oC, three area's temperature 210oC, four area's temperature 210oC, five area's temperature 210oC, six area's temperature 220oC, seven area's temperature 220oC, eight area's temperature 225oC, nine area's temperature 225oC, head temperature 220oC, spiral shell Bar rotating speed 250 turns/min, melt pressure 25MPa.
3) preparation of activeness and quietness antibacterial polypropylene material
67.7% HOPP, 0.5% modified zinc oxide, 30% ultra-high molecular weight polyethylene master batch, the grafting of 1% maleic anhydride is poly- Propylene, 0.2% glyceryl monostearate, 0.2% dibutyl tin laurate, each 0.2% primary antioxidant 3114 and auxiliary anti-oxidant 168 exist It is well mixed in super mixer, then extrudes mixture through double screw extruder to obtain activeness and quietness antibacterial polypropylene material Material.Wherein polypropylene melt index is 1g/10min, and expressing technique is：One area's temperature 190oC, two area's temperature 190oC, three area's temperature Degree 200oC, four area's temperature 200oC, five area's temperature 200oC, six area's temperature 210oC, seven area's temperature 210oC, eight area's temperature 220oC, Nine area's temperature 220oC, head temperature 210oC, screw speed 230 turns/min, melt pressure 20MPa.
Embodiment 3
1) surface modification of inorganic antiseptics
70 are heated to by decentralized medium of isopropanoloC, add silane coupler DL602 and disperse 5min, then add inorganic antibacterial Agent zinc oxide disperses 30min, and drying, grinding, sieving obtain modified zinc oxide, and wherein DL602 dosages are 2%.
2) preparation of ultra-high molecular weight polyethylenes master batch
By 30% ultra-high molecular weight polyethylene, 40% LLDPE, 15% talcum powder, 15% atoleine in mixed at high speed It is well mixed in device.Mixture is standby through double screw extruder extruding pelletization, and wherein ultra-high molecular weight polyethylene molecular weight is 150 Ten thousand, expressing technique is：One area's temperature 190oC, two area's temperature 190oC, three area's temperature 200oC, four area's temperature 200oC, five area's temperature 200oC, six area's temperature 210oC, seven area's temperature 210oC, eight area's temperature 215oC, nine area's temperature 215oC, head temperature 200oC, spiral shell Bar rotating speed 200 turns/min, melt pressure 20MPa.
3) preparation of activeness and quietness antibacterial polypropylene material
By 74% HOPP, 5% modified zinc oxide, 10% ultra-high molecular weight polyethylene master batch, 8% maleic anhydride grafting poly- third Alkene, 1% glyceryl monostearate, 1% dibutyl tin laurate, each 0.5% primary antioxidant 3114 and auxiliary anti-oxidant 168 are mixed in high speed It is well mixed in clutch, then extrudes mixture through double screw extruder to obtain activeness and quietness antibacterial polypropylene material.Wherein Polypropylene melt index is 1g/10min, and expressing technique is：One area's temperature 180oC, two area's temperature 180oC, three area's temperature 190oC, Four area's temperature 190oC, five area's temperature 190oC, six area's temperature 200oC, seven area's temperature 200oC, eight area's temperature 210oC, nine area's temperature 210oC, head temperature 200oC, screw speed 200 turns/min, melt pressure 20MPa.
Fig. 2 is the polypropylene impact fracture surface SEM photograph of embodiment 3.
Embodiment 4
1) surface modification of inorganic antiseptics
70 are heated to by decentralized medium of ethanoloC, add titanate coupling agent UP-131 and disperse 5min, then add inorganic anti- Microbial inoculum zinc oxide disperses 30min, and drying, grinding, sieving obtain modified zinc oxide, and wherein UP-131 dosages are 1%.
2) preparation of ultra-high molecular weight polyethylenes master batch
By 50% ultra-high molecular weight polyethylene, 30% LLDPE, 10% potassium titanate crystal whisker, 10% atoleine at a high speed It is well mixed in blender.Mixture is standby through double screw extruder extruding pelletization, wherein ultra-high molecular weight polyethylene molecular weight For 1,500,000, expressing technique is：One area's temperature 200oC, two area's temperature 200oC, three area's temperature 210oC, four area's temperature 210oC, five Area's temperature 210oC, six area's temperature 220oC, seven area's temperature 220oC, eight area's temperature 225oC, nine area's temperature 225oC, head temperature 220oC, screw speed 250 turns/min, melt pressure 25MPa.
3) preparation of activeness and quietness antibacterial polypropylene material
By 54% HOPP, 5% modified zinc oxide, 30% ultra-high molecular weight polyethylene master batch, 8% maleic anhydride grafting poly- third Alkene, 1% glyceryl monostearate, 1% dibutyl tin laurate, each 0.5% primary antioxidant 1010 and auxiliary anti-oxidant 168 are mixed in high speed It is well mixed in clutch, then extrudes mixture through double screw extruder to obtain activeness and quietness antibacterial polypropylene material.Wherein Polypropylene melt index is 1g/10min, and expressing technique is：One area's temperature 190oC, two area's temperature 190oC, three area's temperature 200oC, Four area's temperature 200oC, five area's temperature 200oC, six area's temperature 210oC, seven area's temperature 210oC, eight area's temperature 220oC, nine area's temperature 220oC, head temperature 210oC, screw speed 250 turns/min, melt pressure 25MPa.
Embodiment 5
1) surface modification of inorganic antiseptics
60 are heated to by decentralized medium of ethanoloC, add Silane coupling agent KH550 and disperse 5min, then add inorganic antiseptic Titanium dioxide disperses 30min, and drying, grinding, sieving obtain modifying titanium dioxide, and wherein KH550 dosages are 0.5%.
2) preparation of ultra-high molecular weight polyethylenes master batch
By 30% ultra-high molecular weight polyethylene, 40% LLDPE, 15% calcium carbonate, 15% atoleine in mixed at high speed It is well mixed in device.Mixture is standby through double screw extruder extruding pelletization, and wherein ultra-high molecular weight polyethylene molecular weight is 150 Ten thousand, expressing technique is：One area's temperature 190oC, two area's temperature 190oC, three area's temperature 200oC, four area's temperature 200oC, five area's temperature 200oC, six area's temperature 210oC, seven area's temperature 210oC, eight area's temperature 215oC, nine area's temperature 215oC, head temperature 200oC, spiral shell Bar rotating speed 200 turns/min, melt pressure 20MPa.
3) preparation of activeness and quietness antibacterial polypropylene material
By 87.7% HOPP, 0.5% modifying titanium dioxide, 10% ultra-high molecular weight polyethylene master batch, the grafting of 1% maleic anhydride Polypropylene, 0.2% glyceryl monostearate, 0.2% dibutyl tin laurate, each 0.2% primary antioxidant 3114 and auxiliary anti-oxidant 168 It is well mixed in super mixer, then extrudes mixture through double screw extruder to obtain activeness and quietness antibacterial polypropylene material Material.Wherein polypropylene melt index is 1g/10min, and expressing technique is：One area's temperature 180oC, two area's temperature 180oC, three area's temperature Degree 190oC, four area's temperature 190oC, five area's temperature 190oC, six area's temperature 200oC, seven area's temperature 200oC, eight area's temperature 210oC, Nine area's temperature 210oC, head temperature 200oC, screw speed 200 turns/min, melt pressure 18MPa.
Embodiment 6
1) surface modification of inorganic antiseptics
65 are heated to by decentralized medium of isopropanoloC, add titanate coupling agent UP-131 and disperse 5min, then add inorganic Antiseptic titanium dioxide disperses 30min, and drying, grinding, sieving obtain modifying titanium dioxide, and wherein UP-131 dosages are 2%.
2) preparation of ultra-high molecular weight polyethylenes master batch
By 50% ultra-high molecular weight polyethylene, 30% LLDPE, 10% talcum powder, 10% atoleine in mixed at high speed It is well mixed in device.Mixture is standby through double screw extruder extruding pelletization, and wherein ultra-high molecular weight polyethylene molecular weight is 500 Ten thousand, expressing technique is：One area's temperature 200oC, two area's temperature 200oC, three area's temperature 210oC, four area's temperature 210oC, five area's temperature 210oC, six area's temperature 220oC, seven area's temperature 220oC, eight area's temperature 225oC, nine area's temperature 225oC, head temperature 220oC, spiral shell Bar rotating speed 250 turns/min, melt pressure 25MPa.
3) preparation of activeness and quietness antibacterial polypropylene material
54% COPP, 5% modifying titanium dioxide, 30% ultra-high molecular weight polyethylene master batch, 8% Glycidyl methacrylate is sweet Grease graft polypropylene, 1% glyceryl tristearate, 1% dibutyitin maleate, each 0.5% primary antioxidant 1010 and auxiliary anti-oxidant 618 are well mixed in super mixer, then extrude mixture through double screw extruder to obtain activeness and quietness antibacterial poly- third Alkene material.Wherein polypropylene melt index is 25g/10min, and expressing technique is：One area's temperature 190oC, two area's temperature 190oC, three Area's temperature 200oC, four area's temperature 200oC, five area's temperature 200oC, six area's temperature 210oC, seven area's temperature 210oC, eight area's temperature 220oC, nine area's temperature 220oC, head temperature 210oC, screw speed 250 turns/min, melt pressure 25MPa.
Embodiment 7
1) surface modification of inorganic antiseptics
60 are heated to by decentralized medium of ethanoloC, add Silane coupling agent KH550 and disperse 5min, then add inorganic antiseptic Zinc oxide disperses 30min, and drying, grinding, sieving obtain modified zinc oxide, and wherein KH550 dosages are 0.5%.Same method, obtain To titanate coupling agent UP-131 modifying titanium dioxides.
2) preparation of ultra-high molecular weight polyethylenes master batch
By 30% ultra-high molecular weight polyethylene, 40% LLDPE, 15% calcium carbonate, 15% atoleine in mixed at high speed It is well mixed in device.Mixture is standby through double screw extruder extruding pelletization, and wherein ultra-high molecular weight polyethylene molecular weight is 250 Ten thousand, expressing technique is：One area's temperature 190oC, two area's temperature 190oC, three area's temperature 200oC, four area's temperature 200oC, five area's temperature 200oC, six area's temperature 210oC, seven area's temperature 210oC, eight area's temperature 215oC, nine area's temperature 215oC, head temperature 200oC, spiral shell Bar rotating speed 200 turns/min, melt pressure 20MPa.
3) preparation of activeness and quietness antibacterial polypropylene material
By 85% COPP, each 0.5% modified zinc oxide and titanium dioxide, 10% ultra-high molecular weight polyethylene master batch, 2% Malaysia Anhydride-grafted polypropylene, 0.5% glyceryl monostearate, 0.5% dibutyl tin laurate, each 0.5% primary antioxidant 3114 and auxiliary anti- Oxygen agent 168 is well mixed in super mixer, then extrudes mixture through double screw extruder to obtain activeness and quietness antibacterial Polypropylene material.Wherein polypropylene melt index is 25g/10min, and expressing technique is：One area's temperature 180oC, two area's temperature 180oC, three area's temperature 190oC, four area's temperature 190oC, five area's temperature 190oC, six area's temperature 200oC, seven area's temperature 200oC, eight Area's temperature 210oC, nine area's temperature 210oC, head temperature 200oC, screw speed 200 turns/min, melt pressure 18MPa.
Embodiment 8
1) surface modification of inorganic antiseptics
70 are heated to by decentralized medium of isopropanoloC, add silane coupler DL602 and disperse 5min, then add inorganic antibacterial Agent zinc oxide disperses 30min, and drying, grinding, sieving obtain modified zinc oxide, and wherein DL602 dosages are 2%.Same method, obtain To titanate coupling agent JW-105 modifying titanium dioxides.
2) preparation of ultra-high molecular weight polyethylenes master batch
By 50% ultra-high molecular weight polyethylene, 30% LLDPE, 10% potassium titanate crystal whisker, 10% atoleine at a high speed It is well mixed in blender.Mixture is standby through double screw extruder extruding pelletization, wherein ultra-high molecular weight polyethylene molecular weight For 2,500,000, expressing technique is：One area's temperature 190oC, two area's temperature 190oC, three area's temperature 200oC, four area's temperature 200oC, five Area's temperature 200oC, six area's temperature 210oC, seven area's temperature 210oC, eight area's temperature 220oC, nine area's temperature 220oC, head temperature 210oC, screw speed 250 turns/min, melt pressure 25MPa.
3) preparation of activeness and quietness antibacterial polypropylene material
By 57% COPP, each 2% modified zinc oxide and titanium dioxide, 30% ultra-high molecular weight polyethylene master batch, 6% methyl-prop Olefin(e) acid ethylene oxidic ester graft polypropylene, 1% glyceryl tristearate, 1% dibutyitin maleate, each 0.5% primary antioxidant 1010 It is well mixed with auxiliary anti-oxidant 618 in super mixer, then extrudes mixture through double screw extruder to obtain enhancing increasing Tough antibacterial polypropylene material.Wherein polypropylene melt index is 25g/10min, and expressing technique is：One area's temperature 180oC, 2nd area Temperature 180oC, three area's temperature 190oC, four area's temperature 190oC, five area's temperature 190oC, six area's temperature 200oC, seven area's temperature 200oC, eight area's temperature 210oC, nine area's temperature 210oC, head temperature 200oC, 250 turns/min of screw speed, melt pressure 25MPa。
Comparative example 1
60 are heated to by decentralized medium of ethanoloC, add Silane coupling agent KH550 and disperse 5min, then add inorganic antiseptic Zinc oxide disperses 30min, and drying, grinding, sieving obtain modified zinc oxide, and wherein KH550 dosages are 0.5%.Then by 95.6% COPP, 1% modified zinc oxide, 2% maleic anhydride inoculated polypropylene, 0.5% glyceryl tristearate, 0.5% maleic acid two Butyl tin, each 0.2% primary antioxidant 1010 and auxiliary anti-oxidant 618 are well mixed in super mixer, then by mixture through double Screw extruder is extruded to obtain modified zinc oxide polypropylene material.Wherein polypropylene melt index is 25g/10min, expressing technique For：One area's temperature 180oC, two area's temperature 180oC, three area's temperature 190oC, four area's temperature 190oC, five area's temperature 190oC, six area's temperature Degree 200oC, seven area's temperature 200oC, eight area's temperature 210oC, nine area's temperature 210oC, head temperature 200oC, 250 turns of screw speed/ Min, melt pressure 25MPa.
Comparative example 2
70 are heated to by decentralized medium of isopropanoloC, add titanate coupling agent UP-131 and disperse 5min, then add inorganic Antiseptic titanium dioxide disperses 30min, and drying, grinding, sieving obtain modifying titanium dioxide, and wherein UP-131 dosages are 2%.With Afterwards by 84% COPP, 5% modifying titanium dioxide, 8% glycidyl methacrylate graft polypropylene, 1% 3 stearic acid Glyceride, 1% dibutyitin maleate, each 0.5% primary antioxidant 1010 and auxiliary anti-oxidant 618 mix in super mixer It is even, then mixture is extruded through double screw extruder to obtain titania modified polypropylene material.Wherein polypropylene fusion refers to Number is 25g/10min, and expressing technique is：One area's temperature 180oC, two area's temperature 180oC, three area's temperature 190oC, four area's temperature 190oC, five area's temperature 190oC, six area's temperature 200oC, seven area's temperature 200oC, eight area's temperature 210oC, nine area's temperature 210oC, machine Head temperature 200oC, screw speed 250 turns/min, melt pressure 25MPa.
Comparative example 3
By 40% ultra-high molecular weight polyethylene, 30% LLDPE, 15% calcium carbonate, 15% atoleine in mixed at high speed It is well mixed in device.Mixture is standby through double screw extruder extruding pelletization, and wherein ultra-high molecular weight polyethylene molecular weight is 150 Ten thousand, expressing technique is：One area's temperature 190oC, two area's temperature 190oC, three area's temperature 200oC, four area's temperature 200oC, five area's temperature 200oC, six area's temperature 210oC, seven area's temperature 210oC, eight area's temperature 220oC, nine area's temperature 220oC, head temperature 210oC, spiral shell Bar rotating speed 240 turns/min, melt pressure 23MPa.Then by 76% COPP, 20% ultra-high molecular weight polyethylene master batch, 2% Maleic anhydride inoculated polypropylene, 0.5% glyceryl tristearate, 0.5% dibutyitin maleate, each and of 0.5% primary antioxidant 1010 Auxiliary anti-oxidant 618 is well mixed in super mixer, then extrudes mixture through double screw extruder to obtain activeness and quietness Antibacterial polypropylene material.Wherein polypropylene melt index is 25g/10min, and expressing technique is：One area's temperature 180oC, two area's temperature Degree 180oC, three area's temperature 190oC, four area's temperature 190oC, five area's temperature 190oC, six area's temperature 200oC, seven area's temperature 200oC, Eight area's temperature 210oC, nine area's temperature 210oC, head temperature 200oC, screw speed 250 turns/min, melt pressure 25MPa.
Performance evaluation mode and implementation standard：
The particle that will be prepared as stated above, 80~90o5~6h is dried in C convection oven, then again by dried grain Son carries out injection moulding sample preparation in injector.
Tensile property is tested：Carried out by GB/T 1040-2006 standards, specimen size 170mm*10mm*4mm, stretching speed Rate is 50mm/min.
Bending property is tested：Carried out by GB/T 9341-2000 standards, specimen size 80mm*10mm*4mm, bending speed Spend for 2mm/min.
Simply supported beam notch impact strength is tested：GB/T 1043.1-2008 standards are carried out, and pattern size is 60mm*10mm* 4mm。
Anti-microbial property detection is investigated with reference to People's Republic of China's light industry standard QB/T2591-2003 film applicator coatings Sample 24h bacteriostasis rate, the measure of total plate count count with reference to QB/T4789.2-2003.By the antibacterial model system of injection formed Into 50mm*50mm.The calculating formula of antibiotic rate is as follows：
Wherein, B represents the average bacterial count recovered of control sample, cfu/ pieces；C represents antibiotic plastic sample average bacterial count recovered, cfu/ Piece.
。

Claims (10)

1. a kind of activeness and quietness antibacterial polypropylene material, using polypropylene as base material, it is characterised in that with inorganic antiseptic, superelevation point Sub- weight northylen master batch, graft polypropylene, dispersant, the proportioning of stabilizer and antioxidant percentage are as follows：
Polypropylene 54~87.7%；
Inorganic antiseptic 0.5~5%；
Ultra-high molecular weight polyethylene master batch 10~30%；
Graft polypropylene 1~8%；
Dispersant 0.2~1%；
Stabilizer 0.2~1%；
Antioxidant 0.4~1%.
2. activeness and quietness antibacterial polypropylene material as claimed in claim 1, it is characterised in that：Described polypropylene be homopolymerization and A kind of or their composition in COPP, its melt index are 1~25g/10min；Described antiseptic is to receive One or more in rice inorganic antibacterial, composite hybridization nano inorganic antimicrobial agent；Described graft polypropylene connects for maleic anhydride Branch polypropylene or one kind or their compositions in glycidyl methacrylate graft polypropylene.
3. activeness and quietness antibacterial polypropylene material as claimed in claim 1, it is characterised in that：Described dispersant is ethylene group One or more in bis-stearamides, glyceryl monostearate, glyceryl tristearate；Described stabilizer is organic tin One or more in middle dibutyl tin laurate, dibutyitin maleate, dibutyltin mercaptide.
4. activeness and quietness antibacterial polypropylene material as claimed in claim 1, it is characterised in that：Described antioxidant includes main anti- Oxygen agent and auxiliary anti-oxidant, primary antioxidant are the one or more in hindered phenol and sulphur ester antioxidant, and auxiliary anti-oxidant is phosphorous acid One or more in salt or esters antioxidant；The inorganic antiseptic being modified using coupling agent surface, wherein coupling agent is silane Coupling agent, titanate coupling agent, the one or more of aluminate coupling agent.
5. activeness and quietness antibacterial polypropylene material as claimed in claim 1, it is characterised in that：Described superhigh molecular weight polyethylene Alkene master batch is made up of following substances in percentage by weight：
Ultra-high molecular weight polyethylene 30~50%；
LLDPE 30~40%；
Inorganic particle 10~15%；
Compatilizer 10~15%.
6. activeness and quietness antibacterial polypropylene material as claimed in claim 5, it is characterised in that：Described superhigh molecular weight polyethylene The molecular weight of alkene is 150~5,000,000；Described LLDPE density is 0.92g/cm3, melt index 24g/ 10min。
7. activeness and quietness antibacterial polypropylene material as claimed in claim 5 and preparation method thereof, it is characterised in that：Described nothing Machine powder is the one or more in calcium carbonate, talcum powder, carbon fiber, glass fibre, silica, potassium titanate crystal whisker；It is described Compatilizer be atoleine, molecular weight is 100~200 g/mol.
8. the preparation method of activeness and quietness antibacterial polypropylene material as described in claim 1-7 is any, it is characterised in that by double Screw extruder by polypropylene, inorganic antiseptic, ultra-high molecular weight polyethylene master batch, graft polypropylene, dispersant, stabilizer and Cooling granulation after antioxidant melting extrusion, is made activeness and quietness antibacterial polypropylene material, and step is as follows：
（1）First at a certain temperature, using coupling agent to inorganic antiseptic carry out surface modification, surface modification temperature be 60~ 70oC, coupling agent dosage are 0.5~2%；
（2）Polypropylene, inorganic antiseptic, ultra-high molecular weight polyethylene master batch, graft polypropylene, scattered is weighed by weight ratio Agent, stabilizer and antioxidant mix 15~20 minutes in super mixer；
（3）Mixed raw material is added in double screw extruder, the cooling granulation after melting extrusion, expressing technique is：One area Temperature 180~190oC, two area's temperature 180~190oC, three area's temperature 190~200oC, four area's temperature 190~200oC, five area's temperature Degree 190~200oC, six area's temperature 200~210oC, seven area's temperature 200~210oC, eight area's temperature 210~220oC, nine area's temperature 210~220oC, head temperature 200~210oC, 200~250 revs/min of screw speed, 18~25MPa of pressure.
9. the preparation method of activeness and quietness antibacterial polypropylene material as described in claim 1-8 is any, it is characterised in that：Described Ultra-high molecular weight polyethylene master batch preparation process is as follows：By the ultra-high molecular weight polyethylene necessarily matched, linear low density polyethylene Alkene, inorganic particle and compatilizer are well mixed in super mixer, then by mixture through double screw extruder extruding pelletization, Expressing technique is：One area's temperature 190~200oC, two area's temperature 190~200oC, three area's temperature 200~210oC, four area's temperature 200~210oC, five area's temperature 200~210oC, six area's temperature 210~220oC, seven area's temperature 210~220oC, eight area's temperature 215~225oC, nine area's temperature 215~225oC, head temperature 200~220oC, 200~250 turns/min of screw speed, melt pressure 20~25MPa of power.
10. application of the activeness and quietness antibacterial polypropylene material as material for car interior trim parts as described in claim 1-7 is any.
CN201711056533.1A 2017-11-01 2017-11-01 Activeness and quietness antibacterial polypropylene material and its preparation method and application Withdrawn CN107793640A (en)

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CN109370029A (en) * 2018-09-21 2019-02-22 黄国飞 A kind of nano-antibacterial composite plastic master batch and preparation method thereof
CN109384993A (en) * 2018-10-12 2019-02-26 黄国飞 A kind of thermoplastic plastic parent particles that stretch-resistance is strong and its processing technology
CN109456563A (en) * 2018-09-06 2019-03-12 福建师范大学 A kind of UHMWPE alloy compatibilization and toughening modified polypropene ripple pipe as special material and preparation method thereof
CN111117073A (en) * 2020-01-09 2020-05-08 山东清河化工科技有限公司 Blending type ultrahigh molecular weight polypropylene/polypropylene alloy and preparation method thereof
CN112574488A (en) * 2019-09-30 2021-03-30 四川大学 Modified master batch for polyolefin reinforcement and toughening and preparation method thereof
CN114350075A (en) * 2022-02-11 2022-04-15 无锡市金华屹圆科技有限公司 Anti-bacterial water inlet pipe and processing technology thereof

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CN109456563A (en) * 2018-09-06 2019-03-12 福建师范大学 A kind of UHMWPE alloy compatibilization and toughening modified polypropene ripple pipe as special material and preparation method thereof
CN109456563B (en) * 2018-09-06 2021-05-04 福建师范大学 Special material for UHMWPE alloy compatibilization toughening modified polypropylene corrugated pipe and preparation method thereof
CN109370029A (en) * 2018-09-21 2019-02-22 黄国飞 A kind of nano-antibacterial composite plastic master batch and preparation method thereof
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CN112574488A (en) * 2019-09-30 2021-03-30 四川大学 Modified master batch for polyolefin reinforcement and toughening and preparation method thereof
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CN114350075A (en) * 2022-02-11 2022-04-15 无锡市金华屹圆科技有限公司 Anti-bacterial water inlet pipe and processing technology thereof
CN114350075B (en) * 2022-02-11 2022-09-13 无锡市金华屹圆科技有限公司 Anti-bacterial water inlet pipe and processing technology thereof

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Application publication date: 20180313