CN106589582A - Reinforced and toughened antibacterial polypropylene material and preparing method thereof - Google Patents
Reinforced and toughened antibacterial polypropylene material and preparing method thereof Download PDFInfo
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- 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
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Abstract
The invention relates to a reinforced and toughened antibacterial polypropylene material and a preparing method thereof. The polypropylene material is prepared from, be weight, 54-87.7% of polypropylene, 0.5%-5% of inorganic antibacterial agent, 10%-30% of ultra-high molecular weight polyethylene masterbatch, 1%-8% of graft polypropylene, 0.2%-1% of dispersant, 0.2%-1% of stabilizer and 0.4%-1% of antioxygen. The method comprises the steps of preparing ultra-high molecular weight polyethylene into ultra-high molecular weight polyethylene masterbatch under a certain condition, and then mixing and extruding inorganic antibacterial agent, polypropylene, ultra-high molecular weight polyethylene masterbatch, graft polypropylene and other auxiliaries at high speed to prepare the polypropylene composite material with high strengh,toughness and antibacterial property. According to the reinforcing and toughening antibacterial polypropylene material and the preparing method thereof, the inorganic antibacterial agent is ensured to be added to endow polypropylene with good antibacterial activity, and meanwhile polypropylene is reinforced and toughened by adding organic ultra-long chain macromolecules. The prepared reinforced and toughened antibacterial polypropylene material has the advantages of being good in antibacterial performance and remarkable in mechanical characteristic.
Description
Technical field
The present invention relates to activeness and quietness antibacterial polypropylene material and preparation method thereof, belongs to technical field of polymer materials.
Background technology
Data shows the various surface of plastic products contaminations touched in daily life and grows various pathogenic bacterias.Such as hotel
Antibacterial on restaurant's toilet seat has escherichia coli, staphylococcus aureuses, White staphylococcus, bacillus subtilis, tetracoccuss etc., bacterium
Fall to counting up to 40；The clump count of public telephone microphone is up to 50；Hospital, the clump count of the door handle at hotel even may be 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 at aspects such as household electrical appliance, packaging for foodstuff, toy for children, kitchen and sanitary bath equipments for the developed country of representative
Research, exploitation and the production work of material, to reduce because of the bacterium infection occurred using plastic.
Polypropylene is widely used in house as a kind of non-toxic plastic because density is little, price is low and good processing characteristics
Each field such as electrical appliance.But polypropylene is easily polluted by various noxious bacteria as other plastics, in the case of being adapted to, it is more easy to
Bacterial growth.Generally adopt now addition antibacterial to improve polyacrylic anti-microbial property.Conventional plastic antimicrobial agent can at present
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 antibacterial effect duration is short, heat resistance is poor.Inorganic antiseptic be mainly silver, zinc, titanium plasma and its
Compound, is characterized in heat-resist, safe, antibacterial effect duration length etc..Such as Chinese patent CN101089038A is disclosed
Nanometer silver addition polypropylene obtains a kind of antibiotic rate 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 nanometer silver, load silver and receives
Rice application of the oxide antibacterial in polypropylene, and obtain certain achievement.But silver-series antibacterial agent there is also many shortcomings, such as easily
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 as the impact energy for absorbing has little time transmission in time under low temperature or high strain rate
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 range of application, all having carried out substantial amounts of polypropylene both at home and abroad strengthens
The research and development of toughening modifying, has achieved certain achievement in terms of multiphase copolymer and blending and modifying.Such as Chinese patent
CN201110308569.0 discloses a kind of using rubber sulfonation flexibilized polypropylene material；Chinese patent CN201010214965.2
Disclose a kind of 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 a kind of 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 in disclosed research study of both Mechanical Properties of PP and antibacterial.
The content of the invention
To overcome the deficiencies in the prior art, the invention provides a kind of activeness and quietness antibacterial polypropylene material and its preparation side
Method, while the material use addition inorganic antiseptic gives polypropylene excellent anti-microbial property, by adding overlength chain high score
Son improves polyacrylic tensile strength and notch impact strength.
What the present invention was realized in.
A kind of activeness and quietness antibacterial polypropylene material, it is characterised in that polypropylene, inorganic antiseptic, super high molecular weight are gathered
The proportioning of ethylene master batch, graft polypropylene, dispersant, stabilizer and antioxidant percentage 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%.
Described polypropylene is the one kind in homopolymerization and COPP or its combination, and its melt index is 1～25g/
10min；During the graft polypropylene is maleic anhydride inoculated polypropylene or glycidyl methacrylate graft polypropylene
A kind of or its combination.
Described antibacterial is nano inorganic antibacterial, the one kind in composite hybridization nano inorganic antimicrobial agent or its combination；Institute
The dispersant stated is ethylene group bis-stearamides, glycerol monostearate, the one kind in glyceryl tristearate or its combination.
Described stabilizer is in dibutyl tin laurate, dibutyitin maleate, dibutyltin mercaptide in organic tin
One kind or its combination；Described antioxidant is primary antioxidant and auxiliary anti-oxidant, and primary antioxidant is hindered phenol and thioesters class antioxygen
One kind or its combination in agent, auxiliary anti-oxidant are the one kind in phosphorite kind antioxidant or its combination.
To increase the affinity of inorganic antiseptic and fluoropolymer resin, the inorganic antiseptic being modified using coupling agent surface,
Wherein coupling agent is silane coupler, titanate coupling agent, one kind of aluminate coupling agent or its combination.
Described ultra-high molecular weight polyethylene master batch is made up of following substances in percentage by weight：
Ultra-high molecular weight polyethylene 30～50%
Linear low density polyethylene 30～40%
Inorganic particle 10～15%
Compatilizer 10～15%
The molecular weight of described ultra-high molecular weight polyethylene is 150～5,000,000；Described linear low density polyethylene density is
0.92g/cm3, melt index is 24g/10min.
Described inorganic particle be Calcium Carbonate, Pulvis Talci, carbon fiber, glass fibre, silicon dioxide, in potassium titanate crystal whisker
A kind of or its combination；Described compatilizer is liquid paraffin, and molecular weight is 100～200 g/mol.
Described ultra-high molecular weight polyethylene master batch preparation process is as follows：By the ultra-high molecular weight polyethylene of certain proportioning,
Linear low density polyethylene, the inorganic particle and compatilizer mix homogeneously in super mixer, then by mixture Jing twin screw
Extruder extruding pelletization, expressing technique is：One 190～200 DEG C of area's temperature, two 190～200 DEG C of area's temperature, three area's temperature 200～
210 DEG C, four 200～210 DEG C of area's temperature, five 200～210 DEG C of area's temperature, six 210～220 DEG C of area's temperature, seven area's temperature 210～
220 DEG C, eight 215～225 DEG C of area's temperature, nine 215～225 DEG C of area's temperature, 200～220 DEG C of head temperature, screw speed 200～
250 turns/min, 20～25MPa of melt pressure.
A kind of preparation method of activeness and quietness antibacterial polypropylene material, it is characterised in that will be poly- by double screw extruder
Propylene, inorganic antiseptic, ultra-high molecular weight polyethylene master batch, graft polypropylene, dispersant, stabilizer and antioxidant melting extrusion
Cooling granulation, is obtained activeness and quietness antibacterial polypropylene material afterwards, and step is as follows：
（1）First at a certain temperature, using coupling agent inorganic antiseptic is carried out surface be modified, surface modification temperature be 60～
70 DEG C, coupling agent consumption is 0.5～2%；
（2）Polypropylene, inorganic antiseptic, ultra-high molecular weight polyethylene master batch, graft polypropylene, dispersion are weighed by weight ratio
Agent, stabilizer and antioxidant mix in super mixer 15～20 minutes；
（3）Mixed raw material is added in double screw extruder, the cooling granulation Jing after melting extrusion, expressing technique is：One area
180～190 DEG C of temperature, two 180～190 DEG C of area's temperature, three 190～200 DEG C of area's temperature, four 190～200 DEG C of area's temperature, 5th area
190～200 DEG C of temperature, six 200～210 DEG C of area's temperature, seven 200～210 DEG C of area's temperature, eight 210～220 DEG C of area's temperature, 9th area
210～220 DEG C of temperature, 200～210 DEG C of head temperature, 200～250 revs/min of screw speed, 18～25MPa of pressure.
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 subject to external impacts, absorbs a large amount of punching by causing the crazing and shear yielding of 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 is improved
, 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 clad be formed in inorganic antiseptic particle surface, reduce the antimicrobial efficiency of inorganic antiseptic.Cause
This, simply adds flexible polymer in inorganic antiseptic/Pp System, although improve polyacrylic to a certain extent
Toughness, but the antimicrobial efficiency with sacrificial inorganic antibacterial is as cost to a great extent.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 using super long chain macromolecule is introduced in polypropylene matrix, using overlength strand shape in the base
Into the framing structure of physical entanglement, when material is subject to external force to act on, in matrix, the skeleton of this entanglement absorbs and transmits impact
Can, to play a part of activeness and quietness.For example, using the PE modified polypropylene that molecular weight is high so as to polypropylene melt
Melt blending and form linear interpenetrating networks or physical cross-linked network, when material under external force, there is large deformation in network, absorb outer
Boundary's energy, plays 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 not with mobility.
The present invention adopts linear low density polyethylene for carrier, and the alkane and super high molecular weight for adding certain low-molecular-weight gathers
Ethylene melt blending generates low viscous ultra-high molecular weight polyethylene master batch；Using nano zine oxide or titanium dioxide as inorganic
Then polypropylene, ultra-high molecular weight polyethylene master batch, inorganic antiseptic, graft polypropylene and other auxiliary agents are passed through by antibacterial
Double screw extruder melt blending extrusion obtains 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 by the use of linear low density polyethylene as carrier
Low viscous ultra-high molecular weight polyethylene master batch is generated with ultra-high molecular weight polyethylene melt blending extrusion；（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 effect that：The polypropylene material that the present invention is prepared
Material antibacterial more rapidly, it is more longlasting, safer；Simultaneously present invention uses super long chain macromolecule improves material as filler
Mechanical property, widened the range of application of antibacterial polypropylene material.
Description of the drawings
Fig. 1 is the TEM pictures of KH550 modified nano zinc oxide powder body in embodiment 1.
Fig. 2 is 3 polypropylene impact fracture surface SEM photograph of embodiment.
Specific embodiment
Following embodiment is that the present invention is further illustrated, and the present invention is not limited to following examples and reality
Applying method.
Embodiment 1
（1) surface modification of inorganic antiseptic
60 DEG C are heated to by disperse medium of ethanol, Silane coupling agent KH550 dispersion 5min are added, is subsequently adding inorganic antiseptic
Zinc Oxide disperses 30min, dries, grinds, sieving obtains modified zinc oxide, and wherein KH550 consumptions are 0.5%.
（2) preparation of ultra-high molecular weight polyethylene master batch
By 30% ultra-high molecular weight polyethylene, 40% linear low density polyethylene, 15% Calcium Carbonate, 15% liquid paraffin in mixed at high speed
Mix homogeneously in device.Mixture Jing double screw extruder extruding pelletizations are standby, and wherein ultra-high molecular weight polyethylene molecular weight is 150
Ten thousand, expressing technique is：One 190 DEG C of area's temperature, two 190 DEG C of area's temperature, three 200 DEG C of area's temperature, four 200 DEG C of area's temperature, five area's temperature
200 DEG C of degree, six 210 DEG C of area's temperature, seven 210 DEG C of area's temperature, eight 215 DEG C of area's temperature, nine 215 DEG C of area's temperature, head temperature 200
DEG C, 200 turns/min of screw speed, melt pressure 20MPa.
（3) preparation of activeness and quietness antibacterial polypropylene material
Will be 87.7% HOPP, 0.5% modified zinc oxide, 10% ultra-high molecular weight polyethylene master batch, the grafting of 1% maleic anhydride poly-
Propylene, 0.2% glycerol monostearate, 0.2% dibutyl tin laurate, each 0.2% primary antioxidant 3114 and auxiliary anti-oxidant 168 exist
Then mixture Jing double screw extruders extrusion is obtained activeness and quietness antibacterial polypropylene material by mix homogeneously in super mixer
Material.Wherein polypropylene melt index is 1g/10min, and expressing technique is：One 180 DEG C of area's temperature, two 180 DEG C of area's temperature, three area's temperature
190 DEG C of degree, four 190 DEG C of area's temperature, five 190 DEG C of area's temperature, six 200 DEG C of area's temperature, seven 200 DEG C of area's temperature, eight area's temperature 210
DEG C, nine 210 DEG C of area's temperature, 200 DEG C of head temperature, 200 turns/min of screw speed, melt pressure 18MPa.
Embodiment 2
（1) surface modification of inorganic antiseptic
60 DEG C are heated to by disperse medium of ethanol, Silane coupling agent KH550 dispersion 5min are added, is subsequently adding inorganic antiseptic
Zinc Oxide disperses 30min, dries, grinds, sieving obtains modified zinc oxide, and wherein KH550 consumptions are 0.5%.
（2) preparation of ultra-high molecular weight polyethylene master batch
By 50% ultra-high molecular weight polyethylene, 30% linear low density polyethylene, 10% Calcium Carbonate, 10% liquid paraffin in mixed at high speed
Mix homogeneously in device.Mixture Jing double screw extruder extruding pelletizations are standby, and wherein ultra-high molecular weight polyethylene molecular weight is 150
Ten thousand, expressing technique is：One 200 DEG C of area's temperature, two 200 DEG C of area's temperature, three 210 DEG C of area's temperature, four 210 DEG C of area's temperature, five area's temperature
210 DEG C of degree, six 220 DEG C of area's temperature, seven 220 DEG C of area's temperature, eight 225 DEG C of area's temperature, nine 225 DEG C of area's temperature, head temperature 220
DEG C, 250 turns/min of screw speed, melt pressure 25MPa.
(3) preparation of activeness and quietness antibacterial polypropylene material
Will be 67.7% HOPP, 0.5% modified zinc oxide, 30% ultra-high molecular weight polyethylene master batch, the grafting of 1% maleic anhydride poly-
Propylene, 0.2% glycerol monostearate, 0.2% dibutyl tin laurate, each 0.2% primary antioxidant 3114 and auxiliary anti-oxidant 168 exist
Then mixture Jing double screw extruders extrusion is obtained activeness and quietness antibacterial polypropylene material by mix homogeneously in super mixer
Material.Wherein polypropylene melt index is 1g/10min, and expressing technique is：One 190 DEG C of area's temperature, two 190 DEG C of area's temperature, three area's temperature
200 DEG C of degree, four 200 DEG C of area's temperature, five 200 DEG C of area's temperature, six 210 DEG C of area's temperature, seven 210 DEG C of area's temperature, eight area's temperature 220
DEG C, nine 220 DEG C of area's temperature, 210 DEG C of head temperature, 230 turns/min of screw speed, melt pressure 20MPa.
Embodiment 3
（1). the surface modification of inorganic antiseptic
70 DEG C are heated to by disperse medium of isopropanol, silane coupler DL602 dispersion 5min are added, is subsequently adding inorganic antibacterial
Agent Zinc Oxide disperses 30min, dries, grinds, sieving obtains modified zinc oxide, and wherein DL602 consumptions are 2%.
（2) preparation of ultra-high molecular weight polyethylene master batch
By 30% ultra-high molecular weight polyethylene, 40% linear low density polyethylene, 15% Pulvis Talci, 15% liquid paraffin in mixed at high speed
Mix homogeneously in device.Mixture Jing double screw extruder extruding pelletizations are standby, and wherein ultra-high molecular weight polyethylene molecular weight is 150
Ten thousand, expressing technique is：One 190 DEG C of area's temperature, two 190 DEG C of area's temperature, three 200 DEG C of area's temperature, four 200 DEG C of area's temperature, five area's temperature
200 DEG C of degree, six 210 DEG C of area's temperature, seven 210 DEG C of area's temperature, eight 215 DEG C of area's temperature, nine 215 DEG C of area's temperature, head temperature 200
DEG C, 200 turns/min of screw speed, 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% glycerol monostearate, 1% dibutyl tin laurate, each 0.5% primary antioxidant 3114 and auxiliary anti-oxidant 168 are mixed in high speed
Then mixture Jing double screw extruders extrusion is obtained activeness and quietness antibacterial polypropylene material by mix homogeneously in clutch.Wherein
Polypropylene melt index is 1g/10min, and expressing technique is：One 180 DEG C of area's temperature, two 180 DEG C of area's temperature, three area's temperature 190
DEG C, four 190 DEG C of area's temperature, five 190 DEG C of area's temperature, six 200 DEG C of area's temperature, seven 200 DEG C of area's temperature, eight 210 DEG C of area's temperature, 9th area
210 DEG C of temperature, 200 DEG C of head temperature, 200 turns/min of screw speed, melt pressure 20MPa.
Embodiment 4
（1) surface modification of inorganic antiseptic
70 DEG C are heated to by disperse medium of ethanol, titanate coupling agent UP-131 dispersion 5min are added, are subsequently adding inorganic anti-
Microbial inoculum Zinc Oxide disperses 30min, dries, grinds, sieving obtains modified zinc oxide, and wherein UP-131 consumptions are 1%.
（2) preparation of ultra-high molecular weight polyethylene master batch
By 50% ultra-high molecular weight polyethylene, 30% linear low density polyethylene, 10% potassium titanate crystal whisker, 10% liquid paraffin at a high speed
Mix homogeneously in blender.Mixture Jing double screw extruder extruding pelletizations are standby, wherein ultra-high molecular weight polyethylene molecular weight
For 1,500,000, expressing technique is：One 200 DEG C of area's temperature, two 200 DEG C of area's temperature, three 210 DEG C of area's temperature, four 210 DEG C of area's temperature, five
210 DEG C of area's temperature, six 220 DEG C of area's temperature, seven 220 DEG C of area's temperature, eight 225 DEG C of area's temperature, nine 225 DEG C of area's temperature, head temperature
220 DEG C, 250 turns/min of screw speed, 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% glycerol monostearate, 1% dibutyl tin laurate, each 0.5% primary antioxidant 1010 and auxiliary anti-oxidant 168 are mixed in high speed
Then mixture Jing double screw extruders extrusion is obtained activeness and quietness antibacterial polypropylene material by mix homogeneously in clutch.Wherein
Polypropylene melt index is 1g/10min, and expressing technique is：One 190 DEG C of area's temperature, two 190 DEG C of area's temperature, three area's temperature 200
DEG C, four 200 DEG C of area's temperature, five 200 DEG C of area's temperature, six 210 DEG C of area's temperature, seven 210 DEG C of area's temperature, eight 220 DEG C of area's temperature, 9th area
220 DEG C of temperature, 210 DEG C of head temperature, 250 turns/min of screw speed, melt pressure 25MPa.
Embodiment 5
（1) surface modification of inorganic antiseptic
60 DEG C are heated to by disperse medium of ethanol, Silane coupling agent KH550 dispersion 5min are added, is subsequently adding inorganic antiseptic
Titanium dioxide disperses 30min, dries, grinds, sieving obtains modifying titanium dioxide, and wherein KH550 consumptions are 0.5%.
（2) preparation of ultra-high molecular weight polyethylene master batch
By 30% ultra-high molecular weight polyethylene, 40% linear low density polyethylene, 15% Calcium Carbonate, 15% liquid paraffin in mixed at high speed
Mix homogeneously in device.Mixture Jing double screw extruder extruding pelletizations are standby, and wherein ultra-high molecular weight polyethylene molecular weight is 150
Ten thousand, expressing technique is：One 190 DEG C of area's temperature, two 190 DEG C of area's temperature, three 200 DEG C of area's temperature, four 200 DEG C of area's temperature, five area's temperature
200 DEG C of degree, six 210 DEG C of area's temperature, seven 210 DEG C of area's temperature, eight 215 DEG C of area's temperature, nine 215 DEG C of area's temperature, head temperature 200
DEG C, 200 turns/min of screw speed, 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% glycerol monostearate, 0.2% dibutyl tin laurate, each 0.2% primary antioxidant 3114 and auxiliary anti-oxidant 168
Then mixture Jing double screw extruders extrusion is obtained activeness and quietness antibacterial polypropylene material by the mix homogeneously in super mixer
Material.Wherein polypropylene melt index is 1g/10min, and expressing technique is：One 180 DEG C of area's temperature, two 180 DEG C of area's temperature, three area's temperature
190 DEG C of degree, four 190 DEG C of area's temperature, five 190 DEG C of area's temperature, six 200 DEG C of area's temperature, seven 200 DEG C of area's temperature, eight area's temperature 210
DEG C, nine 210 DEG C of area's temperature, 200 DEG C of head temperature, 200 turns/min of screw speed, melt pressure 18MPa.
Embodiment 6
（1) surface modification of inorganic antiseptic
65 DEG C are heated to by disperse medium of isopropanol, titanate coupling agent UP-131 dispersion 5min are added, is subsequently adding inorganic
Antibacterial titanium dioxide disperses 30min, dries, grinds, sieving obtains modifying titanium dioxide, and wherein UP-131 consumptions are 2%.
（2) preparation of ultra-high molecular weight polyethylene master batch
By 50% ultra-high molecular weight polyethylene, 30% linear low density polyethylene, 10% Pulvis Talci, 10% liquid paraffin in mixed at high speed
Mix homogeneously in device.Mixture Jing double screw extruder extruding pelletizations are standby, and wherein ultra-high molecular weight polyethylene molecular weight is 500
Ten thousand, expressing technique is：One 200 DEG C of area's temperature, two 200 DEG C of area's temperature, three 210 DEG C of area's temperature, four 210 DEG C of area's temperature, five area's temperature
210 DEG C of degree, six 220 DEG C of area's temperature, seven 220 DEG C of area's temperature, eight 225 DEG C of area's temperature, nine 225 DEG C of area's temperature, head temperature 220
DEG C, 250 turns/min of screw speed, melt pressure 25MPa.
（3) preparation of activeness and quietness antibacterial polypropylene material
Will be 54% COPP, 5% modifying titanium dioxide, 30% ultra-high molecular weight polyethylene master batch, 8% Glycidyl methacrylate sweet
Grease graft polypropylene, 1% glyceryl tristearate, 1% dibutyitin maleate, each 0.5% primary antioxidant 1010 and auxiliary anti-oxidant
618 in super mixer mix homogeneously, then by mixture Jing double screw extruders extrusion obtain activeness and quietness antibacterial poly- third
Alkene material.Wherein polypropylene melt index is 25g/10min, and expressing technique is：One 190 DEG C of area's temperature, two 190 DEG C of area's temperature,
Three 200 DEG C of area's temperature, four 200 DEG C of area's temperature, five 200 DEG C of area's temperature, six 210 DEG C of area's temperature, seven 210 DEG C of area's temperature, eight area's temperature
220 DEG C of degree, nine 220 DEG C of area's temperature, 210 DEG C of head temperature, 250 turns/min of screw speed, melt pressure 25MPa.
Embodiment 7
（1) surface modification of inorganic antiseptic
60 DEG C are heated to by disperse medium of ethanol, Silane coupling agent KH550 dispersion 5min are added, is subsequently adding inorganic antiseptic
Zinc Oxide disperses 30min, dries, grinds, sieving obtains modified zinc oxide, and wherein KH550 consumptions are 0.5%.Same method, obtains
To titanate coupling agent UP-131 modifying titanium dioxides.
（2) preparation of ultra-high molecular weight polyethylene master batch
By 30% ultra-high molecular weight polyethylene, 40% linear low density polyethylene, 15% Calcium Carbonate, 15% liquid paraffin in mixed at high speed
Mix homogeneously in device.Mixture Jing double screw extruder extruding pelletizations are standby, and wherein ultra-high molecular weight polyethylene molecular weight is 250
Ten thousand, expressing technique is：One 190 DEG C of area's temperature, two 190 DEG C of area's temperature, three 200 DEG C of area's temperature, four 200 DEG C of area's temperature, five area's temperature
200 DEG C of degree, six 210 DEG C of area's temperature, seven 210 DEG C of area's temperature, eight 215 DEG C of area's temperature, nine 215 DEG C of area's temperature, head temperature 200
DEG C, 200 turns/min of screw speed, 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% glycerol monostearate, 0.5% dibutyl tin laurate, each 0.5% primary antioxidant 3114 and auxiliary anti-
Then mixture Jing double screw extruders extrusion is obtained activeness and quietness antibacterial by the mix homogeneously in super mixer of oxygen agent 168
Polypropylene material.Wherein polypropylene melt index is 25g/10min, and expressing technique is：One 180 DEG C of area's temperature, two area's temperature 180
DEG C, three 190 DEG C of area's temperature, four 190 DEG C of area's temperature, five 190 DEG C of area's temperature, six 200 DEG C of area's temperature, seven 200 DEG C of area's temperature, 8th area
210 DEG C of temperature, nine 210 DEG C of area's temperature, 200 DEG C of head temperature, 200 turns/min of screw speed, melt pressure 18MPa.
Embodiment 8
（1) surface modification of inorganic antiseptic
70 DEG C are heated to by disperse medium of isopropanol, silane coupler DL602 dispersion 5min are added, is subsequently adding inorganic antibacterial
Agent Zinc Oxide disperses 30min, dries, grinds, sieving obtains modified zinc oxide, and wherein DL602 consumptions are 2%.Same method, obtains
To titanate coupling agent JW-105 modifying titanium dioxides.
(2) preparation of ultra-high molecular weight polyethylene master batch
By 50% ultra-high molecular weight polyethylene, 30% linear low density polyethylene, 10% potassium titanate crystal whisker, 10% liquid paraffin at a high speed
Mix homogeneously in blender.Mixture Jing double screw extruder extruding pelletizations are standby, wherein ultra-high molecular weight polyethylene molecular weight
For 2,500,000, expressing technique is：One 190 DEG C of area's temperature, two 190 DEG C of area's temperature, three 200 DEG C of area's temperature, four 200 DEG C of area's temperature, five
200 DEG C of area's temperature, six 210 DEG C of area's temperature, seven 210 DEG C of area's temperature, eight 220 DEG C of area's temperature, nine 220 DEG C of area's temperature, head temperature
210 DEG C, 250 turns/min of screw speed, 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
With auxiliary anti-oxidant 618 in super mixer mix homogeneously, then by mixture Jing double screw extruders extrusion obtain strengthen increase
Tough antibacterial polypropylene material.Wherein polypropylene melt index is 25g/10min, and expressing technique is：One 180 DEG C of area's temperature, 2nd area
180 DEG C of temperature, three 190 DEG C of area's temperature, four 190 DEG C of area's temperature, five 190 DEG C of area's temperature, six 200 DEG C of area's temperature, seven area's temperature 200
DEG C, eight 210 DEG C of area's temperature, nine 210 DEG C of area's temperature, 200 DEG C of head temperature, 250 turns/min of screw speed, melt pressure 25MPa.
Comparative example 1
60 DEG C are heated to by disperse medium of ethanol, Silane coupling agent KH550 dispersion 5min are added, is subsequently adding inorganic antiseptic
Zinc Oxide disperses 30min, dries, grinds, sieving obtains modified zinc oxide, and wherein KH550 consumptions 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 mix homogeneously in super mixer, it is then that mixture Jing is double
Screw extruder extrusion obtains modified zinc oxide polypropylene material.Wherein polypropylene melt index be 25g/10min, expressing technique
For：One 180 DEG C of area's temperature, two 180 DEG C of area's temperature, three 190 DEG C of area's temperature, four 190 DEG C of area's temperature, five 190 DEG C of area's temperature, 6th area
200 DEG C of temperature, seven 200 DEG C of area's temperature, eight 210 DEG C of area's temperature, nine 210 DEG C of area's temperature, 200 DEG C of head temperature, screw speed 250
Turn/min, melt pressure 25MPa.
Comparative example 2
70 DEG C are heated to by disperse medium of isopropanol, titanate coupling agent UP-131 dispersion 5min are added, is subsequently adding inorganic
Antibacterial titanium dioxide disperses 30min, dries, grinds, sieving obtains modifying titanium dioxide, and wherein UP-131 consumptions 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, mixture Jing double screw extruders extrusion is obtained into titania modified polypropylene material then.Wherein polypropylene fusion refers to
It is 25g/10min to count, and expressing technique is：One 180 DEG C of area's temperature, two 180 DEG C of area's temperature, three 190 DEG C of area's temperature, four area's temperature
190 DEG C, five 190 DEG C of area's temperature, six 200 DEG C of area's temperature, seven 200 DEG C of area's temperature, eight 210 DEG C of area's temperature, nine 210 DEG C of area's temperature,
200 DEG C of head temperature, 250 turns/min of screw speed, melt pressure 25MPa.
Comparative example 3
By 40% ultra-high molecular weight polyethylene, 30% linear low density polyethylene, 15% Calcium Carbonate, 15% liquid paraffin in mixed at high speed
Mix homogeneously in device.Mixture Jing double screw extruder extruding pelletizations are standby, and wherein ultra-high molecular weight polyethylene molecular weight is 150
Ten thousand, expressing technique is：One 190 DEG C of area's temperature, two 190 DEG C of area's temperature, three 200 DEG C of area's temperature, four 200 DEG C of area's temperature, five area's temperature
200 DEG C of degree, six 210 DEG C of area's temperature, seven 210 DEG C of area's temperature, eight 220 DEG C of area's temperature, nine 220 DEG C of area's temperature, head temperature 210
DEG C, 240 turns/min of screw speed, melt pressure 23MPa.Subsequently by 76% COPP, 20% ultra-high molecular weight polyethylene is female
Grain, 2% maleic anhydride inoculated polypropylene, 0.5% glyceryl tristearate, 0.5% dibutyitin maleate, each 0.5% primary antioxidant
1010 and the mix homogeneously in super mixer of auxiliary anti-oxidant 618, then mixture Jing double screw extruders extrusion is increased
Strong toughness reinforcing antibacterial polypropylene material.Wherein polypropylene melt index is 25g/10min, and expressing technique is：One 180 DEG C of area's temperature,
Two 180 DEG C of area's temperature, three 190 DEG C of area's temperature, four 190 DEG C of area's temperature, five 190 DEG C of area's temperature, six 200 DEG C of area's temperature, seven area's temperature
200 DEG C of degree, eight 210 DEG C of area's temperature, nine 210 DEG C of area's temperature, 200 DEG C of head temperature, 250 turns/min of screw speed, melt pressure
25MPa。
Performance evaluation mode and implementation standard：
By the particle for preparing as stated above, 5～6h is dried in 80～90 DEG C of convection oven, then again by dried grain
Son carries out injection moulding sample preparation in injector.
Tensile property is tested：Carry out by GB/T 1040-2006 standards, specimen size is 170mm*10mm*4mm, stretching speed
Rate is 50mm/min.
Bending property is tested：Carry out by GB/T 9341-2000 standards, specimen size is 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 coating
The bacteriostasis rate of sample 24h, the measure of total plate count are counted 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.
1 embodiment of table, 1～8 mechanics and anti-microbial property
TEM photos of the Fig. 1 for Silane coupling agent KH550 modified nano zinc oxide powder body in embodiment 1, modified nano zine oxide
Reunion degree reduces.
SEM photographs of the Fig. 2 for 3 polypropylene impact fracture surface of embodiment, nano zine oxide are uniformly dispersed in polypropylene.
Claims (10)
1. a kind of activeness and quietness antibacterial polypropylene material, it is characterised in that polypropylene, inorganic antiseptic, superhigh molecular weight polyethylene
The proportioning of alkene master batch, graft polypropylene, dispersant, stabilizer and antioxidant percentage 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%.
2. activeness and quietness antibacterial polypropylene material as claimed in claim 1, it is characterised in that described polypropylene be homopolymerization and
One kind or its combination in COPP, its melt index is 1～25g/10min；The graft polypropylene is maleic anhydride
One kind or its combination in graft polypropylene or glycidyl methacrylate graft polypropylene.
3. activeness and quietness antibacterial polypropylene material as claimed in claim 1, it is characterised in that described antibacterial is nanometer nothing
One kind or its combination in machine antibacterial, composite hybridization nano inorganic antimicrobial agent；Described dispersant be ethylene group bis-stearamides,
One kind or its combination in glycerol monostearate, glyceryl tristearate.
4. activeness and quietness antibacterial polypropylene material as claimed in claim 1, it is characterised in that described stabilizer is organotin
One kind or its combination in apoplexy due to endogenous wind dibutyl tin laurate, dibutyitin maleate, dibutyltin mercaptide；Described antioxidant is
Primary antioxidant and auxiliary anti-oxidant, primary antioxidant are the one kind in hindered phenol and sulphur ester antioxidant or its combination, and auxiliary anti-oxidant is
One kind or its combination in phosphorite kind antioxidant.
5. the activeness and quietness antibacterial polypropylene material as described in claim 1-4 is arbitrary, it is characterised in that to increase inorganic antibacterial
The affinity of agent and fluoropolymer resin, the inorganic antiseptic being modified using coupling agent surface, wherein coupling agent be silane coupler,
Titanate coupling agent, one kind of aluminate coupling agent or its combination.
6. 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%
Linear low density polyethylene 30～40%
Inorganic particle 10～15%
Compatilizer 10～15%.
7. activeness and quietness antibacterial polypropylene material as claimed in claim 6, it is characterised in that described superhigh molecular weight polyethylene
The molecular weight of alkene is 150～5,000,000；Described linear low density polyethylene density is 0.92g/cm3, melt index is 24g/
10min。
8. activeness and quietness antibacterial polypropylene material as claimed in claim 6, it is characterised in that described inorganic particle is carbonic acid
One kind or its combination in calcium, Pulvis Talci, carbon fiber, glass fibre, silicon dioxide, potassium titanate crystal whisker；Described compatilizer is
Liquid paraffin, molecular weight are 100～200 g/mol.
9. the activeness and quietness antibacterial polypropylene material as described in claim 6-8 is arbitrary, it is characterised in that described supra polymer
Weight northylen master batch preparation process is as follows：By the ultra-high molecular weight polyethylene of certain proportioning, linear low density polyethylene, inorganic powder
The body and compatilizer mix homogeneously in super mixer, then by mixture Jing double screw extruder extruding pelletizations, expressing technique
For：One 190～200 DEG C of area's temperature, two 190～200 DEG C of area's temperature, three 200～210 DEG C of area's temperature, four area's temperature 200～210
DEG C, five 200～210 DEG C of area's temperature, six 210～220 DEG C of area's temperature, seven 210～220 DEG C of area's temperature, eight area's temperature 215～225
DEG C, nine 215～225 DEG C of area's temperature, 200～220 DEG C of head temperature, 200～250 turns/min of screw speed, melt pressure 20～
25MPa。
10., according to a kind of arbitrary preparation method of activeness and quietness antibacterial polypropylene material of claim 1-5, its feature exists
In by double screw extruder by polypropylene, inorganic antiseptic, ultra-high molecular weight polyethylene master batch, graft polypropylene, dispersion
Cooling granulation after agent, stabilizer and antioxidant melting extrusion, is obtained activeness and quietness antibacterial polypropylene material, and step is as follows：
（1）First at a certain temperature, using coupling agent inorganic antiseptic is carried out surface be modified, surface modification temperature be 60～
70 DEG C, coupling agent consumption is 0.5～2%；
（2）Polypropylene, inorganic antiseptic, ultra-high molecular weight polyethylene master batch, graft polypropylene, dispersion are weighed by weight ratio
Agent, stabilizer and antioxidant mix in super mixer 15～20 minutes；
（3）Mixed raw material is added in double screw extruder, the cooling granulation Jing after melting extrusion, expressing technique is：One area
180～190 DEG C of temperature, two 180～190 DEG C of area's temperature, three 190～200 DEG C of area's temperature, four 190～200 DEG C of area's temperature, 5th area
190～200 DEG C of temperature, six 200～210 DEG C of area's temperature, seven 200～210 DEG C of area's temperature, eight 210～220 DEG C of area's temperature, 9th area
210～220 DEG C of temperature, 200～210 DEG C of head temperature, 200～250 revs/min of screw speed, 18～25MPa of pressure.
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| CN107793640A (en) * | 2017-11-01 | 2018-03-13 | 上海纳米技术及应用国家工程研究中心有限公司 | Activeness and quietness antibacterial polypropylene material and its preparation method and application |
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| CN108034148A (en) * | 2017-12-28 | 2018-05-15 | 东北林业大学 | A kind of antibacterial type cellulose/PP composite material and preparation method |
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Application publication date: 20170426 |