CN101747548A - Compound for preparation of high-strength polyolefin permeable membrane and preparation method thereof - Google Patents
Compound for preparation of high-strength polyolefin permeable membrane and preparation method thereof Download PDFInfo
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- CN101747548A CN101747548A CN200810220057A CN200810220057A CN101747548A CN 101747548 A CN101747548 A CN 101747548A CN 200810220057 A CN200810220057 A CN 200810220057A CN 200810220057 A CN200810220057 A CN 200810220057A CN 101747548 A CN101747548 A CN 101747548A
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Abstract
The invention discloses a compound for preparation of a high-strength polyolefin permeable membrane and a preparation method thereof. The compound comprises the following components in parts by weight: 35-65 of polyolefin resin, 30-60 of micron inorganic filler, 1-10 of nano inorganic filler, 0.2-0.5 of antioxidant, 0.1-1.0 of processing aid and 0.1-3.0 of coupling agent. The invention can improve the mechanical properties of the polyolefin permeable membrane through reasonable selection of the polyolefin resin and the nano inorganic filler, thereby reducing the thickness of the permeable membrane under the condition that the use requirements are satisfied. Moreover, the invention not only can fully develop the strengthening function of the nano filler, but also can obtain the permeable membrane with uniform aperture distribution and with water pressure resistance up to 100cm through the reasonable surface processing and the economical process flow. The transverse tensile strength of the permeable membrane is higher than 15MPa, the vertical tensile strength of the permeable membrane is higher than 30MPa, and the water pressure test reaches a 100cm water column, that is, the membrane can bear the 100cm water column without water permeation, breakage and the like.
Description
Technical field
The present invention relates to the polyolefin permeable membrane technical field, specifically, relate to a kind of mixture and technology of preparing thereof that is used to prepare high-strength polyolefin permeable membrane.
Background technology
Air-permeable envelope can by with thermoplastic polymer with after a certain proportion of mineral filler mixes, by forcing machine casting film-forming or blowing film forming, carry out vertical or horizontal stretching then, make and around filler particles, form the space, the size in this space can be controlled, its allow gases such as water vapour, air by but do not allow liquid to pass through, thereby obtain the polyolefin permeable membrane of permeable watertight.
This functional film product has been widely used in fields such as personal hygiene article, medical garment, food product pack, farm crop are fresh-keeping, buildings waterproof at present.In these fields, after overwhelming majority occasion need be carried out surface printing with air-permeable envelope, carry out to use after compound with other materials such as non-woven fabrics again, along with market competition is growing more intense and the continuous enhancing of people's environmental consciousness, on the market light-weighted requirement has been proposed air-permeable envelope, promptly require satisfying under the situation of service requirements, reduce the weight per unit area or the thickness of air-permeable envelope.
For example, the baby paper diaper counterdie generally is by non-woven fabrics and 35g/m
2The dry type of air-permeable envelope compound, but market demands are reduced to 20g/m with the grammes per square metre of air-permeable envelope
2Below, to reduce product cost, the reduction of air-permeable envelope grammes per square metre simultaneously also can improve the comfort of human body.
Along with reducing of air-permeable envelope grammes per square metre, under the identical situation of material, the intensity of film unavoidably can reduce, thereby problems such as vertical wrinkle, " sudden and violent muscle ", register trouble appear in printing process at film easily, disconnected film, vertical wrinkle etc. then appear in recombination process at film easily, have a strong impact on production efficiency, when especially using advanced printing press and dry compound machine, because the line speed height, the intensity of film there is higher requirement.On the other hand, to most of goods, as baby paper diaper and sanitary napkin, along with reducing of air-permeable envelope grammes per square metre, if the mechanical property of air-permeable envelope is not improved, the human consumer occurs air-permeable envelope in use easily and splits and pollution clothes cruelly.Therefore, no matter be finished product and half-finished course of processing, or human consumer's use, along with reducing of air-permeable envelope grammes per square metre, more and more higher requirement has been proposed for the mechanical property (as tensile strength, water pressure resistance etc.) of air-permeable envelope.
Chinese patent application 03812642.7 discloses a kind of filler that uses bimodal linear low density polyethylene and median size to be in 0.1 micron～10 microns mix by a certain percentage after, obtain a kind of air-permeable envelope that higher water vapour permeability and favorable mechanical performance and good processing characteristics combine that has.This patent focuses on uses physical strength and the processing characteristics of bimodal linear low density polyethylene with the balance film, and its purpose is for grammes per square metre that reduces air-permeable envelope or thickness equally.But along with the reduction of film grammes per square metre, the extrusion capacity of forcing machine will reduce, and the plasticating capacity of forcing machine has more than needed largely, therefore, along with market demands constantly reduce the air-permeable envelope grammes per square metre, should more focus on the mechanical property that improves air-permeable envelope.Because contain some low molecular weight polyethylene in the bimodal linear low density polyethylene to regulate processibility, the physical strength of film unavoidably will be affected.In addition, nano-sized filler (particle diameter is less than 0.1 micron) is also not mentioned to improving acting in this patent of film mechanical property.
Chinese patent 200610034689.5 discloses a kind of materials dedicated for antibacterial and permeable polyolefin film and preparation method thereof.After the water-ground limestone of 10～30 parts nano-calcium carbonates and 10～65 parts mixed, after adding long aliphatic chain monomer, initiator, polyether sulfonate and macromolecular coupling agent and handling, in twin screw extruder, make the pre-dispersed masterbatch of mixed calcium carbonate earlier with 5～80 parts of polyolefin resines, mix with the agent of even hole, oxidation inhibitor, antibacterial matrices and polyolefin resin again, obtain antimicrobial air permeable polyolefin film special material behind the extruding pelletization.The air-permeable envelope pore made from this material is easy, the aperture is even, anti-microbial property is good.This patent focuses on to air-permeable envelope provides anti-microbial property, though in system, introduced the part nano-calcium carbonate, the mechanical property of film is improved, but surface-treated strong owing to what filler was carried out, need to add a certain amount of amido silicon oil as sparing the hole agent.The adding of amido silicon oil forms die head smog at film-forming process easily, and and then form die head oil droplet and incrustation, thereby cause film surface longitudinal stripe to occur and oil droplet pollutes.In addition, earlier nano-calcium carbonate and water-ground limestone are made master batch again with other components through the twin screw extruder granulation, though help the dispersion of filler, operation is numerous and diverse, the tooling cost height.
Though above patent consciously or unconsciously improving the mechanical property of air-permeable envelope, all many-side such as the selection of nanometer inorganic filler, matrix resin, surface treatment mode are not integrated the mechanical property of raising air-permeable envelope.Market presses for high-intensity polyolefin permeable membrane to the lightweight requirements that air-permeable envelope proposed.
Summary of the invention
The objective of the invention is to overcome the deficiency that prior art exists, a kind of mixture that is used to prepare high-strength polyolefin permeable membrane is provided.
Another object of the present invention provides the preparation method of above-mentioned mixture.
To achieve these goals, the present invention adopts following technical scheme:
A kind of mixture that is used to prepare high-strength polyolefin permeable membrane, form by the component of following parts by weight:
Polyolefin resin 35～65
Micron order mineral filler 30～60
Nano grade inorganic filler 1～10
Oxidation inhibitor 0.2～0.5
Processing aid 0.1～1.0
Coupling agent 0.1～3.0.
In above-mentioned mixture, described polyolefin resin is preferably one or more the mixture in new LDPE (film grade), linear low density polyethylene, high density polyethylene(HDPE), copolymer from ethylene and propylene, ethene and butylene copolymer, ethene and hexene copolymer, ethene and octene copolymer, the polypropylene.
In above-mentioned mixture, described micron order mineral filler is preferably one or more the mixture in water-ground limestone, light calcium carbonate, barium sulfate, talcum powder, titanium dioxide, wollastonite, calcium sulfate, silicon-dioxide, the calcium oxide, and its grain size is 0.5 micron～20 microns.
In above-mentioned mixture, described nano grade inorganic filler is preferably one or more the mixture in water-ground limestone, light calcium carbonate, barium sulfate, talcum powder, titanium dioxide, wollastonite, calcium sulfate, silicon-dioxide, the calcium oxide, and its grain size is 50 nanometers～100 nanometers.
In above-mentioned mixture, described oxidation inhibitor is preferably Hinered phenols antioxidant as four-[β-(3,2-di-t-butyl-4 monohydroxy phenyl) propionic acid] pentaerythritol ester (trade(brand)name 1010) and phosphite ester kind antioxidant be as one or both the compound in (2, the 4-di-tert-butyl-phenyl) tris phosphites (trade(brand)name 168).
In above-mentioned mixture, described processing aid is preferably one or more the compound in PE wax, E wax, fluoropolymer additive, rare earth class lubricant, ethylene bis stearamide (EBS), erucicamide, amine hydroxybenzene, the Sorbic Acid acid amides.
In above-mentioned mixture, described coupling agent is preferably one or more the mixture in stearic acid, Zinic stearas, calcium stearate, Magnesium Stearate, stearic acid lanthanum, titanate coupling agent, aluminate coupling agent, the silane coupling agent.
The preparation method of above-mentioned mixture comprises the steps:
(1) obtains pretreated filler with micron order mineral filler, nano grade inorganic filler and after coupling agent mixes in high-speed mixer;
(2) gained pretreated filler and polyolefin resin, oxidation inhibitor, processing aid are dropped into mix in the mixing machine after, obtain mixture;
(3) mixture that obtains is put into extrude in the twin screw extruder after, after tank cooling, pelletizing, drying, vacuumize with aluminium foil bag and to pack.
With the moulding of above-mentioned mixture curtain coating, can obtain high-strength polyolefin permeable membrane, the draw ratio of film is preferably 1.5～2.0 during moulding.
Compared with prior art, the present invention has following beneficial effect:
The present invention can satisfy under the situation of service requirements by the mechanical property of rational polyolefin resin selection and nanometer inorganic filler raising polyolefin permeable membrane, and the thickness of air-permeable envelope is reduced.And by rational surface treatment, adopt economic operational path, make the enhancement that to give full play to Nano filling, can obtain the air-permeable envelope that even aperture distribution, water pressure resistance reach 100cm again, its transverse tensile strength is greater than 15MPa, and longitudinal tensile strength is greater than 30MPa.Water pressure resistance test reaches the 100cm water column, and promptly film can bear the 100cm water column and permeable, situation such as break does not take place.
Embodiment
Embodiment 1
In the fast mixing machine of 500 risings, press the prescription of table 1 embodiment 1, under stirring at low speed, add 50 kilograms of water-ground limestones (1.0 microns of median sizes) successively, 0.5 kilogram Zinic stearas, 1 kilogram of nano imvite, 0.2 kilogram titanate coupling agent, the temperature of charge of commentaries on classics high speed in high-speed mixer reaches 100 ℃ is changeed low speed again, add 5 kilograms of new LDPE (film grade)s (melt flow rate (MFR) is 12g/10min) again, the multipolymer of 40 kg ethylene and octene (C8) (melt flow rate (MFR) is 3g/10min), 0.2 kilogram antioxidant 1010,0.2 kilogram oxidation inhibitor 168,0.2 the kilogram erucicamide, 0.1 kilogram of fluoropolymer additive (trade mark FX-9613); More than after all materials add, changeed high-speed mixing 5 minutes; The material that mixes is put into twin screw extruder (75A type; length-to-diameter ratio 48: 1) in; extruder temperature is set at 220 ℃; engine speed is 250rpm, and the feeding rotating speed is 50rpm, after material is extruded; after tie rod cools off through tank; use the dicing machine granulation, use packaging of aluminium foil bag after drying, obtain high strength air-permeable envelope PP Pipe Compound AT-1#.
The performance of the high-strength polyolefin permeable membrane that high strength air-permeable envelope PP Pipe Compound AT-1# obtains after casting film-forming and stretching is as shown in table 2.
Embodiment 2
In the fast mixing machine of 500 risings, press the prescription of table 1 embodiment 2, under stirring at low speed, add 50 kilograms of water-ground limestones (1.0 microns of median sizes), 0.5 kilogram of Zinic stearas, 2 kilograms of nano-calcium carbonates, 0.2 kilogram of titanate coupling agent successively; The temperature of charge of commentaries on classics high speed in high-speed mixer reaches 100 ℃ is changeed low speed again; Add 5 kilograms of new LDPE (film grade)s (melt flow rate (MFR) is 12g/10min) again, the multipolymer of 35 kg ethylene and octene (C8) (melt flow rate (MFR) is 3g/10min), 5 kg polypropylene (melt flow rate (MFR) is 3g/10min), 0.2 kilogram antioxidant 1010,0.2 kilogram EBS, 0.1 kilogram of fluoropolymer additive (trade mark FX-9613); More than after all materials add, changeed high-speed mixing 5 minutes; The material that mixes is put into twin screw extruder (75A type; length-to-diameter ratio 48: 1) in; extruder temperature is set at 220 ℃; engine speed is 250rpm, and the feeding rotating speed is 50rpm, after material is extruded; after tie rod cools off through tank; use the dicing machine granulation, use packaging of aluminium foil bag after drying, obtain high strength air-permeable envelope PP Pipe Compound AT-2#.
The performance of the high-strength polyolefin permeable membrane that high strength air-permeable envelope PP Pipe Compound AT-2# obtains after casting film-forming and stretching is as shown in table 2.
Embodiment 3
In the fast mixing machine of 500 risings, press the prescription of table 1 embodiment 3, under stirring at low speed, add 50 kilograms of water-ground limestones (median size 100 nanometers), 0.5 kilogram of Zinic stearas, 1 kilogram of nano imvite, 1 kilogram of nano-calcium carbonate, 0.2 kilogram of aluminate coupling agent successively; The temperature of charge of commentaries on classics high speed in high-speed mixer reaches 100 ℃ is changeed low speed again; Add 5 kilograms of new LDPE (film grade)s (melt flow rate (MFR) is 2g/10min) again, the multipolymer of 30 kg ethylene and hexene (C6) (melt flow rate (MFR) is 4.5g/10min), 10 kilograms of high density polyethylene(HDPE)s (melt flow rate (MFR) is 1g/10min), 0.2 kilogram antioxidant 1010,0.2 kilogram oxidation inhibitor 168,0.2 the kilogram erucicamide, 0.1 kilogram of fluoropolymer additive (trade mark FX-9613); More than after all materials add, changeed high-speed mixing 5 minutes; The material that mixes is put into twin screw extruder (75A type; length-to-diameter ratio 48: 1) in; extruder temperature is set at 220 ℃; engine speed is 250rpm, and the feeding rotating speed is 50rpm, after material is extruded; after tie rod cools off through tank; use the dicing machine granulation, use packaging of aluminium foil bag after drying, obtain high strength air-permeable envelope PP Pipe Compound AT-3#.
The performance of the high-strength polyolefin permeable membrane that high strength air-permeable envelope PP Pipe Compound AT-3# obtains after casting film-forming and stretching is as shown in table 2.
Embodiment 4
In the fast mixing machine of 500 risings, press the prescription of table 1 embodiment 4, under stirring at low speed, add 50 kilograms of water-ground limestones (1.0 microns of median sizes), 1 kilogram of calcium oxide (1.0 microns of median sizes), 0.5 kilogram of stearic acid lanthanum, 1 kilogram of nano imvite, 0.5 kilogram of nano silicon, 0.2 kilogram of carboxylic acid rare-earth type coupling agent successively; The temperature of charge of commentaries on classics high speed in high-speed mixer reaches 100 ℃ is changeed low speed again; Add 5 kilograms of high density polyethylene(HDPE)s (melt flow rate (MFR) is 1g/10min) again, the multipolymer of 55 kg ethylene and octene (C8) (melt flow rate (MFR) is 3g/10min), 0.2 kilogram antioxidant 1010,0.2 kilogram oxidation inhibitor 168,0.1 kilogram erucicamide, 0.1 kilogram EBS, 0.1 kilogram of fluoropolymer additive (trade mark FX-9613); More than after all materials add, changeed high-speed mixing 5 minutes; The material that mixes is put into twin screw extruder (75A type; length-to-diameter ratio 48: 1) in; extruder temperature is set at 220 ℃; engine speed is 250rpm, and the feeding rotating speed is 50rpm, after material is extruded; after tie rod cools off through tank; use the dicing machine granulation, use packaging of aluminium foil bag after drying, obtain high strength air-permeable envelope PP Pipe Compound AT-4#.
The performance of the high-strength polyolefin permeable membrane that high strength air-permeable envelope PP Pipe Compound AT-4# obtains after casting film-forming and stretching is as shown in table 2.
The prescription of table 1 embodiment 1～4 (unit: kilogram)
| Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | |
| Water-ground limestone | ??50 | ??50 | ??50 | ??50 |
| Calcium oxide | ??1 |
| Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | |
| Nano-calcium carbonate | ??2 | ??1 | ||
| Nano imvite | ??1 | ??1 | ??1 | |
| Nano silicon | ??0.5 | |||
| Zinic stearas | ??0.5 | ??0.5 | ??0.5 | |
| The stearic acid lanthanum | ??0.5 | |||
| Titanate coupling agent | ??0.2 | ??0.2 | ||
| Aluminate coupling agent | ??0.2 | |||
| Carboxylic acid rare-earth type coupling agent | ??0.2 | |||
| Erucicamide | ??0.2 | ??0.2 | ??0.1 | |
| ??EBS | ??0.2 | ??0.1 | ||
| Fluoropolymer additive | ??0.1 | ??0.1 | ??0.1 | ??0.1 |
| New LDPE (film grade) | ??5 | ??5 | ??5 | |
| The multipolymer of ethene and octene | ??40 | ??35 | ??55 | |
| The multipolymer of ethene and hexene | ??30 | |||
| Polypropylene | ??5 | |||
| High density polyethylene(HDPE) | ??10 | ??5 | ||
| Antioxidant 1010 | ??0.2 | ??0.2 | ??0.2 | ??0.2 |
| Oxidation inhibitor 168 | ??0.2 | ??0.2 | ??0.2 |
Table 2 embodiment 1～4 resulting air-permeable envelope performance
| Project | Unit | ??AT-1# | ?AT-2# | ??AT-3# | ?AT-4# |
| Longitudinal tensile strength | ??MPa | ??30 | ??38 | ??40 | ??36 |
| The longitudinal fracture elongation | ??％ | ??250 | ??180 | ??220 | ??210 |
| Transverse tensile strength | ??MPa | ??18 | ??21 | ??22 | ??20 |
| The transverse breakage elongation | ??％ | ??550 | ??500 | ??550 | ??550 |
| Grammes per square metre | ??g/m 2 | ??20 | ??25 | ??15 | ??20 |
| Vapor transfer rate | ??g/m 2·24h | ??3500 | ??3300 | ??4500 | ??3500 |
| Water pressure resistance | ??cmH 2O | ??110 | ??105 | ??110 | ??120 |
Claims (10)
1. mixture that is used to prepare high-strength polyolefin permeable membrane is characterized in that being made up of the component of following parts by weight:
Polyolefin resin 35～65
Micron order mineral filler 30～60
Nano grade inorganic filler 1～10
Oxidation inhibitor 0.2～0.5
Processing aid 0.1～1.0
Coupling agent 0.1～3.0.
2. mixture according to claim 1, it is characterized in that described polyolefin resin is one or more the mixture in new LDPE (film grade), linear low density polyethylene, high density polyethylene(HDPE), copolymer from ethylene and propylene, ethene and butylene copolymer, ethene and hexene copolymer, ethene and octene copolymer, the polypropylene.
3. mixture according to claim 1, it is characterized in that, described micron order mineral filler is one or more the mixture in water-ground limestone, light calcium carbonate, barium sulfate, talcum powder, titanium dioxide, wollastonite, calcium sulfate, silicon-dioxide, the calcium oxide, and its grain size is 0.5 micron～20 microns.
4. mixture according to claim 1, it is characterized in that, described nano grade inorganic filler is one or more the mixture in water-ground limestone, light calcium carbonate, barium sulfate, talcum powder, titanium dioxide, wollastonite, calcium sulfate, silicon-dioxide, the calcium oxide, and its grain size is 50 nanometers～100 nanometers.
5. mixture according to claim 1 is characterized in that, described oxidation inhibitor is one or both the compound in Hinered phenols antioxidant and the phosphite ester kind antioxidant.
6. mixture according to claim 1, it is characterized in that described processing aid is one or more the compound in PE wax, E wax, fluoropolymer additive, rare earth class lubricant, ethylene bis stearamide, erucicamide, amine hydroxybenzene, the Sorbic Acid acid amides.
7. mixture according to claim 1, it is characterized in that described coupling agent is one or more the mixture in stearic acid, Zinic stearas, calcium stearate, Magnesium Stearate, stearic acid lanthanum, titanate coupling agent, aluminate coupling agent, the silane coupling agent.
8. the preparation method of the described mixture of claim 1 is characterized in that comprising the steps:
(1) obtains pretreated filler with micron order mineral filler, nano grade inorganic filler and after coupling agent mixes in high-speed mixer;
(2) gained pretreated filler and polyolefin resin, oxidation inhibitor, processing aid are dropped into mix in the mixing machine after, obtain mixture;
(3) mixture that obtains is put into extrude in the twin screw extruder after, after tank cooling, pelletizing, drying, vacuumize with aluminium foil bag and to pack.
9. a high-strength polyolefin permeable membrane is characterized in that by the moulding of the described mixture curtain coating of claim 1.
10. high-strength polyolefin permeable membrane as claimed in claim 9 is characterized in that, the draw ratio of film is 1.5～2.0 during moulding.
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-
2008
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