CN100572035C - The preparation method of a kind of polytetrafluoroethylmulti multi-layer composite film and protective materials thereof - Google Patents
The preparation method of a kind of polytetrafluoroethylmulti multi-layer composite film and protective materials thereof Download PDFInfo
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- CN100572035C CN100572035C CNB2006101459941A CN200610145994A CN100572035C CN 100572035 C CN100572035 C CN 100572035C CN B2006101459941 A CNB2006101459941 A CN B2006101459941A CN 200610145994 A CN200610145994 A CN 200610145994A CN 100572035 C CN100572035 C CN 100572035C
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Abstract
The present invention relates to the preparation method of a kind of polytetrafluoroethylmulti multi-layer composite film and protective materials thereof, this method adopts polytetrafluoroethylene (PTFE) base band and thermoplasticity moisture-permeable film to carry out common longitudinal stretching under 100～220 ℃ temperature, then under 50～300 ℃ temperature, on expander, carry out cross directional stretch, finalize the design at 200～400 ℃ sintering temperature at last, be prepared into laminated film, adopt the lamination mode to be prepared into protective materials by adhesive prepared laminated film and woven cloth, looped fabric or non-weaving cloth.The saturating vapour amount of this material reaches 3000～12000 grams/square metres 24 hours, 50～220 kPas of water pressure resistances, and the filter efficiency of microorganism 〉=99% in the air, filter efficiency 〉=99% of microorganism such as poliovirus in the liquid, repeatedly washing back performance does not descend.This material can be widely used as materials such as biochemical protection, Waterproof Breathable, wind-proof warming.
Description
Technical field
The present invention relates to the preparation method of a kind of polytetrafluoroethylmulti multi-layer composite film and protective materials thereof.
Background technology
In the prior art, the existing multinomial patent of the made protective fabric of microporous teflon membran, although have waterproofing and moisture-penetration performances preferably, barrier propterty such as its waterproof can descend significantly in washing process, has directly influenced result of use.In recent years, although the polytetrafluoroethylcomposite composite film of being invented solves to some extent to this problem, complex process often, cost is higher, and vapor transfer rate all has bigger decline simultaneously, has influenced snugness of fit.
In the past, biochemical protective garment mainly adopted isolation type, and its principle is that contaminated air or toxic agent drop and human body skin air is isolated, to reach the purpose of gas defence.The material that adopts mainly is a butyl rubber, the complete steam-proof of this material, and the sweat on the skin can not evaporate, and has a strong impact on human-body radiating, causes the part soldier because of the death of suffering heatstroke.Under the weather conditions of sweltering heat, this clothes generally can only be worn 10 minutes, and in vigorous health can not surpass half an hour.Saturating vapour formula protective garment is that the fifties is taken the lead in developing by the U.S. latter stage, the fabric that it adopts chloramines dipping is equipped on non-chemical defence specialized force, and it has overcome the shortcoming of butyl rubber protective garment, steam permeability and good heat dispersion performance, but have following drawback: the one, chloramines has selectivity to the absorption of toxic agent; The 2nd, chloramines has spread effect to skin; The 3rd, chloramines corrosion fabric has shortened clothes service life.A large amount of active carbon particle or activated carbon fibers of adopting in the saturating vapour formula protective garment utilize its strong absorption property to reach biochemical purpose of protecting, but shortcoming are to use the life-span short, the regeneration difficulty.Therefore, the focus studied in recent years of western developed country is to be that material of main part is developed vapour formula protective materials with the differential permeability composite membrane.
Under this background, the inventor provides a kind of have barrier propterty and the polytetrafluoroethylmulti multi-layer composite film of saturating wet effect and the preparation method of protective materials thereof, and this protective materials is applicable to fields such as Waterproof Breathable, wind-proof warming, biochemical protective clothes, easy suit and shoes and hats.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of polytetrafluoroethylmulti multi-layer composite film, this method is carried out common longitudinal stretching with polytetrafluoroethylene (PTFE) degreasing base band and thermoplasticity moisture-permeable film under 80～300 ℃ of temperature, under 50～300 ℃ of temperature, on expander, carry out cross directional stretch then, 200～400 ℃ of sintering temperature typings, prepare multilayer complex films again.
The preparation method of polytetrafluoroethylmulti multi-layer composite film provided by the invention comprises the steps:
(1) expanded PTFE toner, fluid lubricant are fully mixed, after placing, form the polytetrafluoroethylene (PTFE) compound;
Its part by weight is: 1～20 part of expanded PTFE toner, 0.2～0.6 part of fluid lubricant;
Adopt preferably that degree of crystallinity is 98～99.9%, molecular weight is 2,000,000～1,000 ten thousand expanded PTFE toner;
Described fluid lubricant is atoleine, benzinum or kerosene.
(2) above-mentioned polytetrafluoroethylene (PTFE) compound is pressed into cylindrical blank, again this blank is extruded club by the pushing machine, then this club is rolled into the polytetrafluoroethylene (PTFE) base band;
(3) with above-mentioned polytetrafluoroethylene (PTFE) base band at 100～300 ℃ of following longitudinal stretchings, be processed into the degreasing base band;
(4) with above-mentioned degreasing base band and thermoplasticity moisture-permeable film at 80～250 ℃ of following longitudinal stretchings, be processed into composite baseband.
Described thermoplasticity moisture-permeable film is any one in moisture permeability polyethylene, polypropylene, polyester or the polyurethane, 10～100 microns of its thickness, with moisture permeability for well.Composite baseband is two-layer composite baseband or two-layer above composite baseband, preferably polytetrafluoroethylene-three layers of composite baseband of thermoplasticity moisture-permeable film-polytetrafluoroethylene (PTFE).
(5) with above-mentioned composite baseband at 50～300 ℃ of following cross directional stretch, 200-400 ℃ of following sintering typing, sintering time is 10 seconds～1 minute, obtains polytetrafluoroethylmulti multi-layer composite film then.
Preferred sintering temperature is 200～380 ℃.
Another object of the present invention is to provide a kind of preparation method of protective materials of the polytetrafluoroethylmulti multi-layer composite film that contains method for preparing, this method is to adopt the lamination mode to be prepared into protective materials by adhesive the multilayer complex films of method for preparing and woven cloth, looped fabric or non-weaving cloth.This protective materials has durable water resistant, windproof, anti-biochemical, saturating multiple performance such as wet, is applicable to fields such as Waterproof Breathable, wind-proof warming, biochemical protective clothes, easy suit and shoes and hats.
The preparation method of the protective materials of a kind of polytetrafluoroethylmulti multi-layer composite film that contains method for preparing provided by the invention comprises the steps:
(1) expanded PTFE toner, fluid lubricant are fully mixed, after placing, form the polytetrafluoroethylene (PTFE) compound;
Its part by weight is: 1～20 part of expanded PTFE toner, 0.2～0.6 part of fluid lubricant;
Adopt preferably that degree of crystallinity is 98～99.9%, molecular weight is 2,000,000～1,000 ten thousand expanded PTFE toner;
Described fluid lubricant is atoleine, benzinum or kerosene.
(2) above-mentioned polytetrafluoroethylene (PTFE) compound is pressed into cylindrical blank, again this blank is extruded club by the pushing machine, then this club is rolled into the polytetrafluoroethylene (PTFE) base band;
(3) with above-mentioned polytetrafluoroethylene (PTFE) base band at 100～300 ℃ of following longitudinal stretchings, be processed into the degreasing base band;
(4) with above-mentioned degreasing base band and thermoplasticity moisture-permeable film at 80～250 ℃ of following longitudinal stretchings, be processed into composite baseband;
Described thermoplasticity moisture-permeable film is any one in moisture permeability polyethylene, polypropylene, polyester or the polyurethane, 10～100 microns of its thickness, with moisture permeability for well.Composite baseband is two-layer composite baseband or two-layer above composite baseband, preferably polytetrafluoroethylene-three layers of composite baseband of thermoplasticity moisture-permeable film-polytetrafluoroethylene (PTFE).
(5) with above-mentioned composite baseband at 50～300 ℃ of following cross directional stretch, 200-400 ℃ of following sintering typing, sintering time is 10 seconds～1 minute, obtains polytetrafluoroethylmulti multi-layer composite film then;
Preferred sintering temperature is 200～380 ℃.
(6) adopt the lamination mode to be prepared into protective materials by adhesive above-mentioned polytetrafluoroethylmulti multi-layer composite film and fabric with multiple protection water vapour permeability.
Described fabric is any one in woven fabric, knitted fabric or the nonwoven.
Described adhesive is polyamide, organosilicon, ethene-ethyl acetate, polyester and/or polyurethane.
Described lamination mode is the combination of one or more modes in dusting, powder point, slurry point, two point, fusion glue point, crackle film, spraying and/or the blade coating.
Test the vapour amount according to GB/T12704-1991, FZ/T01004-1991 tests water pressure resistance, by microorganism barrier properties in the WSB58-2003 of the Ministry of Public Health of the General Logistics Department biological protection clothes general specification test air, by poliovirus barrier properties in the WSB58-2003 of the Ministry of Public Health of the General Logistics Department biological protection clothes general specification test liquid.The saturating vapour amount of prepared protective materials can reach 3000～12000 grams/square metres 24 hours, 50～220 kPas of water pressure resistances, the filter efficiency of microorganism 〉=99% in the air, filter efficiency 〉=99% of microorganism such as poliovirus in the liquid.Performance does not descend substantially after repeatedly washing.
The present invention compared with prior art has following advantage:
1. the inventive method technology is simple, cost is low, does not need Special Equipment can prepare polytetrafluoroethylmulti multi-layer composite film.
2. the polytetrafluoroethylmulti multi-layer composite film of using the method for the invention preparation can be widely used as the biochemical protective materials of permeability type, also can be used for fields such as wind-proof warming, water proof and moisture permeable material and easy suit, has remarkable economic efficiency and social benefit.
3. use the prepared protective materials of this polytetrafluoroethylmulti multi-layer composite film, have waterproof, windproof, anti-biochemical, warming, saturating multiple function such as wet, the while, these functions can not descend in washing process.
The specific embodiment
Below be specific embodiments of the invention, described embodiment is used to describe the present invention, rather than restriction the present invention.
[embodiment 1] preparation polytetrafluoroethylmulti multi-layer composite film
(1) 1 kilogram of expanded PTFE toner, atoleine are fully mixed for 0.5 kilogram, after placing, form the polytetrafluoroethylene (PTFE) compound;
(2) above-mentioned polytetrafluoroethylene (PTFE) compound is pressed into cylindrical blank, this blank is extruded club by the pushing machine, then this club is rolled into the polytetrafluoroethylene (PTFE) base band;
(3) with above-mentioned polytetrafluoroethylene (PTFE) base band at 180 ℃ of following longitudinal stretchings, be processed into the degreasing base band;
(4) with three layers of wet polyurethane films of above-mentioned degreasing base band/thoroughly/described degreasing base band at 100 ℃ of following longitudinal stretchings, be processed into sandwich composite baseband, the used thickness that wets polyurethane film is 12 microns;
(5) with above-mentioned sandwich base band at 120 ℃ of following cross directional stretch, 250 ℃ of following sintering typings, the time is 40 seconds, obtains the sandwich laminated film then.
Embodiment 2,3,4,5 is identical with embodiment 1 with the step of embodiment 6 preparation polytetrafluoroethylmulti multi-layer laminated films, and just the technological parameter in each step is seen attached list with raw materials used slightly different.
Subordinate list:
[embodiment 7] preparation contains the protective materials of the polytetrafluoroethylmulti multi-layer composite film of method for preparing
Adopt powder point method that polyester binder is transferred on the lining, embodiment 1 prepared laminated film is passed through pressure roller with the terylene woven fabric, 170 ℃ of roller surface temperature are prepared into vapour formula protective materials.
Detect according to the method for GB/T12704-1991, FZ/T01004-1991 and WSB58-2003 general specification protective materials the polytetrafluoroethylmulti multi-layer composite film of method for preparing, its saturating vapour amount reaches 7800 grams/square metres 24 hours, 190 kPas of water pressure resistances, the filter efficiency of microorganism 〉=99% in the air, filter efficiency 〉=99% of microorganism such as poliovirus in the liquid.The above-mentioned material performance does not descend substantially after 20 washings.
[embodiment 8] preparation contains the protective materials of the polytetrafluoroethylmulti multi-layer composite film of method for preparing
Adopt slurry point method that polyurethane binder is transferred on the lining, embodiment 2 prepared laminated films are passed through pressure roller with the terylene woven fabric, 160 ℃ of roller surface temperature are prepared into vapour formula protective materials.
Detect according to the method for GB/T12704-1991, FZ/T01004-1991 and WSB58-2003 general specification protective materials the polytetrafluoroethylmulti multi-layer composite film of method for preparing, its saturating vapour amount reaches 6000 grams/square metres 24 hours, 200 kPas of water pressure resistances, the filter efficiency of microorganism 〉=99% in the air, filter efficiency 〉=99% of microorganism such as poliovirus in the liquid.The above-mentioned material performance does not descend substantially after 20 washings.
[embodiment 9] preparation contains the protective materials of the polytetrafluoroethylmulti multi-layer composite film of method for preparing
Adopt knife coating that polyurethane binder is transferred on the lining, embodiment 3 prepared laminated films are passed through pressure roller with the terylene woven fabric, 160 ℃ of roller surface temperature are prepared into vapour formula protective materials.
Detect according to the method for GB/T12704-1991, FZ/T01004-1991 and WSB58-2003 general specification protective materials the polytetrafluoroethylmulti multi-layer composite film of method for preparing, its saturating vapour amount reaches 5000 grams/square metres 24 hours, 120 kPas of water pressure resistances, the filter efficiency of microorganism 〉=99% in the air, filter efficiency 〉=99% of microorganism such as poliovirus in the liquid, the above-mentioned material performance does not descend substantially after 15 washings.
Claims (9)
1, a kind of preparation method of polytetrafluoroethylmulti multi-layer composite film is characterized in that this method comprises the steps:
1) expanded PTFE toner 1-20 weight portion, fluid lubricant 0.2-0.6 weight portion are mixed, place the back and form the polytetrafluoroethylene (PTFE) compound;
2) above-mentioned polytetrafluoroethylene (PTFE) compound is pressed into cylindrical blank, this blank is extruded club by the pushing machine, then this club is rolled into the polytetrafluoroethylene (PTFE) base band;
3) with above-mentioned polytetrafluoroethylene (PTFE) base band at 100-300 ℃ of following longitudinal stretching, be processed into the degreasing base band;
4) with above-mentioned degreasing base band and thermoplasticity moisture-permeable film at 80～250 ℃ of following longitudinal stretchings, be processed into composite baseband; Described thermoplasticity moisture-permeable film is polyethylene film, polypropylene film, polyester film or polyurethane film, and its thickness is 10～100 microns;
5) with above-mentioned composite baseband at 50～300 ℃ of following cross directional stretch, 200～400 ℃ of following sintering typings, sintering time 10 seconds～60 seconds obtains laminated film then.
2, the preparation method of a kind of polytetrafluoroethylmulti multi-layer composite film according to claim 1 is characterized in that: the degree of crystallinity of described expanded PTFE toner is 98～99.9%, molecular weight is 2,000,000～10,000,000.
3, the preparation method of a kind of polytetrafluoroethylmulti multi-layer composite film according to claim 1 is characterized in that: described composite baseband is two-layer composite baseband or two-layer above composite baseband.
4, the preparation method of a kind of polytetrafluoroethylmulti multi-layer composite film according to claim 3 is characterized in that: described composite baseband is polytetrafluoroethylene (PTFE)-three layers of composite baseband of thermoplasticity moisture-permeable film-polytetrafluoroethylene (PTFE).
5, a kind of preparation method who contains the protective materials of the described polytetrafluoroethylmulti multi-layer composite film of claim 1 is characterized in that this method comprises the steps:
1) expanded PTFE toner 1-20 weight portion, fluid lubricant 0.2-0.6 weight portion are mixed, place the back and form the polytetrafluoroethylene (PTFE) compound;
2) above-mentioned polytetrafluoroethylene (PTFE) compound is pressed into cylindrical blank, this blank is extruded club by the pushing machine, then this club is rolled into the polytetrafluoroethylene (PTFE) base band;
3) with above-mentioned polytetrafluoroethylene (PTFE) base band at 100-300 ℃ of following longitudinal stretching, be processed into the degreasing base band;
4) with above-mentioned degreasing base band and thermoplasticity moisture-permeable film at 80～250 ℃ of following longitudinal stretchings, be processed into composite baseband;
5) with above-mentioned composite baseband at 50～300 ℃ of following cross directional stretch, 200～400 ℃ of following sintering typings, sintering time 10 seconds～60 seconds obtains laminated film then;
6) adopt the lamination mode to be prepared into protective materials by adhesive above-mentioned laminated film and fabric.
6, a kind of preparation method who contains the protective materials of the described polytetrafluoroethylmulti multi-layer composite film of claim 1 according to claim 5 is characterized in that: the degree of crystallinity of described expanded PTFE toner is 98～99.9%, molecular weight is 2,000,000～10,000,000.
7, a kind of preparation method who contains the protective materials of the described polytetrafluoroethylmulti multi-layer composite film of claim 1 according to claim 5, it is characterized in that: the thermoplasticity moisture-permeable film described in the step 4) is a kind of in polyethylene film, polypropylene film, polyester film or the polyurethane film, and its thickness is 10～100 microns.
8, a kind of preparation method who contains the protective materials of the described polytetrafluoroethylmulti multi-layer composite film of claim 1 according to claim 7 is characterized in that: described composite baseband is two-layer composite baseband or two-layer above composite baseband.
9, a kind of preparation method who contains the protective materials of the described polytetrafluoroethylmulti multi-layer composite film of claim 1 according to claim 8 is characterized in that: described composite baseband is polytetrafluoroethylene (PTFE)-three layers of composite baseband of thermoplasticity moisture-permeable film-polytetrafluoroethylene (PTFE).
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