CN1054108A - Improved waterproofing of polyester fiberfill - Google Patents
Improved waterproofing of polyester fiberfill Download PDFInfo
- Publication number
- CN1054108A CN1054108A CN90110425A CN90110425A CN1054108A CN 1054108 A CN1054108 A CN 1054108A CN 90110425 A CN90110425 A CN 90110425A CN 90110425 A CN90110425 A CN 90110425A CN 1054108 A CN1054108 A CN 1054108A
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- China
- Prior art keywords
- elastomeric material
- fiberfill fibers
- ester
- ester units
- gluing
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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Classifications
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M15/507—Polyesters
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Laminated Bodies (AREA)
- Nonwoven Fabrics (AREA)
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
- Multicomponent Fibers (AREA)
- Polyesters Or Polycarbonates (AREA)
Abstract
The hydrophilic polymerized ether-ether film of a kind of waterproof has high steam transmitance, can be fixed on well on the polyester fiberfill fibers wadding tire, thereby make easily, when said composition is used for clothes, wears more comfortable.
Description
The application is by the subsequent application of Frankosky in 07/449, No. 615 unexamined patent of proposition on December 12nd, 1989.
The present invention relates to improvement, be particularly useful for clothes with the polyester fiberfill fibers of waterproof coating.
Polyester fiberfill fibers (being sometimes referred to as the polyester fiber packing material) is as a kind of low-cost filler and/or insulation material, generally accepted by people, a large amount of production, and be used for pillow, mat and other ornament materials (comprising bedding), and clothes.Because select the polyester fiberfill fibers more more economical effectively than eider down or feather heat-insulation layer, and good water-proof effect, so be used for commercially producing of many clothes manufactured goods.Yet people wish that clothes can waterproof, and as in the rainy day of cold, permeable clothes can make the people uncomfortable.Purpose of the present invention that Here it is.
Common waterproof has stoped sweat to ooze out from clothes, and this is not a solution.Because the sweat that goes out finally can form sweat stream, make the people very uncomfortable.Now, various forms of cover layers (comprising film) are arranged, be improved to steam is seen through, liquid then can not see through.Generally, this film has been used for or attached to being used for making " waterproof/ventilative " clothes on the fabric.In fact, this clothes are connected or adhere to the place at fabric with film need carry out special stitching, as sleeve and pocket place.This special stitching cost height is restricted in the design, also influences (for example to as thin as a wafer fabric) attractive in appearance.At present, waterproof/breathable films adheres to as lining with scrim, and this improvement has enlarged scope of design, has reduced the stitching amount, still, in order gluing together with scrim, need to pass through particular processing when making film, and to need substep attached on the scrim.
In order to improve the aesthetic of polyester fiberfill fibers; preferably to fiberfill fibers " gluing "; be coated with one deck protective surface (for example washable face), silicone normally, the i.e. polysiloxanes that solidifies of one deck; as be disclosed in the United States Patent (USP) 3 of Hofmann; 271,189; people's such as Mead United States Patent (USP) 3,454; 422; the United States Patent (USP) 3 of Ryan; 488,217; people's such as Salamon United States Patent (USP) 4,146; 674; the United States Patent (USP) 4 of Pamm; 281,042; the United States Patent (USP) 4,304 of Frankosky; 817; and the Japan Patent 58-214 of Takemoto grease Co., Ltd, 585(1983).In these lists of references, being discussed (as Pamm and Frankosky), obtain to have serious problem aspect the better bonding effect at gluing face always.
When the polyester fiberfill fibers with this polyester fiberfill fibers, particularly gluing was filled in clothes or other goods, to the problems referred to above that the water-proof polyester fiberfill fibers exists, people wished to find a kind of effective solution to overcome described shortcoming always.
Another problem that exists, at United States Patent (USP) 4,869,771 is described as LeVan, and the polyester fiberfill fibers spills from the outer cover of fabric; This piece patent is also mentioned the problem of materials that adheres to the polyester fiberfill fibers in addition.
According to the present invention, we have invented a kind of special copolyether ester elastic film now, and it is hydrophilic, can be fixed on the polyester fiberfill fibers of gluing, for example with the wadding tire form.Other advantage will be described below.
One aspect of the present invention provides a kind of polyester fiberfill fibers wadding tire, or a kind of clothes or other goods that are filled with the polyester fiberfill fibers.Wherein the polyester fiberfill fibers is to be fixed on a kind of continuous soft layer of waterproof hydrophilic elastic material, and this layer has the steam transmitance and is at least 3500gm.mil/m
2/ 24 hours, according to ASTME96-66(program BW) described, this hydrophilic elastomeric material is the mixture of a kind of copolyether ester elastomeric material or two or more copolyether ester elastomeric material, have a large amount of long-chain ester units and short-chain ester units, join end to end by ester linkage, described long-chain ester units is represented with following formula:
Described short-chain ester units is represented with following formula:
Here, G is the divalent group after terminal hydroxyl is removed from poly-alkylene oxyethanol (mean molecule quantity is 400-3500).Then, add ethylene oxide group by poly-alkylene oxygen glycol in the mixture of copolyether ester or two or more copolyether ester, the amount of ethylene oxide of adding is about 25-68%(weight with respect to two or more the total amount of mixture of copolyether ester or its); R is the divalent group after carboxyl is removed from dicarboxylic acids (molecular weight is less than 300); D is the divalent group after hydroxyl is removed from glycol (molecular weight is less than 250).Two or more mixture of described copolymerized ether ester of hydrophile or its has about 25-80%(weight) short-chain ester units.
Advantage is, if necessary, fiberfill fibers is fixed on the pantostrat of hydrophilic elastic material by a kind of hydrophobic elastomeric material insert layer, and the hydrophobic elastomeric material has steam transmitance 400-2500gm.mil/m
2/ 24 hours, be preferably 800-1200gm.mil/m
2Described hydrophobic elastomeric material was a kind of copolyether ester in/24 hours, and it has the long-chain ester units and the short-chain ester units of many repetitions, and described long-chain ester units is expressed from the next:
Described short-chain ester units is expressed from the next:
Wherein G is one and removes the substituting group of divalence behind the terminal hydroxyl from poly-alkylene oxygen glycol (the about 400-3500 of the mean molecule quantity that has), is not more than 20 percentage by weights by gathering alkylene oxygen glycol adds oxirane in copolyether ester amount; R is from having molecular weight less than a divalent substituent of removing 300 the dicarboxylic acids behind the carbonyl; D is from having molecular weight less than the divalent group of removing 250 the glycol behind the hydroxyl; Described hydrophobic elastomeric material preferably has about 25-80 percentage by weight short-chain ester units.Fiberfill fibers can glue by point easily or other discontinuous mode combines with the hydrophobic elastomeric material off and on, preferably uses to have low-melting binder fiber.
Being appreciated that above-mentioned elastomeric material may be single copolyether ester elastomeric material, also may be the mixture of two or more copolyether ester elastomeric material if desired.
Another aspect of the present invention is that fexible film is made up of more than one elastomeric layer.One deck is hydrophilic elastomeric material, as above-mentioned.The second layer may be combined with each other with ground floor, it also may be the hydrophobic elastomeric material, for example a kind of copolyether ester, it contains 1 of 20.3 percentage by weights, the 4-butylene terephthalate, 1 of 7.9 percentage by weights, 4-M-phthalic acid fourth diester, 51.7 the poly-butyl ether isophthalic acid ester of percentage by weight and poly terephthalic acid fourth two ether-ethers of 20.1 percentage by weights, wherein used polytetramethylene glycol fourth diether ester molecule amount is 2000.Second layer hydrophobicity is better, and lower fusing point is arranged so that bonding.
The best gluing of polyester fiberfill fibers.The density range of wadding tire etc. is preferably in 0.5-1 pound/cubic feet (about 0.008-0.016gm/cm
3), density also can reach 1.5 or 2 pounds/cubic feet (about 0.025 or 0.03gm/cm
3).Waterproof fiberfill fibers composition has good performance, and it can avoid in use for some time (as running into) when clothes are worn, because stretching and bending and the phenomenon of layering.
Others of the present invention and advantage will be described below.
The present invention attempts to make the fibrefill of above-mentioned gluing to have special purposes, all disclosed files at this all as a reference, the United States Patent (USP) 4,304 of Frankosky particularly, the mixture described in 817.
Hydrophilic polymerized preferably ether-ether elastomeric material is those (special United States Patent (USP)s 4 at Ostapchenko, 725, described in 481) the hydrophilic elastic material, prior art has been done improvement, people's such as Vrouenraets United States Patent (USP) 4 for example, on October 1st, 493,870 and 1976, disclosed Japanese patent application 50-35623 wherein disclosed not really desirable copolyether ester.In fact, need make this copolyether ester membrane firm by adhering technique as described herein it is believed that, this be because also do not find other method at present.We find, when this film directly is pressed on the fabric (for example a kind of nonwoven scrim of polyethylene terephthalate fiber), not composition bonding very ineffective, stretching in the use and bending can produce local delamination afterwards, promptly the bonding part branch between film and fabric is destroyed, therefore, the globality of this composition on the whole interface between fabric and the film just do not existed.And polyester fiber filling wadding tire of the present invention can combine better with this copolyether ester membrane integral body, and the fastness of its interlayer combination is more stable, can stretch repeatedly in actual applications and bend.A kind of suitable polyester fiber is filled the wadding tire and is preferably had low density, be approximately 0.5-1 pound/cubic feet, but density also can be about 1.5, or even 2 pounds/cubic feet (be equivalent to about 0.008 to 0.016, arrive about 0.025, or even about 0.03gm/cm
3).Fiber filled wadding tire does not resemble most of fabrics close, even not as good as close (a kind of nonwoven light weight scrim fabric of nonwoven light weight scrim with the spunbond one-tenth of polyethylene terephthalate, for example in the patent 4 of Ostapcheko, 725, use in 481 examples 1, be about 7-7.5 pound/cubic feet, just about 0.12gm/cm
3), it and film have less contact point.People may expect that these differences may be the main causes of the unexpected effect that produces in the reality, but the present invention does not want to be subjected to the limitation of any theory.
Composition of the present invention provides a kind of dress materials, and this material will be incubated with anti-liquid (water) layer that only allows steam to see through and combine.Best material is answered existing certain intensity, and is simultaneously attractive in appearance again.This material can be as required at an easy rate by sticking film of hot glue and wadding tire are pressed together, or the technology manufacturing by the above-mentioned fabrics gummed.When prefabricated film adhesive is incorporated on the wadding tire, use a kind of solvent cement (adhesive with LMP is better usually) possibly with the binder fiber form, adopt sticking or other technology that can avoid pantostrat and film to be bonded together of point.Material can be processed into clothes or other goods as required.A significant advantage compared with the prior art is that this new composition tool on stitching is handled has an enormous advantage.
The present invention describes by following embodiment.All parts and units of percent all are weight, except as otherwise noted.In each case, can both obtain satisfied bonding effect between wadding tire and waterproofing membrane.
Example 1
In example 1, (density is about 1 pound/cubic feet to 50 yards 3.0 ounce per square yard bonded batt tire samples, three bursts of blending of binder fiber by the drying of silicone gluing form) compound with a kind of copolyether ester elastic material membrane, when film has just been extruded by extruder die head slit, keep 229 ℃, mould outlet is opened about 10 mils, this copolyether ester elastomeric material comprises the mixture of 45% butylene terephthalate and 55%, contain 60% poly(ethylene oxide) (molecular weight 2000) terephthalate and 40% poly(ethylene oxide)/polyoxypropylene (molecular weight=2150, ethylene oxide content=25%) terephthalate in this mixture.The linear velocity of extruding is about 2 yards/minute, and when the take up roll rotating speed speeds 15 times (30 yards/minute), the film thickness that is covered on the wadding tire reduces to about 0.7 mil.First time contact with the wadding tire occurs on two roll gaps between the take up roll, and when following take up roll preheating wadding tire and be with the wadding tire contact with film, top pressure roller compresses film and the tire of wadding a quilt with cotton, and cools off film and make its curing.To 3.0 ounces wadding tire, keep 80 ℃ when the wadding tire around roller strap, and pressure roller/chill roll is when remaining 60 ℃, the bonding effect that can obtain to be fit to, to a large amount of wadding tires, its loss can be ignored.
Example 2
Conditions all in example 2 is all identical with example 1, and the tire weight of just wadding a quilt with cotton is 4.5 ounces, and the temperature of first pair of touch roll is also different, and what wearing the tire of wadding a quilt with cotton down is 93 ℃ around roller, and top pressure roller keeps 60 ℃.
Example 3
Film is that layering is manufactured in example 3, bilayer film by copolyether ester elastomeric material (A) and (B) co-extrusion pressure make.Wherein (A) contains the mixture of 45% butylene terephthalate and 55%, this mixture contains 60% poly(ethylene oxide) (molecular weight=2000) terephthalate and 40% poly(ethylene oxide)/polyoxypropylene (molecular weight=2150, ethylene oxide content=25%) terephthalate, (B) contain 20.3% 1, the 4-butylene terephthalate, 7.9% 1,4-M-phthalic acid fourth diester, 51.7% poly terephthalic acid fourth, two ether-ethers and 20.1% poly-M-phthalic acid fourth two ether-ethers, it is 2000 that wherein employed polytetramethylene glycol fourth two ether-ethers have molecular weight.The preparation co-extrusion film is to add copolyether ester (A) in a diameter is the extruder of 2.5 English inch (6.4 centimetres), in diameter is the extruder of 1.5 English inch (3.8 centimetres), add copolyether ester (B), enter after extruding that hybrid template and corresponding polymer solution are compound before extruding by slot die to be stratiform.The extruder of diameter 1.5 English inch keeps 215 ℃, and the extruder of diameter 2.5 English inch remains on 205 ℃.It is 10 mils (0.25 millimeters) that die head exit is opened, and die head temperature remains 215 ℃.Co-extrusion film with 18 yards (16.6 meters)/minute speed production, the final film thickness that obtains is 0.7 mil (0.018 millimeter).Keep the speed of extruder, the thickness that makes copolymer (A) is 0.6 mil, and copolymer (B) is 0.1 mil.
When substep is operated, 10 yards wadding tire samples as example 2 are put in the flat layer pressure device with bilayer film and nonwoven web fabric (this fabric is commercially available low-melting point polyester binder fiber), this device can heat above-mentioned material from top to bottom, by scribbling Teflon
(R)The endless conveyor Contact Heating of TFE fluorocarbon.Space between the conveyer belt should be adjusted with the tire of avoiding wadding a quilt with cotton and be compressed.Film contacts and is mounted to following belt and makes copolymer (B) towards the wadding tire.Bonded nonwoven is a kind of polyester textile of 0.63 ounce per square yard, it has 135 ℃ fusing point, and trade name is " Spunfab Type PE204 ", places between film and the wadding tire, the composite bed temperature is 150 ℃ a conveyer belt, with about 7 yards (6.4 meters)/minute speed process.
Example 4
The all conditions of making film in example 4 is all identical with example 3.In lamination step, 10 yards commodity wadding tire samples are put into the flat layer pressure device with bilayer film, do not have bonded mat.Replaced the nonwoven bonded mat, " Bostik " 5178 polyester powders have been added to film surface with about 0.5 ounce per square yard.The composite bed conveyer belt with about 7 yards (6.4 meters)/minute, process at 150 ℃.
Griltex EMS 6D2-2 also can be used as powder adhesives and replaces " Bostik " 5178 polyester powders.
Do not need to add too much adhesive, the amount that adds 0.25 ounce per square yard can obtain bonding effect preferably.Be appreciated that accurate addition depends on many factors, for example on technology: the kind of application and style, predetermined use, the selection of aesthetic and material.
These compositions have shown good waterproof/gas permeability, the phenomenon that does not have local delamination, and this phenomenon had run into when the spunbond poly-para Toluic Acid's fourth diester fabric of film and a kind of nonwoven light weight scrim combines, because film only only depends on extruding to cover on the fabric.Unless scrim fabric use a kind of film and the fine bonding adhesive of fabric puts glued the local delamination phenomenon can not appear.Film also can seal, and makes fiberfill fibers not see through outer cover.
Claims (4)
1, a kind of polyester fiberfill fibers of gluing wadding tire, or a kind of clothes or other goods that are filled with gluing polyester fiberfill fibers, wherein the polyester fiberfill fibers of gluing is to be fixed on the continuous flexible layer of a waterproof hydrophilic elastic material, and the steam transmitance of this elastomeric material is at least 3500gm.mil/m
224 hours [as described in ASTME96-66 (Procedure BW)], described hydrophilic elastic material is a kind of copolyether ester elastomeric material or two or more copolyether ester elastomeric material mix, a large amount of long-chain ester units and short-chain ester units are arranged in this elastomeric material, and they join end to end by ester linkage.Described long-chain ester units is represented with following formula:
Described short-chain ester units is represented with following formula:
Here, G is the divalent group after terminal hydroxyl is removed from poly-alkylene oxyethanol (mean molecule quantity is 400-3500).Then, add ethylene oxide group by poly-alkylene oxygen glycol in the mixture of copolyether ester or two or more copolyether ester, the amount of ethylene oxide of adding is about 25-68% (weight) with respect to two or more the total amount of mixture of copolyether ester or its; R is the divalent group after carboxyl is removed from dicarboxylic acids (molecular weight is less than 300); D is the divalent group after hydroxyl is removed from glycol (molecular weight is less than 250).Two or more mixture of described copolymerized ether ester of hydrophile or its has the short-chain ester units of about 25-80% (weight).
2, the polyester fiberfill fibers of gluing according to claim 1 wadding tire or clothes or other goods, wherein fiberfill fibers is that insert layer by a hydrophobic elastomeric material is fixed on the continuous flexible layer of described hydrophilic elastomeric material, and it is 400-2500gm.mil/m that this hydrophobic elastomeric material has the steam transmitance
2/ 24 hours, described hydrophobic elastomeric material was the mixture of a kind of copolyether ester elastomeric material or two or more copolyether ester elastomeric material, had the long-chain ester units and the short-chain ester units of many repetitions, and described long-chain ester units is represented with following formula:
Described short-chain ester units is represented with following formula:
Wherein G is one and removes the substituting group of divalence behind the terminal hydroxyl from poly-alkylene oxygen glycol (the about 400-3500 of the mean molecule quantity that has), and the amount by ethylene oxide group in the poly-alkylene oxygen glycol adding copolyether ester is not more than 20 percentage by weights; R is from having molecular weight less than a divalent substituent of removing 300 the dicarboxylic acids behind the carbonyl; D is from having molecular weight less than the divalent group of removing 250 the glycol behind the hydroxyl; Described hydrophobic copolyether ester or two or more copolyether ester mixture have the short-chain ester units of about 25-80 percentage by weight.
3, gluing polyester fiberfill fibers wadding tire according to claim 2 or clothes or other goods, wherein fiberfill fibers is bonded on the described hydrophobic elastomeric material discontinuously with a kind of adhesive.
4, gluing polyester fiberfill fibers wadding tire according to claim 3 or clothes or other goods, wherein said hydrophobic elastomeric material is to use binder fiber and fiberfill fibers bonding, and the fusing point of this binder fiber is lower than polyester fiberfill fibers and described hydrophobic elastomeric material.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US44961589A | 1989-12-12 | 1989-12-12 | |
| US449,615 | 1989-12-12 |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN1054108A true CN1054108A (en) | 1991-08-28 |
Family
ID=23784827
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN90110425A Pending CN1054108A (en) | 1989-12-12 | 1990-12-12 | Improved waterproofing of polyester fiberfill |
Country Status (10)
| Country | Link |
|---|---|
| EP (1) | EP0505466A1 (en) |
| JP (1) | JPH05502194A (en) |
| KR (1) | KR927003901A (en) |
| CN (1) | CN1054108A (en) |
| AR (1) | AR244362A1 (en) |
| AU (1) | AU6979791A (en) |
| BR (1) | BR9007909A (en) |
| CA (1) | CA2071202A1 (en) |
| MA (1) | MA22012A1 (en) |
| WO (1) | WO1991009166A1 (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105621340A (en) * | 2015-12-30 | 2016-06-01 | 3M创新有限公司 | Insulating filling material, preparing method thereof and insulating product |
| CN112739862A (en) * | 2018-09-24 | 2021-04-30 | 科德宝两合公司 | Application of non-woven fabric in preparation of filling lining |
Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE9408097U1 (en) * | 1994-05-17 | 1995-09-14 | M. Faist GmbH & Co KG, 86381 Krumbach | Soundproofing component |
| DE69811573T2 (en) * | 1997-07-31 | 2003-12-11 | Teijin Ltd., Osaka | Multi-layer material and tent made with it |
| US6203872B1 (en) | 1998-07-23 | 2001-03-20 | Akzo Nobel Nv | Waterproof and water vapour permeable lining |
| US7070841B2 (en) * | 2001-04-11 | 2006-07-04 | E. I. Du Pont De Nemours And Company | Insulating label stock |
| US20210164140A1 (en) * | 2018-06-14 | 2021-06-03 | 3M Innovative Properties Company | Thermal insulation flocculus material, preparation method thereof, and thermal insulation article |
| CN108754868B (en) * | 2018-06-14 | 2022-01-14 | 3M创新有限公司 | Heat-insulating flocculus material, preparation method thereof and heat-insulating product |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4304817A (en) * | 1979-02-28 | 1981-12-08 | E. I. Dupont De Nemours & Company | Polyester fiberfill blends |
| US4725481A (en) * | 1986-10-31 | 1988-02-16 | E. I. Du Pont De Nemours And Company | Vapor-permeable, waterproof bicomponent structure |
-
1990
- 1990-12-07 KR KR1019920701389A patent/KR927003901A/en not_active Application Discontinuation
- 1990-12-07 WO PCT/US1990/007051 patent/WO1991009166A1/en not_active Application Discontinuation
- 1990-12-07 JP JP91501948A patent/JPH05502194A/en active Pending
- 1990-12-07 BR BR909007909A patent/BR9007909A/en unknown
- 1990-12-07 EP EP91901528A patent/EP0505466A1/en not_active Withdrawn
- 1990-12-07 CA CA002071202A patent/CA2071202A1/en not_active Abandoned
- 1990-12-07 AU AU69797/91A patent/AU6979791A/en not_active Abandoned
- 1990-12-10 MA MA22287A patent/MA22012A1/en unknown
- 1990-12-12 CN CN90110425A patent/CN1054108A/en active Pending
- 1990-12-12 AR AR90318604A patent/AR244362A1/en active
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105621340A (en) * | 2015-12-30 | 2016-06-01 | 3M创新有限公司 | Insulating filling material, preparing method thereof and insulating product |
| CN112739862A (en) * | 2018-09-24 | 2021-04-30 | 科德宝两合公司 | Application of non-woven fabric in preparation of filling lining |
Also Published As
| Publication number | Publication date |
|---|---|
| EP0505466A1 (en) | 1992-09-30 |
| WO1991009166A1 (en) | 1991-06-27 |
| CA2071202A1 (en) | 1991-06-13 |
| KR927003901A (en) | 1992-12-18 |
| AU6979791A (en) | 1991-07-18 |
| BR9007909A (en) | 1992-09-15 |
| JPH05502194A (en) | 1993-04-22 |
| AR244362A1 (en) | 1993-10-29 |
| MA22012A1 (en) | 1991-07-01 |
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| C01 | Deemed withdrawal of patent application (patent law 1993) | ||
| WD01 | Invention patent application deemed withdrawn after publication |