CN113564937B - Polyurethane composition for capsule material, and preparation method and application thereof - Google Patents

Polyurethane composition for capsule material, and preparation method and application thereof Download PDF

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Publication number
CN113564937B
CN113564937B CN202110836658.6A CN202110836658A CN113564937B CN 113564937 B CN113564937 B CN 113564937B CN 202110836658 A CN202110836658 A CN 202110836658A CN 113564937 B CN113564937 B CN 113564937B
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polyurethane
fiber fabric
layer
parts
polyurethane composition
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CN113564937A (en
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刘军虎
纪雪梅
赵伟涛
郑燕
陈帅
宋鑫
刘贤豪
臧立恒
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China Lucky Group Corp
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China Lucky Group Corp
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    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06N—WALL, FLOOR, OR LIKE COVERING MATERIALS, e.g. LINOLEUM, OILCLOTH, ARTIFICIAL LEATHER, ROOFING FELT, CONSISTING OF A FIBROUS WEB COATED WITH A LAYER OF MACROMOLECULAR MATERIAL; FLEXIBLE SHEET MATERIAL NOT OTHERWISE PROVIDED FOR
    • D06N3/00—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof
    • D06N3/12—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof with macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds, e.g. gelatine proteins
    • D06N3/14—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof with macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds, e.g. gelatine proteins with polyurethanes
    • D06N3/145—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof with macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds, e.g. gelatine proteins with polyurethanes two or more layers of polyurethanes
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B64—AIRCRAFT; AVIATION; COSMONAUTICS
    • B64B—LIGHTER-THAN AIR AIRCRAFT
    • B64B1/00—Lighter-than-air aircraft
    • B64B1/58—Arrangements or construction of gas-bags; Filling arrangements
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F283/00—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G
    • C08F283/006—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polymers provided for in C08G18/00
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    • D06N3/00—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof
    • D06N3/0002—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof characterised by the substrate
    • D06N3/0015—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof characterised by the substrate using fibres of specified chemical or physical nature, e.g. natural silk
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    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06N—WALL, FLOOR, OR LIKE COVERING MATERIALS, e.g. LINOLEUM, OILCLOTH, ARTIFICIAL LEATHER, ROOFING FELT, CONSISTING OF A FIBROUS WEB COATED WITH A LAYER OF MACROMOLECULAR MATERIAL; FLEXIBLE SHEET MATERIAL NOT OTHERWISE PROVIDED FOR
    • D06N3/00—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof
    • D06N3/0002—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof characterised by the substrate
    • D06N3/0015—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof characterised by the substrate using fibres of specified chemical or physical nature, e.g. natural silk
    • D06N3/0022—Glass fibres
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    • D06N—WALL, FLOOR, OR LIKE COVERING MATERIALS, e.g. LINOLEUM, OILCLOTH, ARTIFICIAL LEATHER, ROOFING FELT, CONSISTING OF A FIBROUS WEB COATED WITH A LAYER OF MACROMOLECULAR MATERIAL; FLEXIBLE SHEET MATERIAL NOT OTHERWISE PROVIDED FOR
    • D06N3/00—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof
    • D06N3/0002—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof characterised by the substrate
    • D06N3/0015—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof characterised by the substrate using fibres of specified chemical or physical nature, e.g. natural silk
    • D06N3/0034—Polyamide fibres
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    • D06N3/00—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof
    • D06N3/0002—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof characterised by the substrate
    • D06N3/0015—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof characterised by the substrate using fibres of specified chemical or physical nature, e.g. natural silk
    • D06N3/0038—Polyolefin fibres
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    • D06N3/00—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof
    • D06N3/0056—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof characterised by the compounding ingredients of the macro-molecular coating
    • D06N3/0063—Inorganic compounding ingredients, e.g. metals, carbon fibres, Na2CO3, metal layers; Post-treatment with inorganic compounds
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    • D06N3/00—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof
    • D06N3/007—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof characterised by mechanical or physical treatments
    • D06N3/0077—Embossing; Pressing of the surface; Tumbling and crumbling; Cracking; Cooling; Heating, e.g. mirror finish
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    • D06N2201/00—Chemical constitution of the fibres, threads or yarns
    • D06N2201/02—Synthetic macromolecular fibres
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    • D06N2201/00—Chemical constitution of the fibres, threads or yarns
    • D06N2201/08—Inorganic fibres
    • D06N2201/082—Glass fibres
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    • D06N2209/00—Properties of the materials
    • D06N2209/16—Properties of the materials having other properties
    • D06N2209/1692—Weather resistance
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    • D06N2211/00—Specially adapted uses
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    • D06N2211/26—Vehicles, transportation
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    • D06N2213/00—Others characteristics
    • D06N2213/03—Fibrous web coated on one side with at least two layers of the same polymer type, e.g. two coatings of polyolefin

Abstract

The invention discloses a polyurethane composition for a capsule material, a preparation method and application thereof, wherein the composition comprises 10-40 parts by weight of thermoplastic polyurethane elastomer, 5-20 parts by weight of polyurethane prepolymer, 0.1-1.5 parts by weight of chain extender, 0.3-2.5 parts by weight of grafting agent, 0.01-0.5 part by weight of initiator, 0.5-10 parts by weight of coupling agent, 0.5-5 parts by weight of inorganic nano particles and 60-300 parts by weight of solvent. The polyurethane composition is improved and is applied to the fiber fabric of the capsule body material to form a functional integrated bearing layer, so that the problem of poor bonding performance between the fiber fabric and other functional layers is solved; meanwhile, the capsule material is ensured to still have excellent welding performance under the high temperature condition of 85 ℃.

Description

Polyurethane composition for capsule material, and preparation method and application thereof
Technical Field
The invention belongs to the field of dielectric materials, and particularly relates to a polyurethane composition for a capsule material, and a preparation method and application thereof.
Background
Stratospheric airship refers to an airship flying in an atmospheric stratosphere, and the working height is generally about 18-24 km and mainly depends on static lift force to stay in the air for working. Due to the application advantages of stratospheric airships in the fields of military reconnaissance, space early warning, communication relay, space exploration and the like, the stratospheric airships are increasingly attracting attention in recent years. The performance of the capsule material as the main structural material of the airship directly influences the application efficiency of the airship, such as the floating height, the duration of flight, the effective load, the service life and the like.
The working environment of stratospheric airship is very harsh: the temperature is low (the lowest temperature is about-55 ℃), and the day-night temperature difference is large; the atmospheric lean density was about 0.0889kg/m 3 Only 1/14 of the ground; ultraviolet radiation and ozone have strong actions. If the airship is operated for a long period of time in such an environment, the capsule material must have high strength and weather resistance as well as low areal density and helium permeability. The capsule body materials are all in a multi-layer composite structure, and the structure generally comprises a welding layer, a bearing layer, a barrier layer, a weather-proof layer and a bonding layer between the layers.
The polyurethane material has wide application in the capsule material with excellent impact resistance, durability, low temperature resistance, fatigue resistance and good construction performance. For example, polyurethane materials are used as the balloon material welding layer and the adhesive layer. However, the following problems are found in the practical application process of the polyurethane material:
(1) The polyurethane material is used as an adhesive layer between the layers of the capsule body material, is generally a single-component or double-component polyurethane adhesive, is mainly used for bonding the interlayer structure of the capsule body material, has enough sizing amount for realizing excellent bonding performance, particularly has enough sizing amount for bonding between the bearing layer and the functional layer, and generally has the total sizing amount of 40g/m 2 ～50g/m 2 . The requirement of the stratospheric airship on the low surface density of the capsule material is influenced, and meanwhile, the difference of the bonding strength between the warps and the wefts (generally, the bonding strength of the warp direction is higher than that of the weft direction) is caused due to the difference of the tension between the warps and the wefts in the compounding process, so that the overall strength performance of the capsule material is influenced.
(2) The polyurethane material is used as a welding layer of the capsule body material, is generally thermoplastic polyurethane material, is easy to process and has excellent bonding performance, but has poor temperature resistance, and when the prepared welding material reaches 80 ℃ at the ambient temperature, the bonding strength is obviously reduced, so that the overall service life of the stratospheric airship is influenced.
Therefore, the polyurethane composition applied to the capsule material is developed, the technical problems of poor bonding performance between the polyurethane composition and the bearing layer and poor temperature resistance of the polyurethane composition are solved, and the polyurethane composition has profound significance for promoting the development of the stratospheric airship capsule material.
Disclosure of Invention
The present invention aims to solve at least one of the technical problems in the related art to some extent. To this end, an object of the present invention is to propose a polyurethane composition for a capsule material, a process for its preparation and its use. The polyurethane composition is improved and is applied to the fiber fabric of the capsule body material to form a functional integrated bearing layer, so that the problem of poor bonding performance between the fiber fabric and other functional layers is solved; meanwhile, the capsule material is ensured to still have excellent welding performance under the high temperature condition of 85 ℃.
In one aspect of the invention, the invention provides a polyurethane composition for a bladder material, comprising, in accordance with an embodiment of the invention: 10 to 40 weight parts of thermoplastic polyurethane elastomer, 5 to 20 weight parts of polyurethane prepolymer, 0.1 to 1.5 weight parts of chain extender, 0.3 to 2.5 weight parts of grafting agent, 0.01 to 0.5 weight parts of initiator, 0.5 to 10 weight parts of coupling agent, 0.5 to 5 weight parts of inorganic nano particles and 60 to 300 weight parts of solvent.
According to the polyurethane composition for the capsule body material, disclosed by the embodiment of the invention, the polyurethane composition can be used for preparing the heat sealing layer and the buffer layer on two sides of the functional integrated bearing layer in the capsule body material, wherein the polyurethane composition has excellent welding adhesion performance as a heat sealing layer, particularly in the testing process of tensile strength in a high-temperature environment at 85 ℃, so that the capsule body material is ensured to still have excellent welding performance under the high-temperature condition at 85 ℃, and the fracture welding part of the capsule body material is ensured not to crack; as the buffer layer, the buffer layer has excellent bonding performance with the surface of the fiber, and has excellent bonding performance with other functional layers, so that the use of an adhesive between the functional layer and the bearing layer is reduced, the surface density is effectively reduced, and the problem of poor bonding performance between the fiber fabric and other functional layers is solved.
In addition, the polyurethane composition for a bladder material according to the above embodiment of the present invention may have the following additional technical features:
in some embodiments of the invention, the mass ratio of the polyurethane prepolymer to the thermoplastic polyurethane elastomer is from 1/8 to 1/2.
In some embodiments of the invention, the mass ratio of the inorganic nanoparticles to the thermoplastic polyurethane elastomer is from 1/80 to 1/20, preferably from 1/80 to 1/50.
In some embodiments of the invention, the thermoplastic polyurethane elastomer is selected from at least one of a polycarbonate-type polyurethane elastomer, a polyolefin-type polyurethane elastomer, a polyether-type polyurethane elastomer, and a polyester-type polyurethane elastomer.
In some embodiments of the invention, the thermoplastic polyurethane elastomer has a molecular weight of 50000 to 250000.
In some embodiments of the invention, the polyurethane prepolymer is selected from at least one of an isocyanate-terminated polyurethane prepolymer, a hydroxyl-terminated polyurethane prepolymer, a blocked group-containing polyurethane prepolymer, a silane-terminated polyurethane prepolymer, and an alkyl acrylate-terminated polyurethane prepolymer.
In some embodiments of the invention, the chain extender is selected from at least one of trimethylolpropane, glycerol, diethylene glycol, triethylene glycol, neopentyl glycol, sorbitol, 1, 4-butanediol, triethylene glycol, 1, 4-cyclohexanedimethanol, diethylaminoethanol, 3 '-dichloro-4, 4' -diamino-diphenylmethane, ethylenediamine, N-dihydroxy (diisopropyl) aniline, 3', 4' -biphenyltetracarboxylic dianhydride, 3', 4' -benzophenone tetracarboxylic anhydride, and 1,2,4, 5-benzene tetracarboxylic dianhydride.
In some embodiments of the invention, the grafting agent is selected from at least one of methyl methacrylate, butyl acrylate, acrylic acid, hydroxypropyl acrylate, hydroxyethyl acrylate, N-methylolacrylamide, propyl methacrylate triethoxysilane, vinyltrimethoxysilane, vinyltriethoxysilane, 1,3, 5-tris (3-trimethoxysilylpropyl) isocyanurate, gamma-ureidopropyltrimethoxysilane, gamma-ureidotriethoxysilane, gamma-isocyanatopropyltrimethoxysilane, gamma-isocyanatotriethoxysilane, and trimethyl propenyl phosphate.
In some embodiments of the invention, the initiator is an azo-type initiator.
In some embodiments of the present invention, the azo-based initiator is selected from at least one of azobisisobutyronitrile, azobisisoheptonitrile, dimethyl azobisisobutyrate, and azobisisovaleronitrile.
In some embodiments of the invention, the coupling agent is selected from at least one of tetramethoxysilane, tetraethoxysilane, gamma-aminopropyl trimethoxysilane, gamma-aminopropyl triethoxysilane, diethylaminomethyl triethoxysilane, N- (beta-aminoethyl) -gamma-aminopropyl trimethoxysilane, gamma-mercaptopropyl triethoxysilane, gamma- (2, 3-glycidoxy) propyl trimethoxysilane, gamma- (2, 3-glycidoxy) propyl triethoxysilane, triethyl borate, and nitrilotris (methylenephosphonic acid).
In some embodiments of the invention, the inorganic nanoparticles are selected from at least one of nano titanium dioxide, nano zinc oxide, nano aluminum oxide, nano silicon oxide, graphene, carbon nanotubes, mica, and montmorillonite.
In some embodiments of the invention, the inorganic nanoparticles have a particle size of 10nm to 100nm.
In a second aspect of the invention, the invention provides a capsule material. According to the embodiment of the invention, the capsule material comprises a weather-resistant layer, a helium-blocking layer and a functional integrated bearing layer which are sequentially laminated; the functional integrated bearing layer comprises a buffer layer, a fiber fabric and a heat sealing layer which are sequentially laminated; the buffer layer and the heat seal layer were prepared using the polyurethane composition described in the above examples as a raw material. Therefore, the polyurethane composition is used for preparing a heat sealing layer and a buffer layer on two sides of a functional integrated bearing layer in a capsule material, wherein the polyurethane composition has excellent welding bonding performance as a heat sealing layer, particularly in the testing process of tensile strength in a high-temperature environment at 85 ℃, ensures that the capsule material still has excellent welding performance under the high-temperature environment at 85 ℃, and ensures that the broken welding part of the material is not cracked; as the buffer layer, on one hand, the buffer layer has excellent bonding performance with the surface of the fiber, and meanwhile, the buffer layer has excellent bonding performance with other functional layers, so that the use of an adhesive between the functional layers and the bearing layer is reduced, the surface density is effectively reduced, and the problem of poor bonding performance between the fiber fabric and other functional layers is solved.
In addition, the capsule material according to the above embodiment of the present invention may further have the following additional technical features:
in some embodiments of the invention, the functional integrated load bearing layer has an areal density of 20-200 g/m 2 。
In some embodiments of the invention, the buffer layer has an areal density of 1 to 10g/m 2 The surface density of the fiber fabric is 5-150 g/m 2 The surface density of the heat sealing layer is 30-110 g/m 2 。
In some embodiments of the present invention, the helium-blocking layer has an areal density of 5-30 g/m 2 。
In some embodiments of the invention, the areal density of the weathering layer is from 10 to 30g/m 2 。
In some embodiments of the invention, the fiber fabric is selected from at least one of a Vectran fiber fabric, a carbon fiber fabric, a glass fiber fabric, a basalt fiber fabric, a silicon nitride fiber fabric, a polyetheretherketone fiber fabric, a Kevlar fiber fabric, a polyimide fiber fabric, a poly-p-phenylene bisoxazole fiber fabric, and an ultra high molecular weight polyethylene fiber.
In a third aspect of the invention, the invention provides a process for preparing the polyurethane composition described above for a bladder material. According to an embodiment of the invention, the method comprises:
(1) Mixing and stirring a thermoplastic polyurethane elastomer, a polyurethane prepolymer, a chain extender, a grafting agent, an initiator and a solvent to obtain a mixed solution B;
(2) The mixed liquid B, the coupling agent and the inorganic nano particles are mixed and dispersed on a high shear emulsifying machine so as to obtain a polyurethane composition C.
According to the method for preparing the polyurethane composition for the capsule material, disclosed by the embodiment of the invention, the polyurethane composition prepared by the method can be used for preparing the heat sealing layer and the buffer layer on two sides of the functional integrated bearing layer in the capsule material, wherein the polyurethane composition has excellent welding adhesion performance as a heat sealing layer, particularly in the testing process of tensile strength in a high-temperature environment at 85 ℃, so that the capsule material is ensured to still have excellent welding performance under the high-temperature condition at 85 ℃, and the fracture welding position of the material is ensured not to crack; as the buffer layer, on one hand, the buffer layer has excellent bonding performance with the surface of the fiber, and meanwhile, the buffer layer has excellent bonding performance with other functional layers, so that the use of an adhesive between the functional layers and the bearing layer is reduced, the surface density is effectively reduced, and the problem of poor bonding performance between the fiber fabric and other functional layers is solved.
In addition, the method for preparing the polyurethane composition for a bladder material according to the above embodiment of the present invention may further have the following additional technical features:
In some embodiments of the invention, step (1) further comprises the steps of:
(1-1) mixing the thermoplastic polyurethane elastomer and the solvent, and stirring to obtain a mixed liquid A;
(1-2) mixing the mixed liquid A, the polyurethane prepolymer, the chain extender, the grafting agent and the initiator, and stirring to obtain a mixed liquid B.
In some embodiments of the invention, in step (1), the stirring temperature is from 40 ℃ to 85 ℃.
In some embodiments of the invention, in step (2), the high shear emulsifying machine is operated at a speed of 3000 rpm to 5000 rpm for a dispersing time of 1 to 2 hours.
In some embodiments of the invention, in step (2), the solids content of the polyurethane composition C is 5% to 20%.
In a fourth aspect of the invention, the invention provides a method of preparing the capsule material described above. According to an embodiment of the invention, the method comprises:
(a) Polyurethane composition C was prepared according to the method for preparing polyurethane composition described in the above examples;
(b) Respectively coating the polyurethane composition C on two sides of the fiber fabric, and curing to obtain a heat sealing layer and a buffer layer;
(c) And sequentially coating a helium blocking layer and a weather-resistant layer on the surface of the buffer layer, which is far away from the fiber fabric, and curing to obtain the capsule material.
According to the method for preparing the capsule material, disclosed by the embodiment of the invention, the polyurethane composition forms the functional integrated bearing layer on the fiber fabric through a coating technology, so that the use of an adhesive is avoided in the preparation process of the capsule material, the strength of the capsule material is ensured, and the overall surface density is effectively reduced. In addition, the functional layers are all realized through a coating technology, so that an interlayer structure is simplified, and the surface density of the prepared capsule material is effectively reduced.
In addition, the method for preparing the capsule material according to the above embodiment of the present invention may further have the following additional technical features:
in some embodiments of the invention, in step (b), the curing temperature is from 30 ℃ to 100 ℃.
In some embodiments of the invention, in step (c), the curing temperature is 75 ℃ to 120 ℃.
In a fifth aspect of the invention, the invention provides a flying device. According to an embodiment of the invention, the flight device is provided with the capsule body material described in the above embodiment or the capsule body material prepared by the method described in the above embodiment. Therefore, the capsule material of the flight device has better strength performance and longer service life.
Additional aspects and advantages of the invention will be set forth in part in the description which follows, and in part will be obvious from the description, or may be learned by practice of the invention.
Drawings
The foregoing and/or additional aspects and advantages of the invention will become apparent and may be better understood from the following description of embodiments taken in conjunction with the accompanying drawings in which:
FIG. 1 is a schematic structural diagram of a capsule material prepared according to the present invention;
fig. 2 is a schematic structural view of a welded belt prepared using the capsule material of the present invention.
In the figure, a 1-weather resistant layer; a 2-helium blocking layer; 3-a functional integrated force bearing layer; 31-a buffer layer; 32-a fibrous web; 33-heat seal layer; 100-capsule material; 101-heat sealing layers of capsule material; 102-a weather-resistant layer of capsule material; 200-welding a belt; 300-sealing tape.
Detailed Description
Reference will now be made in detail to embodiments of the present invention, examples of which are illustrated in the accompanying drawings. The embodiments described below by referring to the drawings are illustrative and intended to explain the present invention and should not be construed as limiting the invention.
In one aspect of the invention, the invention proposes a polyurethane composition for a balloon material, comprising, according to an embodiment of the invention: 10 to 40 weight parts of thermoplastic polyurethane elastomer, 5 to 20 weight parts of polyurethane prepolymer, 0.1 to 1.5 weight parts of chain extender, 0.3 to 2.5 weight parts of grafting agent, 0.01 to 0.5 weight parts of initiator, 0.5 to 10 weight parts of coupling agent, 0.5 to 5 weight parts of inorganic nano particles and 60 to 300 weight parts of solvent. Therefore, the polyurethane composition can be used for preparing a heat sealing layer and a buffer layer on two sides of a functional integrated bearing layer in a capsule material, wherein the polyurethane composition has excellent welding bonding performance as a heat sealing layer, particularly in the testing process of tensile strength in a high-temperature environment at 85 ℃, ensures that the capsule material still has excellent welding performance under the high-temperature environment at 85 ℃, and ensures that the broken welding part of the material is not cracked; as the buffer layer, the buffer layer has excellent bonding performance with the surface of the fiber, and has excellent bonding performance with other functional layers, so that the use of an adhesive between the functional layer and the bearing layer is reduced, the surface density is effectively reduced, and the problem of poor bonding performance between the fiber fabric and other functional layers is solved. The inventors found that if the content of the thermoplastic polyurethane elastomer is too small, the adhesion property of the buffer layer and the fiber fabric layer becomes poor, and the buffer layer becomes brittle, so that the flexibility of the prepared capsule material becomes poor, and if the content is too large, the temperature resistance of the prepared capsule material becomes poor, particularly, when tested at a high temperature of 85 ℃, the tensile strength becomes poor, and the welded part slips; if the content of the polyurethane prepolymer is too low, the temperature resistance and the adhesion of the polyurethane composition are deteriorated, and if the content of the prepolymer is too high, the adhesion and the adhesion between the polyurethane composition and the fiber fabric are deteriorated; if the content of the chain extender is too small, the prepared polyurethane composition cannot achieve the expected bonding effect, and if the content is too large, the prepared polyurethane composition is too high in viscosity and poor in stability, so that the processability is affected; if the content of the grafting agent is too small, the prepared polyurethane composition cannot achieve the expected bonding effect, and if the content is too large, the prepared polyurethane composition has too high viscosity and poor stability, so that the use is affected; if the content of the initiator is too small, the prepared polyurethane combination cannot achieve the expected bonding effect, and if the content is too large, the stability of the prepared polyurethane combination is poor, and the use is affected; if the content of the inorganic nanoparticles is too large, the adhesive property of the polyurethane composition is affected, and if the content is too low, the desired effect cannot be achieved.
The thermoplastic polyurethane elastomer is a granular solid thermoplastic material prepared by polyaddition reaction of isocyanate and polyol, molecules are basically in a linear state, almost no chemical crosslinking points exist, physical crosslinking exists, the thermoplastic polyurethane elastomer is plasticized into liquid molecules after heating, and the liquid molecules become solid molecules after cooling, so that the thermoplastic polyurethane elastomer is the main component of the polyurethane composition. In the embodiment of the present invention, the specific kind of the thermoplastic polyurethane elastomer is not particularly limited, and a person skilled in the art may optionally select according to the actual situation, and as a preferable embodiment, the thermoplastic polyurethane elastomer is at least one selected from the group consisting of a polycarbonate type polyurethane elastomer, a polyolefin type polyurethane elastomer, a polyether type polyurethane elastomer and a polyester type polyurethane elastomer.
Further, the molecular weight of the thermoplastic polyurethane elastomer is 50000 to 250000, preferably 100000 to 20000, and the inventors found that if the molecular weight is too low, the adhesion property of the heat-seal layer as a capsule material is deteriorated; if the molecular weight is too high, the solubility of the polyurethane material is deteriorated, which is disadvantageous for the subsequent modification treatment of the polyurethane material.
The polyurethane prepolymer, also called isocyanate prepolymer, is a reactive semi-finished product prepared by reacting polyisocyanate and polyol according to a certain proportion. The invention adjusts the proportion of the whole soft segment and the hard segment of the polyurethane composition through the selection of the type of the polyurethane prepolymer and the control of the addition amount, thereby leading the prepared polyurethane composition to achieve the optimal performance in the aspects of cohesiveness and temperature resistance. Further, the polyurethane prepolymer is at least one selected from the group consisting of isocyanate-terminated polyurethane prepolymer, hydroxyl-terminated polyurethane prepolymer, blocked group-containing polyurethane prepolymer, silane-terminated polyurethane prepolymer and alkyl acrylate-terminated polyurethane prepolymer.
Further, the mass (m 2 ) Mass (m) with thermoplastic elastomer 1 ) Ratio m 2 /m 1 Between 1/8 and 1/2, the inventors found that if the amount of the polyurethane prepolymer added is too low, the heat resistance and adhesion properties of the polyurethane composition are deteriorated, and if the amount of the prepolymer added is too high, the adhesion and adhesion between the polyurethane composition and the fiber fabric are deteriorated.
The chain extender disclosed by the invention has the main effects of promoting the crosslinking modification between the thermoplastic elastomer and the polyurethane prepolymer in the polyurethane composition, so that the effect of controlling the integral soft segment and hard segment is achieved. The chain extender comprises a polyfunctional compound containing amine groups and/or hydroxyl groups. In the embodiment of the present invention, the specific kind of the chain extender is not particularly limited, and a person skilled in the art may optionally select it according to the actual situation, and as a preferable scheme, the chain extender is at least one selected from trimethylolpropane, glycerol, diethylene glycol, triethylene glycol, neopentyl glycol, sorbitol, 1, 4-butanediol, triethylene glycol, 1, 4-cyclohexanedimethanol, diethylaminoethanol, 3 '-dichloro-4, 4' -diamino-diphenylmethane, ethylenediamine, N-dihydroxy (diisopropyl) aniline, 3', 4' -biphenyltetracarboxylic dianhydride, 3', 4' -benzophenone tetracarboxylic anhydride and 1,2,4, 5-benzoic dianhydride.
The grafting agent refers to a multifunctional compound with a conjugated double bond structure, and on one hand, unreacted amino or hydroxyl on a molecular chain in the polyurethane composition can be reacted to form a grafted compound; on the other hand, the conjugated double bond structure in the grafting agent is polymerized under the action of the initiator to form a grafted polymer on the molecular chain of the polyurethane composition, so that the chemical crosslinking property in the polyurethane composition is enhanced, and the overall adhesive property of the composition is improved. In the embodiment of the present invention, the specific kind of the grafting agent is not particularly limited, and a person skilled in the art may optionally select it according to the actual situation, and as a preferable embodiment, the grafting agent is at least one selected from the group consisting of methyl methacrylate, butyl acrylate, acrylic acid-hydroxypropyl ester, acrylic acid-hydroxyethyl ester, N-methylolacrylamide, propyl methacrylate-based triethoxysilane, vinyltrimethoxysilane, vinyltriethoxysilane, 1,3, 5-tris (3-trimethoxysilylpropyl) isocyanurate, γ -ureidopropyltrimethoxysilane, γ -ureidotriethoxysilane, γ -isocyanatopropyltrimethoxysilane, γ -isocyanatotriethoxysilane, and trimethyl propenyl phosphate.
The initiator is mainly used for initiating the polymerization reaction of the conjugated double bond in the grafting agent, and azo initiators are preferred. The specific kind of the azo initiator is not particularly limited, and may be arbitrarily selected by those skilled in the art according to the actual circumstances, and as a preferable embodiment, the azo initiator is selected from at least one of azobisisobutyronitrile, azobisisoheptonitrile, dimethyl azobisisobutyrate, and azobisisovaleronitrile.
The coupling agent disclosed by the invention can promote the fusion and coupling of the components of the polyurethane composition, improve the adhesive property of the polyurethane composition, and effectively improve the adhesive force between the polyurethane composition and the fiber fabric. In the embodiment of the present invention, the specific kind of the coupling agent is not particularly limited, and a person skilled in the art may optionally select it according to the actual situation, and as a preferable scheme, the coupling agent is at least one selected from the group consisting of tetramethoxysilane, tetraethoxysilane, gamma-aminopropyl trimethoxysilane, gamma-aminopropyl triethoxysilane, diethylaminomethyl triethoxysilane, N- (β -aminoethyl) -gamma-aminopropyl trimethoxysilane, gamma-mercaptopropyl triethoxysilane, gamma- (2, 3-glycidoxy) propyl trimethoxysilane, gamma- (2, 3-glycidoxy) propyl triethoxysilane, triethyl borate and nitrilotris (methylenephosphonic acid).
The nano particles of the invention are cooperated with thermoplastic polyurethane elastomer in the polyurethane composition to improve the temperature resistance, strength and weather resistance of the whole polyurethane composition. In the embodiment of the present invention, the specific kind of the inorganic nanoparticle is not particularly limited, and a person skilled in the art may optionally select according to the actual situation, and as a preferred embodiment, the inorganic nanoparticle is selected from at least one of nano titanium dioxide, nano zinc oxide, nano aluminum oxide, nano silicon oxide, graphene, carbon nanotube, mica and montmorillonite.
Further, the inorganic nanoparticle mass (m 5 ) Mass (m) with thermoplastic elastomer 1 ) Mass ratio m of (2) 5 /m 1 Preferably 1/80 to 1/20, more preferably 1/80 to 1/50. The inventors found that if the amount of the inorganic nanoparticles added is too large, the adhesive property of the polyurethane composition is affected, and if the amount is too low, the desired effect cannot be achieved.
Further, the particle size of the inorganic nanoparticles is 10nm to 100nm, and the inventors found that if the particle size of the inorganic nanoparticles is too large, the dispersibility of the nanoparticles in a polyurethane system is affected; if the particle size is too small, the cost is too high, which is uneconomical.
The solvent is a mixture solvent of butanone and ethyl acetate, the mass ratio of butanone to ethyl acetate is not particularly limited, the thermoplastic polyurethane elastomer can be stably dissolved as a standard, the mass ratio of butanone to ethyl acetate is preferably 10/1-1/5, the higher the addition amount of ethyl acetate is, the dissolution performance of the thermoplastic elastomer is deteriorated, and the higher the addition amount of butanone is, the uneconomical.
In a second aspect of the invention, the invention provides a capsule material. According to an embodiment of the present invention, referring to fig. 1, the capsule material 100 includes a weather-resistant layer 1, a helium-blocking layer 2, and a functional integrated bearing layer 3, which are sequentially stacked; the function integrated bearing layer 3 comprises a buffer layer 31, a fiber fabric 32 and a heat sealing layer 33 which are sequentially stacked; the buffer layer 31 and the heat seal layer 33 are prepared using the polyurethane composition described in the above examples as a raw material. Therefore, the polyurethane composition is used for preparing the heat sealing layer 33 and the buffer layer 31 on two sides of the functional integrated bearing layer in the capsule material, wherein the heat sealing layer has excellent welding bonding performance, particularly in the testing process of tensile strength in a high-temperature environment at 85 ℃, so that the capsule material still has excellent welding performance at the high-temperature environment at 85 ℃, and the broken welding part of the material is prevented from cracking; as the buffer layer, on one hand, the buffer layer has excellent bonding performance with the surface of the fiber, and meanwhile, the buffer layer has excellent bonding performance with other functional layers, so that the use of an adhesive between the functional layers and the bearing layer is reduced, the surface density is effectively reduced, and the problem of poor bonding performance between the fiber fabric and other functional layers is solved.
Fig. 2 is a schematic structural view of a weld tape made using the balloon material made in accordance with the present invention, wherein the weld tape 200 is disposed on the heat seal layer 101 of the balloon material and the seal tape 300 is disposed on the weather resistant layer 102 of the balloon material. Wherein the welding strip 200 is the base material of the capsule body material, and the sealing strip 300 is a pressure-sensitive adhesive strip with weather resistance.
In some embodiments of the present invention, the helium-blocking layer has an areal density of 5-30 g/m 2 . Helium-resistant layer 2 of the capsule material is a helium-resistant coating formed by modifying polyethylene alcohol and polyacrylic acid which are independently developed by China LeKai group through ester crosslinking or other commercial helium-resistant performanceAnd (3) coating.
In some embodiments of the invention, the areal density of the weathering layer is from 10 to 30g/m 2 . The weather-resistant layer 1 is a weather-resistant coating or a commercial fluorine-containing resin layer which is independently developed by China Lekai group.
In the embodiment of the present invention, the specific kind of the fiber fabric is not particularly limited, and a person skilled in the art may optionally select it according to the actual situation, and as a preferable scheme, the fiber fabric is selected from at least one of Vectran fiber fabric, carbon fiber fabric, glass fiber fabric, basalt fiber fabric, silicon nitride fiber fabric, polyether ether ketone fiber fabric, kevlar fiber fabric, polyimide fiber fabric, poly (p-phenylene bisoxazole) fiber fabric and ultra high molecular weight polyethylene fiber. The manner of knitting the fiber fabric is not particularly limited, and plain weave, rib weave, twill weave, or basket weave is preferable.
In some embodiments of the invention, the surface density of the functional integrated bearing layer 3 is 20-200 g/m 2 The method comprises the steps of carrying out a first treatment on the surface of the Wherein the surface density of the buffer layer is 1-10 g/m 2 The surface density of the fiber fabric is 5-150 g/m 2 The surface density of the heat sealing layer is 30-110 g/m 2 。
In a third aspect of the invention, the invention provides a process for preparing the polyurethane composition described above for a bladder material. According to an embodiment of the invention, the method comprises:
s100: mixing thermoplastic polyurethane elastomer, polyurethane prepolymer, chain extender, grafting agent, initiator and solvent, stirring
In this step, a thermoplastic polyurethane elastomer, a polyurethane prepolymer, a chain extender, a grafting agent, an initiator and a solvent are mixed and stirred to obtain a mixed liquid B. Further, the stirring temperature is 40-85 ℃. The stirring time is not particularly limited as long as each substance is completely dissolved in the solvent.
As a preferred embodiment, the step further comprises the steps of:
s110: mixing the thermoplastic polyurethane elastomer and the solvent, and stirring to obtain a mixed solution A;
s120: and mixing and stirring the mixed solution A, the polyurethane prepolymer, the chain extender, the grafting agent and the initiator to obtain a mixed solution B.
S200: mixing the mixed solution B, the coupling agent and the inorganic nano particles, and dispersing on a high-shear emulsifying machine
In this step, the mixed liquid B, the coupling agent and the inorganic nanoparticles are mixed and dispersed on a high shear emulsifying machine to obtain a polyurethane composition C.
Further, the rotational speed of the high shear emulsifying machine is 3000 rpm to 5000 rpm, and the dispersing time is 1 to 2 hours, thereby sufficiently dispersing the coupling agent and the inorganic nanoparticles in the mixed liquid B to form the polyurethane composition C.
Further, the solid content of the polyurethane composition C is 5% -20%, and the inventor finds that the too low or too high solid content is not beneficial to continuous production of the capsule body material.
According to the method for preparing the polyurethane composition for the capsule material, disclosed by the embodiment of the invention, the polyurethane composition prepared by the method can be used for preparing the heat sealing layer and the buffer layer on two sides of the functional integrated bearing layer in the capsule material, wherein the polyurethane composition has excellent welding adhesion performance as a heat sealing layer, particularly in the testing process of tensile strength in a high-temperature environment at 85 ℃, so that the capsule material is ensured to still have excellent welding performance under the high-temperature condition at 85 ℃, and the fracture welding position of the material is ensured not to crack; as the buffer layer, on one hand, the buffer layer has excellent bonding performance with the surface of the fiber, and meanwhile, the buffer layer has excellent bonding performance with other functional layers, so that the use of an adhesive between the functional layers and the bearing layer is reduced, the surface density is effectively reduced, and the problem of poor bonding performance between the fiber fabric and other functional layers is solved.
In a fourth aspect of the invention, the invention provides a method of preparing the capsule material described above. According to an embodiment of the invention, the method comprises:
(a) Polyurethane composition C was prepared according to the method for preparing polyurethane composition described in the above examples;
(b) The polyurethane composition C was coated on both sides of the fabric, respectively, and cured to obtain a heat-seal layer and a buffer layer. Further, the curing temperature is 30-100 ℃.
The buffer layer and the heat sealing layer both adopt polyurethane composition C, but the buffer layer and the weather-proof layer realize the control of different sizing amounts of the buffer layer and the weather-proof layer by adjusting the coating process, so as to achieve the required surface density of each layer.
(c) And sequentially coating a helium blocking layer and a weather-resistant layer on the surface of the buffer layer, which is far away from the fiber fabric, and curing to obtain the capsule material. Further, the curing temperature is 75-120 ℃.
The coating method used in the preparation process of the capsule material is at least one selected from dip coating, spray coating, blade coating, slit coating, slide coating and micro gravure coating.
According to the method for preparing the capsule material, disclosed by the embodiment of the invention, the polyurethane composition forms the functional integrated bearing layer on the fiber fabric through a coating technology, so that the use of an adhesive is avoided in the preparation process of the capsule material, the strength of the capsule material is ensured, and the overall surface density is effectively reduced. In addition, the functional layers are all realized through a coating technology, so that an interlayer structure is simplified, and the surface density of the prepared capsule material is effectively reduced.
In a fifth aspect of the invention, the invention provides a flying device. According to an embodiment of the invention, the flight device is provided with the capsule body material described in the above embodiment or the capsule body material prepared by the method described in the above embodiment. Therefore, the capsule material of the flight device has better strength performance and longer service life.
Compared with the prior art, the invention has the following advantages:
1) The functional integrated bearing layer prepared by the invention ensures excellent adhesion performance between the bearing layer and other functional layers.
2) The polyurethane composition prepared by the invention is used as a heat sealing layer of a capsule body material, and still has excellent welding performance at the temperature of 85 ℃.
3) The weather-resistant layer and the helium-resistant layer in the capsule wall material prepared by the invention are both coated, so that the use of an adhesive is avoided, the surface density of the capsule wall material is effectively reduced, and the preparation process of the capsule wall material is simplified.
The following detailed description of embodiments of the invention is provided for the purpose of illustration only and is not to be construed as limiting the invention. In addition, all reagents employed in the examples below are commercially available or may be synthesized according to methods herein or known, and are readily available to those skilled in the art for reaction conditions not listed, if not explicitly stated.
Example 1
The polyurethane composition formula:
95.08 parts by mass of a polyether type thermoplastic elastomer (molecular weight: 50000), 425 parts by mass of butanone and 425 parts by mass of ethyl acetate were mixed and stirred sufficiently at 80℃until dissolved, to obtain A-1 liquid.
After the solution A-1 is restored to room temperature, 47.54 parts by mass of hydroxyl-terminated polyurethane prepolymer, 0.71 part by mass of chain extender glycerol, 1.43 parts by mass of grafting agent methyl methacrylate and 0.03 part by mass of initiator azobisisobutyronitrile are sequentially added into the solution A-1; after stirring evenly, heating to 80 ℃ and continuing to stir rapidly to obtain the B-1 liquid.
After the solution B-1 is restored to room temperature, 0.48 part by mass of coupling agent gamma-aminopropyl triethoxysilane and 4.75 parts by mass of inorganic nanoparticle titanium dioxide are sequentially added, the rotating speed is set to 3000 rpm on a high-shear emulsifying machine, the solution is rapidly dispersed for 1 hour, and then impurities are filtered, so that polyurethane composition solution APP-01 with the solid content of 15% is obtained.
Preparation of a capsule material:
the surface density is selected to be 105g/m 2 The Vectran fiber fabric is coated with a heat sealing layer and a buffer layer on two sides of the fiber fabric respectively by using a polyurethane composition solution APP-01 in a slit coating mode, wherein the sizing amount of the heat sealing layer is 37g/m 2 The sizing amount of the buffer layer is 8g/m 2 In the coating process, a release film is paved below the fiber in order to prevent glue leakage from sticking to the roller.
Selecting a doctor blade coating mode, firstly coating a helium-resistant coating on the surface of a buffer layer of the fiber fabric by using a LeKai helium-resistant coating liquid SC-1, wherein the curing condition is 100 ℃, the curing time is 3min, and the coating sizing amount is 10g/m 2 The method comprises the steps of carrying out a first treatment on the surface of the After the helium-resistant coating is finished, coating a fluorocarbon resin coating, wherein the curing condition is 110 ℃ for 3min, and the coating sizing amount is 10g/m 2 After the completion, the capsule material is obtained, and the surface density is 170g/m 2 。
Example 2
The polyurethane composition formula:
63.38 parts by mass of a polyether type thermoplastic elastomer (molecular weight: 150000), 600 parts by mass of methyl ethyl ketone and 300 parts by mass of ethyl acetate were mixed and stirred sufficiently at 80℃until dissolved, to obtain a-2 liquid.
After the solution A-2 is restored to room temperature, 31.69 parts by mass of isocyanate-terminated polyurethane prepolymer, 0.58 part by mass of chain extender 1, 4-butanediol, 0.95 part by mass of grafting agent propyl methacrylate triethoxysilane and 0.02 part by mass of initiator azo diisobutyl cyanide are sequentially added into the solution A-2; and after stirring uniformly, heating to 80 ℃ and continuing to stir rapidly to obtain the B-2 liquid.
After the solution B-2 is restored to room temperature, 0.32 mass part of coupling agent gamma-aminopropyl triethoxysilane and 3.17 mass parts of inorganic nanoparticle titanium dioxide are sequentially added, the rotating speed is set to 3500 revolutions per minute on a high-shear emulsifying machine, the solution is rapidly dispersed for 1 hour, and then impurities are filtered, so that polyurethane composition solution APP-02 with the solid content of 10% is obtained.
Preparation of a capsule material:
the surface density is selected to be 105g/m 2 The Vectran fiber fabric is coated with a heat sealing layer and a buffer layer on two sides of the fiber fabric respectively by using a polyurethane composition solution APP-02 in a slit coating mode, wherein the sizing amount of the heat sealing layer is 30g/m 2 The sizing amount of the buffer layer is 8g/m 2 In the coating process, a release film is paved below the fiber in order to prevent glue leakage from sticking to the roller.
Selecting a doctor blade coating methodFirstly, coating helium-resistant coating liquid SC-1 of LeKai on the surface of a buffer layer of a fiber fabric, wherein the curing condition is 100 ℃, the curing time is 3min, and the coating sizing amount is 10g/m 2 The method comprises the steps of carrying out a first treatment on the surface of the After the helium-resistant coating is finished, coating a fluorocarbon resin coating, wherein the curing condition is 110 ℃ for 3min, and the coating sizing amount is 10g/m 2 After the completion, the capsule material is obtained, and the surface density is 163g/m 2 。
Example 3
The polyurethane composition formula:
50.7 parts by mass of a polyether type thermoplastic elastomer (molecular weight 250000), 690 parts by mass of butanone and 230 parts by mass of ethyl acetate were mixed and stirred sufficiently at a temperature of 85℃until dissolved, to obtain a-3 liquid.
After the solution A-3 is restored to room temperature, 25.35 parts by mass of hydroxyl-terminated polyurethane prepolymer, 0.38 part by mass of chain extender 1, 4-butanediol, 0.76 part by mass of grafting agent propyl methacrylate triethoxysilane and 0.015 part by mass of initiator azo diisobutyl cyanide are sequentially added into the solution A-3; after stirring evenly, heating to 85 ℃ and continuing to stir rapidly to obtain the B-3 liquid.
After the solution B-3 is restored to room temperature, 0.25 mass part of coupling agent gamma- (2, 3-glycidoxy) propyl trimethoxy silane and 2.54 mass parts of inorganic nano particle silicon dioxide are sequentially added, the rotating speed is set to 3500 revolutions per minute on a high shear emulsifying machine, the solution is rapidly dispersed for 1 hour, and then impurities are filtered to obtain polyurethane composition solution APP-03 with the solid content of 8%.
Preparation of a capsule material:
the surface density is selected to be 105g/m 2 The Vectran fiber fabric is coated with a heat sealing layer and a buffer layer on two sides of the fiber fabric respectively by using a polyurethane composition solution APP-03 in a slit coating mode, wherein the sizing amount of the heat sealing layer is 30g/m 2 The sizing amount of the buffer layer is 8g/m 2 In the coating process, a release film is paved below the fiber in order to prevent glue leakage from sticking to the roller.
Selecting a doctor blade coating mode, firstly coating helium-resistant coating liquid SC-1 of LeKai on the surface of a buffer layer of the fiber fabric, wherein the curing condition is 100 ℃, the curing time is 3min, and the coating sizing amount is 10g/m 2 The method comprises the steps of carrying out a first treatment on the surface of the Waiting to blockAfter helium coating is completed, fluorocarbon resin coating is coated, the curing condition is 110 ℃ for 3min, and the coating sizing amount is 10g/m 2 After the completion, the capsule material is obtained, and the surface density is 163g/m 2 。
Example 4
Polyurethane composition solution APP-02 was prepared as in example 2.
Preparation of a capsule material:
the surface density is 110g/m 2 Polyimide fiber fabric, wherein a heat sealing layer and a buffer layer are respectively coated on two sides of the fiber fabric by using polyurethane composition solution APP-02 in a slit coating mode, and the sizing amount of the heat sealing layer is 30g/m 2 The sizing amount of the buffer layer is 10g/m 2 In the coating process, a release film is paved below the fiber in order to prevent glue leakage from sticking to the roller.
Selecting a doctor blade coating mode, firstly coating helium-resistant coating liquid SC-1 of LeKai on the surface of a buffer layer of the fiber fabric, wherein the curing condition is 120 ℃ for 3min, and the coating sizing amount is 10g/m 2 The method comprises the steps of carrying out a first treatment on the surface of the After the helium-resistant coating is finished, coating a fluorocarbon resin coating, wherein the curing condition is 125 ℃, the curing time is 3min, and the coating sizing amount is 10g/m 2 After the completion, the capsule material is obtained, and the surface density is 170g/m 2 。
Example 5
Polyurethane composition solution APP-02 was prepared as in example 2.
Preparation of a capsule material:
the surface density is selected to be 85g/m 2 The poly-p-phenylene benzobisoxazoline fiber fabric is coated with a heat sealing layer and a buffer layer on two sides of the fiber fabric respectively by using a polyurethane composition solution APP-02 in a slit coating mode, wherein the sizing amount of the heat sealing layer is 30g/m 2 The sizing amount of the buffer layer is 10g/m 2 In the coating process, a release film is paved below the fiber in order to prevent glue leakage from sticking to the roller.
Selecting a doctor blade coating mode, firstly coating helium-resistant coating liquid SC-1 of LeKai on the surface of a buffer layer of the fiber fabric, wherein the curing condition is 120 ℃ for 3min, and the coating sizing amount is 10g/m 2 The method comprises the steps of carrying out a first treatment on the surface of the After the helium-resistant coating is finished, fluorocarbon is coatedResin coating, curing condition is 125 ℃, 3min, coating sizing amount is 10g/m 2 After the completion, the capsule material is obtained, and the surface density is 145g/m 2 。
Example 6
Polyurethane composition solution APP-03 was prepared as in example 3.
Preparation of a capsule material:
the surface density is selected to be 90g/m 2 The ultra-high molecular weight polyethylene fiber fabric is coated with a heat sealing layer and a buffer layer on two sides of the fiber fabric respectively by using polyurethane composition solution APP-03 in a slit coating mode, wherein the sizing amount of the heat sealing layer is 35g/m 2 The sizing amount of the buffer layer is 15g/m 2 In the coating process, a release film is paved below the fiber in order to prevent glue leakage from sticking to the roller.
Selecting a doctor blade coating mode, firstly coating helium-resistant coating liquid SC-1 of LeKai on the surface of a buffer layer of the fiber fabric, wherein the curing condition is 85 ℃ for 3min, and the coating sizing amount is 10g/m 2 The method comprises the steps of carrying out a first treatment on the surface of the After the helium-resistant coating is finished, coating a fluorocarbon resin coating, wherein the curing condition is 95 ℃ for 3min, and the coating sizing amount is 10g/m 2 After the completion, the capsule material is obtained, and the surface density is 150g/m 2 。
Comparative example 1
Preparation of polyurethane composition:
150 parts by weight of a polyether type thermoplastic elastomer (molecular weight: 150000), 425 parts by weight of butanone and 425 parts by weight of ethyl acetate were mixed and stirred sufficiently at 80℃until dissolved, to obtain a polyurethane composition solution APP-04.
Preparation of a capsule material:
the surface density is selected to be 105g/m 2 The Vectran fiber fabric is coated with a heat sealing layer and a buffer layer on two sides of the fiber fabric respectively by using a polyurethane composition solution APP-01 in a slit coating mode, wherein the sizing amount of the heat sealing layer is 37g/m 2 The sizing amount of the buffer layer is 8g/m 2 In the coating process, a release film is paved below the fiber in order to prevent glue leakage from sticking to the roller.
Selecting a doctor blade coating mode, firstly coating liquid SC-1 with LeKai heliumCoating helium-resistant coating on the surface of the buffer layer of the fiber fabric, wherein the curing condition is 100 ℃, the curing time is 3min, and the coating sizing amount is 5g/m 2 The method comprises the steps of carrying out a first treatment on the surface of the After the helium-resistant coating is finished, coating a fluorocarbon resin coating, wherein the curing condition is 110 ℃ for 3min, and the coating sizing amount is 10g/m 2 After the completion, the capsule material is obtained, and the surface density is 165g/m 2 。
Comparative example 2
Preparation of polyurethane composition:
63.38 parts by mass of a polyether type thermoplastic elastomer (molecular weight: 150000), 600 parts by mass of methyl ethyl ketone and 300 parts by mass of ethyl acetate were mixed and stirred sufficiently at 80℃until dissolved, to obtain a-2 liquid.
After the solution A-2 is restored to room temperature, 31.69 parts by mass of isocyanate-terminated polyurethane prepolymer, 0.58 part by mass of chain extender 1, 4-butanediol, 0.95 part by mass of grafting agent propyl methacrylate triethoxysilane and 0.02 part by mass of initiator azo diisobutyl cyanide are sequentially added into the solution A-2; and after uniformly stirring, heating to 80 ℃, and continuously and rapidly stirring to obtain polyurethane composition solution APP-05.
Preparation of a capsule material:
the surface density is selected to be 105g/m 2 The Vectran fiber fabric is coated with a heat sealing layer and a buffer layer on two sides of the fiber fabric respectively by using a polyurethane composition solution APP-01 in a slit coating mode, wherein the sizing amount of the heat sealing layer is 37g/m 2 The sizing amount of the buffer layer is 8g/m 2 In the coating process, a release film is paved below the fiber in order to prevent glue leakage from sticking to the roller.
Selecting a doctor blade coating mode, firstly coating a helium-resistant coating on the surface of a buffer layer of the fiber fabric by using a LeKai helium-resistant coating liquid SC-1, wherein the curing condition is 100 ℃, the curing time is 3min, and the coating sizing amount is 5g/m 2 The method comprises the steps of carrying out a first treatment on the surface of the After the helium-resistant coating is finished, coating a fluorocarbon resin coating, wherein the curing condition is 110 ℃ for 3min, and the coating sizing amount is 10g/m 2 After the completion, the capsule material is obtained, and the surface density is 165g/m 2
Comparative example 3
The polyurethane composition formula:
63.38 parts by mass of a polyether type thermoplastic elastomer (molecular weight: 150000), 600 parts by mass of methyl ethyl ketone and 300 parts by mass of ethyl acetate were mixed and stirred sufficiently at 80℃until dissolved, to obtain a-2 liquid.
After the solution A-2 is restored to room temperature, 0.32 mass part of coupling agent gamma-aminopropyl triethoxysilane and 3.17 mass parts of inorganic nano particle titanium dioxide are sequentially added, the rotating speed is set to 3500 revolutions per minute on a high-shear emulsifying machine, and impurities are filtered after the solution A-2 is rapidly dispersed for 1 hour, so that polyurethane composition solution APP-06 is obtained.
Preparation of a capsule material:
the surface density is selected to be 105g/m 2 The Vectran fiber fabric is coated with a heat sealing layer and a buffer layer on two sides of the fiber fabric respectively by using a polyurethane composition solution APP-01 in a slit coating mode, wherein the sizing amount of the heat sealing layer is 37g/m 2 The sizing amount of the buffer layer is 8g/m 2 In the coating process, a release film is paved below the fiber in order to prevent glue leakage from sticking to the roller.
Selecting a doctor blade coating mode, firstly coating a helium-resistant coating on the surface of a buffer layer of the fiber fabric by using a LeKai helium-resistant coating liquid SC-1, wherein the curing condition is 100 ℃, the curing time is 3min, and the coating sizing amount is 5g/m 2 The method comprises the steps of carrying out a first treatment on the surface of the After the helium-resistant coating is finished, coating a fluorocarbon resin coating, wherein the curing condition is 110 ℃ for 3min, and the coating sizing amount is 10g/m 2 After the completion, the capsule material is obtained, and the surface density is 165g/m 2 。
The overall properties of the polyurethane compositions prepared according to the invention were examined in the examples and comparative examples above, respectively, in combination with the performance tests of the prepared capsule materials.
(1) Performance testing of capsule materials
According to the basic requirements of the stratospheric airship on the capsule material, the tensile strength, the tearing strength and the helium resistance of the capsule material are respectively tested according to relevant standards, and the details are shown in table 1.
(2) Test of kneading Performance of Capsule Material
According to the kneading performance requirements of the stratospheric airship on the capsule material, the capsule material is cut into A4 sample pieces, kneaded on a kneader, and then the strength and helium permeability of the kneaded tensile sample strips are tested, and are shown in Table 2.
(3) High temperature resistance test of capsule material
According to the basic requirements of the stratospheric airship on the capsule material, cutting the capsule material into test bars, placing the test bars into a temperature-controlled tensile machine, and preserving the temperature for 10 minutes at 85 ℃ for tensile strength performance test, wherein the tensile strength performance test is shown in Table 3.
(4) Testing of welding Properties of balloon Material
According to the basic requirements of the stratospheric airship on the welding performance of the capsule body material, the preparation of a welding belt is carried out according to the figure 2, wherein the inner welding belt is the main material of the capsule body material, the sealing belt is a pressure-sensitive adhesive belt with weather resistance, the normal temperature performance test and the high temperature resistance performance test are respectively carried out, the high temperature resistance performance test is carried out, the prepared welding spline is placed in a temperature control tensile machine for heat preservation for 10min at 85 ℃, and the tensile strength performance test is carried out, and is shown in Table 4 in detail.
Method of performance testing of the above examples and comparative examples:
1. areal density testing
According to the national standard GB/T4669-2008 'determination of mass per unit length and mass per unit area of textile woven fabrics'.
2. Tensile Strength test
The measurement was performed according to the American Standard FED-STD-191A 5102.
3. Tear Strength test
The determination was performed according to U.S. standard MIL-C-21189Para 10.2.4.
4. Peel force test
According to the national standard GB/T8808-1988, method for peel test of Soft composite plastics materials.
5. Helium permeability
According to the national standard GB/T1038-2000 "differential pressure method for testing gas permeability of Plastic films and sheets".
TABLE 1
TABLE 2
TABLE 3 Table 3
TABLE 4 Table 4
As can be seen from tables 1, 2 and 3, when the polyurethane compositions prepared in examples 1 to 6 of the present invention were used as the buffer layer and the heat-sealing layer, the adhesion property between the functional layers was good, and excellent tensile strength, tear strength and helium resistance were exhibited, and even though the capsule material was rubbed 200 times, the attenuation rate of the tensile strength was still less than 2%, and the helium permeability was not significantly deteriorated, and the attenuation rate of the tensile strength was less than 15% at a high temperature of 85 ℃, whereas the attenuation rate of the tensile strength after 200 times of rubbing was 20% -35% for the capsule material prepared in comparative examples 1 to 3, and the attenuation rate of the tensile strength was more than 37% at a temperature of 85 ℃, which indicates that the rubbing resistance and the temperature resistance of the present material of the capsule material prepared in the present invention were significantly improved.
As is clear from Table 4, the polyurethane compositions prepared in examples 1 to 6 of the present invention exhibited excellent weldability when used as a heat-sealing layer, even when tested for tensile strength at a high temperature of 85 ℃, the tensile bars were all broken at the present material, no peeling at the welded portion occurred, and the welded portion was good in sealing property; the heat-seal layers prepared in comparative examples 1 to 3 were remarkably inferior in heat resistance, and the welded portion was peeled off at a high temperature of 85℃and inferior in sealing property.
In the description of the present specification, a description referring to terms "one embodiment," "some embodiments," "examples," "specific examples," or "some examples," etc., means that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the present invention. In this specification, schematic representations of the above terms are not necessarily directed to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples. Furthermore, the different embodiments or examples described in this specification and the features of the different embodiments or examples may be combined and combined by those skilled in the art without contradiction.
While embodiments of the present invention have been shown and described above, it will be understood that the above embodiments are illustrative and not to be construed as limiting the invention, and that variations, modifications, alternatives and variations may be made to the above embodiments by one of ordinary skill in the art within the scope of the invention.

Claims (8)

1. A polyurethane composition for a bladder material comprising: 10-40 parts by weight of a thermoplastic polyurethane elastomer, 5-20 parts by weight of a polyurethane prepolymer, 0.1-1.5 parts by weight of a chain extender, 0.3-2.5 parts by weight of a grafting agent, 0.01-0.5 parts by weight of an initiator, 0.5-10 parts by weight of a coupling agent, 0.5-5 parts by weight of inorganic nanoparticles and 60-300 parts by weight of a solvent;
the mass ratio of the polyurethane prepolymer to the thermoplastic polyurethane elastomer is 1/8~1/2;
the mass ratio of the inorganic nano particles to the thermoplastic polyurethane elastomer is 1/80-1/20;
the solvent is a mixture solvent of butanone and ethyl acetate, wherein the mass ratio of the butanone to the ethyl acetate is 10/1-1/5; the solid content of the polyurethane composition is 5% -20%;
the molecular weight of the thermoplastic polyurethane elastomer is 50000-250000;
The grafting agent is a multifunctional compound with a conjugated double bond structure;
the polyurethane prepolymer is at least one of isocyanate-terminated polyurethane prepolymer, hydroxyl-terminated polyurethane prepolymer, polyurethane prepolymer containing a blocking group, silane-terminated polyurethane prepolymer and alkyl acrylate-terminated polyurethane prepolymer.
2. The polyurethane composition for a bladder material according to claim 1, wherein the thermoplastic polyurethane elastomer is selected from at least one of a polycarbonate-type polyurethane elastomer, a polyolefin-type polyurethane elastomer, a polyether-type polyurethane elastomer, and a polyester-type polyurethane elastomer.
3. The polyurethane composition for a capsule material according to claim 1, wherein the inorganic nanoparticles are selected from at least one of nano titanium dioxide, nano zinc oxide, nano aluminum oxide, nano silicon oxide, graphene, carbon nanotubes, mica, and montmorillonite; the particle size of the inorganic nano particles is 10 nm-100 nm.
4. A process for preparing a polyurethane composition for a bladder material as claimed in claim 1, comprising:
(1) Mixing and stirring a thermoplastic polyurethane elastomer, a polyurethane prepolymer, a chain extender, a grafting agent, an initiator and a solvent to obtain a mixed solution B;
Step (1) further comprises the following steps:
(1-1) mixing the thermoplastic polyurethane elastomer and the solvent, and stirring to obtain a mixed liquid A;
(1-2) mixing the mixed solution a, the polyurethane prepolymer, the chain extender, the grafting agent and the initiator, and stirring to obtain a mixed solution B;
(2) The mixed liquid B, the coupling agent and the inorganic nano particles are mixed and dispersed on a high shear emulsifying machine so as to obtain a polyurethane composition C.
5. The capsule material is characterized by comprising a weather-resistant layer, a helium-blocking layer and a functional integrated bearing layer which are sequentially laminated; the functional integrated bearing layer comprises a buffer layer, a fiber fabric and a heat sealing layer which are sequentially laminated; the buffer layer and the heat-sealing layer are prepared by using the polyurethane composition as the raw material in claim 1.
6. The bladder material according to claim 5 wherein the fiber fabric is selected from one of Vectran fiber fabric, polyimide fiber fabric, poly-p-phenylene bisoxazole fiber fabric, and ultra-high molecular weight polyethylene fiber fabric.
7. A method of preparing the capsule material of claim 5, comprising:
(a) Preparing a polyurethane composition C according to the process of claim 4;
(b) Respectively coating the polyurethane composition C on two sides of the fiber fabric, and curing to obtain a heat sealing layer and a buffer layer;
(c) Sequentially coating a helium blocking layer and a weather-resistant layer on the surface of the buffer layer, which is far away from the fiber fabric, and curing to obtain a capsule material;
in the step (b), the curing temperature is 30-100 ℃;
in the step (c), the curing temperature is 75-120 ℃.
8. A flying device comprising the capsule material of claim 5 or the capsule material produced by the method of claim 7.
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