CN113307994B - TPU film with high elasticity and high moisture permeability and preparation method thereof - Google Patents

TPU film with high elasticity and high moisture permeability and preparation method thereof Download PDF

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CN113307994B
CN113307994B CN202110482734.8A CN202110482734A CN113307994B CN 113307994 B CN113307994 B CN 113307994B CN 202110482734 A CN202110482734 A CN 202110482734A CN 113307994 B CN113307994 B CN 113307994B
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tpu film
parts
tpu
weight
elasticity
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CN113307994A (en
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何建雄
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Suzhou Xionglin New Material Science & Technology Co ltd
Dongguan Xionglin New Materials Technology Co Ltd
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Suzhou Xionglin New Material Science & Technology Co ltd
Dongguan Xionglin New Materials Technology Co Ltd
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    • C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
    • C08J5/18—Manufacture of films or sheets
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    • C08G18/00—Polymeric products of isocyanates or isothiocyanates
    • C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
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    • C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
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    • C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
    • C08J9/04—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent
    • C08J9/12—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a physical blowing agent
    • C08J9/14—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a physical blowing agent organic
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    • C08J2375/00—Characterised by the use of polyureas or polyurethanes; Derivatives of such polymers
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Abstract

The invention provides a high-elasticity and high-moisture permeability TPU film and a preparation method thereof, wherein the preparation raw materials of the TPU film comprise a combination of perfluoropolyether dihydric alcohol, aliphatic diisocyanate, a chain extender, a catalyst, polystyrene, foaming silicone master batch, an abrasion-resistant additive and an anti-UV agent; the TPU is generated by adopting specific parts of perfluoropolyether glycol, aliphatic diisocyanate and chain extender under the condition of a catalyst, and the specific parts of polystyrene added in the preparation raw materials are matched, so that the moisture permeability of the finally obtained TPU film is enhanced; and the foaming silicone master batch is added into the preparation raw material, so that the elasticity of the TPU film is enhanced, and finally, the TPU film with excellent elasticity and moisture permeability is obtained, and the method has important research significance.

Description

TPU film with high elasticity and high moisture permeability and preparation method thereof
Technical Field
The invention belongs to the technical field of composite materials, and particularly relates to a TPU film with high elasticity and high moisture permeability and a preparation method thereof.
Background
TPU materials are increasingly popular because of their excellent properties and environmental protection, not only have excellent high tension, toughness and aging resistance, but also are environmentally friendly materials that are mature, and at present, TPU has been widely used: shoe materials, ready-made clothes, inflatable toys, sports equipment on water and under water, medical equipment, fitness equipment, automobile seat materials, umbrellas, leather cases, leather bags and the like.
The Thermoplastic Polyurethane (TPU) material is mainly divided into a polyester type TPU material and a polyether type TPU material, wherein the halogen-free flame retardant TPU material can also replace soft PVC to meet the environmental protection requirements of more and more fields. TPU elastomers are a relatively special class of elastomers, and have a wide hardness range and a wide performance range, so that TPU elastomers are high molecular materials which are intermediate to rubber and plastic, can be heated and plasticized, have no or little crosslinking in chemical structure, have basically linear molecules, and have certain physical crosslinking. Therefore, the elasticity of the TPU material is not particularly desirable. CN109401281a discloses a high-elastic TPU film and a preparation method thereof, the preparation method of the high-elastic TPU film comprises the steps of mixing the prepared TPU particles, the foaming silicone master batch and the modified nano silicon dioxide master batch according to a proportion in three stages, then sending the mixture into a casting machine through an automatic feeding system, and extruding the mixture to form the film. The TPU film provided by the invention has high elasticity, and can be widely applied to the fields of shock absorption materials, packaging toys, children toys, sports goods, aviation models, heat preservation and insulation materials, automobile interior trim materials and the like. However, the product produced by the TPU material obtained by the patent has low moisture permeability, and can not quickly discharge sweat emitted by a human body in hot weather so as to provide dry and comfortable feeling for the skin.
CN107043531a discloses a TPU film with good moisture permeability, comprising the following materials: perfluoropolyether glycol, chain extender, aliphatic diisocyanate, TPO resin, color master batch, antioxidant, light stabilizer, anti-yellowing agent, erucamide, oleamide and stearic acid. The preparation method of the TPU film comprises the following steps: 1) Preparing fluorine-containing TPU; 2) Uniformly stirring fluorine-containing TPU, TPO resin, color master batch, antioxidant, anti-yellowing agent, erucic acid amide, oleic acid amide and stearic acid; 3) And (2) adding the materials obtained in the step (2) into an internal mixer for banburying for 5-10 minutes, and extruding by an extruder. CN112497877a discloses a waterproof moisture permeable composite TPU film, which comprises the following raw materials in parts by weight: the material comprises the following raw materials in parts by weight: thermoplastic polyurethane: 100-120 parts; 50-70 parts of polystyrene; 40-60 parts of polyisobutene; 50-60 parts of dimethyl terephthalate; 50-60 parts of ethylene glycol; 10-20 parts of a catalyst; 30-40 parts of polypropylene; 50-60 parts of triethanolamine; 3-5 parts of azodiisobutyl cyanide; 10-20 parts of methanol; 25-35 parts of polytetrafluoroethylene; 5-9 parts of curing agent; and (3) adding the rest water into a reaction kettle according to the steps to react. The invention can realize the composite TPU film integrating moisture permeability and waterproof performance, and the material layer A in the composite TPU film can lead the composite TPU film to have higher strength, durability and chemical corrosion resistance, however, the moisture permeability of the TPU film prepared by the two patents is still to be improved, and the elasticity is poor.
Therefore, developing a TPU film with both excellent elasticity and moisture permeability is a technical problem that needs to be solved by those skilled in the art.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a high-elasticity and high-moisture-permeability TPU film and a preparation method thereof, wherein the preparation raw materials of the high-elasticity and high-moisture-permeability TPU film comprise specific parts of perfluoropolyether dihydric alcohol and aliphatic diisocyanate, and specific parts of polystyrene are added in a matching way, so that the moisture permeability of the prepared TPU film is enhanced; the foaming silicone master batch with the characteristic parts is added into the preparation raw materials, so that the elasticity of the TPU film is enhanced, and finally the TPU film with excellent elasticity and moisture permeability is obtained, and the foaming silicone master batch has important research significance.
In order to achieve the aim of the invention, the invention adopts the following technical scheme:
in a first aspect, the invention provides a high-elasticity and high-moisture permeability TPU film, which is prepared from the following raw materials in parts by weight:
Figure BDA0003049857410000031
the perfluoropolyether diol may be 33, 36, 39, 43, 46, 49, 53, 56, or 59 parts by weight, and specific point values between the above are limited in length and for brevity, and the invention is not intended to be exhaustive of the specific point values included in the range.
The aliphatic diisocyanate may be 53 parts by weight, 56 parts by weight, 59 parts by weight, 63 parts by weight, 66 parts by weight, 69 parts by weight, 73 parts by weight, 76 parts by weight or 79 parts by weight, and specific point values between the above point values are limited in length and for the sake of brevity, the present invention is not exhaustive of the specific point values included in the range.
The chain extender may be 10.5 parts by weight, 11 parts by weight, 11.5 parts by weight, 12 parts by weight, 12.5 parts by weight, 13 parts by weight, 13.5 parts by weight, 14 parts by weight or 14.5 parts by weight, and specific point values between the above point values, are limited in length and for brevity, the invention is not intended to be exhaustive list of the specific point values included in the range.
The catalyst may be 3 parts by weight, 4 parts by weight, 5 parts by weight, 6 parts by weight, 7 parts by weight, 8 parts by weight or 9 parts by weight, and specific point values between the above point values, are for the sake of brevity and for the sake of brevity, the present invention is not intended to exhaustively list the specific point values included in the range.
The polystyrene may be 17 parts by weight, 19 parts by weight, 21 parts by weight, 23 parts by weight, 25 parts by weight, 27 parts by weight or 29 parts by weight, and specific point values between the above point values, are for brevity and for simplicity, the present invention is not intended to be exhaustive of the specific point values included in the range.
The foaming silicone master batch may be 1.2 parts by weight, 1.4 parts by weight, 1.6 parts by weight, 1.8 parts by weight, 2 parts by weight, 2.2 parts by weight, 2.4 parts by weight, 2.6 parts by weight or 2.8 parts by weight, and specific point values between the above point values, are limited in length and for brevity, the present invention is not exhaustive of the specific point values included in the range.
The wear additive may be 5.5 parts by weight, 6 parts by weight, 6.5 parts by weight, 7 parts by weight, 7.5 parts by weight, 8 parts by weight, 8.5 parts by weight, 9 parts by weight or 9.5 parts by weight, and specific point values between the above point values, are limited in length and for brevity, the invention is not intended to be exhaustive list of the specific point values included in the range.
The UV resistant agent may be 1.5 parts by weight, 2 parts by weight, 2.5 parts by weight, 3 parts by weight, 3.5 parts by weight, 4 parts by weight or 4.5 parts by weight, and specific point values between the above point values, are limited in length and for brevity, the present invention is not intended to exhaustively list the specific point values included in the range.
On one hand, the high-elasticity and high-moisture-permeability TPU film is used for preparing the TPU material by selecting the perfluoropolyether dihydric alcohol and the aliphatic diisocyanate in the preparation raw materials under the condition of a catalyst, polar groups are introduced into TPU molecules, and the hydrophilicity of the prepared TPU material is improved; and furthermore, a specific part of polystyrene is added into the preparation raw material of the TPU film, and the molecular structure design and the selection of an auxiliary agent are adopted by the coordination of the inside and the outside of the molecule, so that the hydrophilicity of the TPU film is further improved, water molecules can be adsorbed in a high-humidity environment, and the water molecules can be transferred to a low-humidity environment for desorption through chain segment movement.
On the other hand, because the TPU material is a high molecular material between rubber and plastic, the TPU material can be heated and plasticized, and has no or little crosslinking on chemical structure, and the molecules of the TPU material are basically linear, so the elasticity is poor.
The invention provides a TPU film with high elasticity and high moisture permeability, wherein the high elasticity refers to a TPU film with 100% stretching recovery rate of not less than 90%; "high moisture permeability" means the mass of water vapor passing through a unit area of a sample per unit time under prescribed temperature conditions, that is, a moisture permeability of not less than 9050g/m 2 24h TPU film.
Preferably, the aliphatic diisocyanate comprises any one or a combination of at least two of hexamethylene diisocyanate, isophorone diisocyanate, dicyclohexylmethane-4, 4' -diisocyanate, tetramethylxylylene diisocyanate, xylylene diisocyanate or methylcyclohexane diisocyanate.
Preferably, the chain extender comprises 1,4 butanediol.
Preferably, the catalyst comprises an organotin catalyst, and one or a combination of at least two of CT-E229, stannous octoate and dibutyltin dilaurate may be selected.
Preferably, the polystyrene has a particle size of 200 to 300 mesh, such as 210 mesh, 220 mesh, 230 mesh, 240 mesh, 250 mesh, 260 mesh, 270 mesh, 280 mesh or 290 mesh, and specific point values between the above point values, which are limited in space and for the sake of brevity, the present invention is not intended to be exhaustive of the specific point values included in the range.
As a preferable technical scheme of the invention, the TPU film prepared when the particle size of the polystyrene provided by the invention is 200-300 meshes has excellent elasticity and moisture absorption performance; on the one hand, if the particle size of the polystyrene is smaller than 200 meshes, the polystyrene is easy to agglomerate, and the elasticity and hygroscopicity of the TPU film are affected; on the other hand, if the particle size of the polystyrene is more than 300 mesh, the particle size is excessively large, affecting the hygroscopicity of the TPU film.
Preferably, the preparation raw materials of the foaming silicone master batch comprise the following components in parts by weight:
90-100 parts by weight of TPU particles;
2-10 parts by weight of a foaming agent;
80-90 parts of silicone powder.
The TPU particles may be 91 parts by weight, 92 parts by weight, 93 parts by weight, 94 parts by weight, 95 parts by weight, 96 parts by weight, 97 parts by weight, 98 parts by weight or 99 parts by weight, and specific point values between the above point values, are for brevity and for brevity the invention is not intended to be exhaustive.
Preferably, the mass ratio of TPU particles to silicone powder is 1 (0.8-1.2), such as 1:0.85, 1:0.9, 1:0.95, 1:1, 1:1.05, 1:1.1 or 1:1.15, etc.
Preferably, the blowing agent comprises any one or a combination of at least two of carbon dioxide, nitrogen, propane, n-butane, isobutane, n-pentane or isopentane.
Preferably, the foaming silicone master batch is prepared by a method comprising: and mixing TPU particles, a foaming agent and silicone powder, and extruding to obtain the foaming silicone master batch.
Preferably, the wear resistant additive comprises any one or a combination of at least two of polytetrafluoroethylene fibers, molybdenum disulfide, graphite or polyimide fibers, more preferably polytetrafluoroethylene fibers and/or polyimide fibers.
Preferably, the anti-UV agent comprises any one or a combination of at least two of salicylate-based anti-UV agents, benzophenone-based anti-UV agents, benzotriazole-based anti-UV agents, substituted acrylonitrile-based anti-UV agents, triazine-based anti-UV agents or hindered amine-based anti-UV agents.
Preferably, the preparation raw materials of the high-elasticity and high-moisture-penetrability TPU film also comprise any one or a combination of at least two of an antioxidant, a lubricant and a pigment.
Preferably, the antioxidant comprises pentaerythritol tetrakis [ beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate ].
Preferably, the high elasticity, high moisture permeability TPU film is prepared from the antioxidant in an amount of 1 to 5 parts by weight, for example, 1.5 parts by weight, 2 parts by weight, 2.5 parts by weight, 3 parts by weight, 3.5 parts by weight, 4 parts by weight, or 4.5 parts by weight, and specific point values between the above point values, are limited in scope and for brevity, the invention is not exhaustive of the specific point values included in the ranges.
Preferably, the high elasticity, high moisture permeability TPU film is prepared from the starting materials having a slip agent content of 0.5 to 2 parts by weight, for example 0.7 parts by weight, 0.9 parts by weight, 1.1 parts by weight, 1.3 parts by weight, 1.5 parts by weight, 1.7 parts by weight or 1.9 parts by weight, and specific point values between the above point values, which are limited in length and for brevity, the present invention is not exhaustive list of the specific point values included in the range.
Preferably, the slip agent comprises any one or a combination of at least two of erucamide, oleamide, C wax or montan wax.
Preferably, the high elasticity, high moisture vapor permeation TPU film is prepared with a pigment content of from 0.5 to 2 parts by weight, for example, 0.7 parts by weight, 0.9 parts by weight, 1.1 parts by weight, 1.3 parts by weight, 1.5 parts by weight, 1.7 parts by weight or 1.9 parts by weight, and specific point values between the above point values, which are limited in length and for brevity, the invention is not intended to be exhaustive.
Preferably, the pigment comprises any one or a combination of at least two of phthalocyanine red, phthalocyanine blue, phthalocyanine green, sun-fast scarlet, macromolecular red, macromolecular yellow, permanent violet or azo red.
In a second aspect, the present invention provides a process for preparing a high elasticity, high moisture vapor transmission TPU film according to the first aspect, said process comprising the steps of:
(1) Reacting perfluoropolyether dihydric alcohol, aliphatic diisocyanate and a catalyst to obtain a prepolymer;
(2) Reacting the prepolymer obtained in the step (1) with a chain extender, and extruding to obtain TPU resin;
(3) And (3) carrying out melt extrusion, cooling and stretching on the TPU resin, the polystyrene, the foaming silicone master batch, the wear-resistant additive, the UV resistant agent, the optional antioxidant, the optional slipping agent and the optional pigment obtained in the step (2) to obtain the high-elasticity and high-moisture permeability TPU film.
Preferably, the temperature of the reaction described in step (1) is 70 to 80 ℃, such as 71 ℃, 72 ℃, 73 ℃, 74 ℃, 75 ℃, 76 ℃, 77 ℃, 78 ℃ or 79 ℃, and specific point values between the above point values, limited in space and for the sake of brevity, the invention is not exhaustive of the specific point values comprised in the range.
Preferably, the reaction time in step (1) is 2 to 3 hours, such as 2.1 hours, 2.2 hours, 2.3 hours, 2.4 hours, 2.5 hours, 2.6 hours, 2.7 hours, 2.8 hours or 2.9 hours, and the specific point values between the above point values, are limited in space and for reasons of brevity the invention is not exhaustive of the specific point values comprised in the range.
Preferably, the temperature of the reaction in step (2) is 40 to 60 ℃, such as 42 ℃, 44 ℃, 46 ℃, 48 ℃, 50 ℃, 52 ℃, 54 ℃, 56 ℃ or 58 ℃, and specific point values between the above point values, limited in space and for the sake of brevity, the invention is not exhaustive of the specific point values comprised in the range.
Preferably, the reaction time in step (2) is from 6 to 12 hours, such as 6.5 hours, 7 hours, 7.5 hours, 8 hours, 8.5 hours, 9 hours, 9.5 hours, 10 hours, 10.5 hours, 11 hours or 11.5 hours, and the specific point values between the above point values, are limited in space and for reasons of brevity the invention is not exhaustive of the specific point values comprised in the range.
Preferably, the melt extrusion temperature in step (3) is 170 to 200 ℃, such as 173 ℃, 176 ℃, 179 ℃, 183 ℃, 186 ℃, 189 ℃, 193 ℃, 196 ℃, or 199 ℃, and specific point values between the above point values, limited in space and for brevity, the invention is not exhaustive of the specific point values comprised in the range.
Preferably, the pressure of the melt extrusion in step (3) is 10-20 Mpa, for example 11Mpa, 12Mpa, 13Mpa, 14Mpa, 15Mpa, 16Mpa, 17Mpa, 18Mpa or 19Mpa, and the specific values between the above values are limited in length and for the sake of brevity the invention is not intended to be exhaustive.
Preferably, the melt extrusion of step (3) is performed by a single screw extruder.
Preferably, the single screw extruder is rotated at 20 to 100rpm, such as 25rpm, 30rpm, 35rpm, 40rpm, 45rpm, 50rpm, 60rpm, 70rpm, 80rpm or 90rpm, and specific point values between the above point values, are limited in space and for the sake of brevity, the present invention is not exhaustive of the specific point values included in the ranges.
As a preferable technical scheme, the preparation method comprises the following steps:
(1) Reacting perfluoropolyether dihydric alcohol, aliphatic diisocyanate and a catalyst at 70-80 ℃ for 2-3 hours to obtain a prepolymer;
(2) Reacting the prepolymer obtained in the step (1) with a chain extender at 40-60 ℃ for 6-12 hours, and extruding to obtain TPU resin;
(3) And (3) carrying out melt extrusion, cooling and stretching on the TPU resin, the polystyrene, the foaming silicone master batch, the wear-resistant additive, the UV resistant agent, the optional antioxidant, the optional slipping agent and the optional pigment obtained in the step (2) at 170-200 ℃ by a single screw extruder with the rotating speed of 20-100 rpm to obtain the high-elasticity and high-moisture permeability TPU film.
Compared with the prior art, the invention has the following beneficial effects:
according to the high-elasticity and high-moisture-permeability TPU film, a TPU material is generated by adopting specific parts of perfluoropolyether dihydric alcohol, aliphatic diisocyanate and a chain extender under the condition of a catalyst, and polar groups are introduced into the TPU molecular chain to improve the hydrophilicity of the TPU film; the specific parts of polystyrene added in the preparation raw materials are matched, so that the moisture permeability of the TPU film is further enhanced; the foaming silicone master batch with the characteristic parts is further added into the preparation raw materials, so that the elasticity of the TPU film is enhanced, and finally the TPU film with excellent elasticity and moisture permeability is obtained; specifically, the moisture permeability of the TPU film provided by the invention is 9050-10500 g/m < 2 >. 24h; the recovery rate of 100% stretching is 90-98%; the elongation at break is 468-490%, which completely meets the market requirement and has important research significance.
Detailed Description
The technical scheme of the invention is further described by the following specific embodiments. It will be apparent to those skilled in the art that the examples are merely to aid in understanding the invention and are not to be construed as a specific limitation thereof.
Preparation example 1
The foaming silicone master batch comprises the following components in parts by weight:
95 parts by weight of TPU particles;
5 parts by weight of a foaming agent;
85 parts by weight of silicone powder;
the preparation method comprises the following steps: TPU particles (S90A), a foaming agent (ethanol) and silicone powder are mixed and extruded at 180 ℃ to obtain the foaming silicone master batch.
Preparation example 2
The foaming silicone master batch comprises the following components in parts by weight:
90 parts by weight of TPU particles;
2 parts by weight of a foaming agent;
80 parts by weight of silicone powder;
the preparation method comprises the following steps: TPU particles (S90A), a foaming agent (ethanol) and silicone powder are mixed and extruded at 180 ℃ to obtain the foaming silicone master batch.
Preparation example 3
The foaming silicone master batch comprises the following components in parts by weight:
100 parts by weight of TPU particles;
2 parts by weight of a foaming agent;
90 parts by weight of silicone powder;
the preparation method comprises the following steps: TPU particles (S90A), a foaming agent (ethanol) and silicone powder are mixed and extruded at 180 ℃ to obtain the foaming silicone master batch.
Preparation example 4
The foaming silicone master batch differs from preparation example 1 only in that the addition amount of TPU particles is 110 parts by weight, the addition amount of silicone powder is 70 parts by weight, and other components, amounts and preparation methods are the same as those of preparation example 1.
Preparation example 5
The foaming silicone master batch differs from preparation example 1 only in that the addition amount of TPU particles is 80 parts by weight, the addition amount of silicone powder is 100 parts by weight, and other components, amounts and preparation methods are the same as those of preparation example 1.
Comparative preparation example 1
A silicone master batch was different from that of preparation example 1 in that no foaming agent was added, and other components, amounts and preparation methods were the same as those of preparation example 1.
Example 1
The TPU film with high elasticity and high moisture permeability is prepared from the following raw materials in parts by weight:
Figure BDA0003049857410000111
Figure BDA0003049857410000121
the preparation method of the TPU film with high elasticity and high moisture permeability provided by the embodiment comprises the following steps:
(1) Reacting perfluoropolyether glycol (Dow chemical), isophorone diisocyanate and a catalyst (CT-E229) at 75 ℃ for 2.5 hours to obtain a prepolymer;
(2) Reacting the prepolymer obtained in the step (1) with 1,4 butanediol at 50 ℃ for 10.5 hours, and extruding to obtain TPU resin;
(3) And (3) melting, extruding, cooling and stretching the TPU resin obtained in the step (2), polystyrene (HIPS 622P of Shanghai Saicaceae, 200 meshes), foaming silicone master batch (preparation example 1), molybdenum disulfide, an anti-UV agent (UV-531), an antioxidant (antioxidant 1010), erucamide and pigment (phthalocyanine blue) at 180 ℃ through a single screw extruder with the rotating speed of 80rpm, so as to obtain the high-elasticity and high-moisture-permeability TPU film.
Example 2
The TPU film with high elasticity and high moisture permeability is prepared from the following raw materials in parts by weight:
Figure BDA0003049857410000122
Figure BDA0003049857410000131
the preparation method of the TPU film with high elasticity and high moisture permeability provided by the embodiment comprises the following steps:
(1) Reacting perfluoropolyether glycol (Dow chemical), isophorone diisocyanate and a catalyst (CT-E229) at 70 ℃ for 3 hours to obtain a prepolymer;
(2) Reacting the prepolymer obtained in the step (1) with 1, 4-butanediol at 40 ℃ for 12 hours, and extruding to obtain TPU resin;
(3) And (3) melting, extruding, cooling and stretching the TPU resin obtained in the step (2), polystyrene (HIPS 622P of Shanghai Saicaceae, 250 meshes), foaming silicone master batch (preparation example 2), molybdenum disulfide, an anti-UV agent (UV-531), an antioxidant (antioxidant 1010), erucamide and pigment (phthalocyanine blue) at 170 ℃ through a single screw extruder with the rotating speed of 100rpm, so as to obtain the high-elasticity and high-moisture-permeability TPU film.
Example 3
The TPU film with high elasticity and high moisture permeability is prepared from the following raw materials in parts by weight:
Figure BDA0003049857410000132
Figure BDA0003049857410000141
the preparation method of the TPU film with high elasticity and high moisture permeability provided by the embodiment comprises the following steps:
(1) Reacting perfluoropolyether glycol (Dow chemical), isophorone diisocyanate and a catalyst (CT-E229) at 80 ℃ for 2 hours to obtain a prepolymer;
(2) Reacting the prepolymer obtained in the step (1) with 1,4 butanediol at 60 ℃ for 6 hours, and extruding to obtain TPU resin;
(3) And (3) melting, extruding, cooling and stretching the TPU resin obtained in the step (2), polystyrene (HIPS 622P of Shanghai Saicaceae, 300 meshes), foaming silicone master batch (preparation example 3), molybdenum disulfide, an anti-UV agent (UV-531), an antioxidant (antioxidant 1010), erucamide and pigment (phthalocyanine blue) at 200 ℃ through a single screw extruder with the rotating speed of 20rpm, so as to obtain the high-elasticity and high-moisture-permeability TPU film.
Example 4
A high elasticity, high moisture permeability TPU film differs from example 1 only in that the expanded silicone masterbatch obtained in preparation example 4 is used instead of the expanded silicone masterbatch obtained in example 1, and other components, amounts and preparation methods are the same as in example 1.
Example 5
A high elasticity, high moisture permeability TPU film differs from example 1 only in that the expanded silicone masterbatch obtained in preparation example 5 is used instead of the expanded silicone masterbatch obtained in example 1, and other components, amounts and preparation methods are the same as in example 1.
Example 6
A high elasticity, high moisture permeability TPU film differs from example 1 only in that 100 mesh polystyrene is used instead of 200 mesh polystyrene in example 1, and the other components, amounts and preparation methods are the same as in example 1.
Example 7
A high elasticity, high moisture permeability TPU film differs from example 1 only in that 400 mesh polystyrene is used instead of 200 mesh polystyrene in example 1, and the other components, amounts and preparation methods are the same as in example 1.
Comparative example 1
A TPU film differs from example 1 only in that the silicone masterbatch obtained in comparative preparation 1 is used instead of the expanded silicone masterbatch obtained in example 1, and the other components, amounts and preparation methods are the same as in example 1.
Comparative example 2
A TPU film differs from example 1 only in that the perfluoropolyether diol of example 1 is replaced by a polyether polyol (GE 210), the other components, amounts and preparation methods being the same as in example 1.
Comparative example 3
A TPU film differing from example 1 only in that 10 parts by weight of polystyrene was added and 15 parts by weight of TPU particles (S90A) were additionally added, the other components, amounts and preparation methods being the same as in example 1.
Comparative example 4
A TPU film differing from example 1 only in that no expanded silicone master batch was added, 2 parts by weight of TPU particles (S90A) were additionally added, and the other components, amounts and preparation methods were the same as in example 1.
Performance test:
(1) Moisture permeability: testing according to the test method specified in GB/T2679.2-2015;
(2) Elongation at break and 100% elongation recovery: the test was performed according to the test method specified in GB/T528-2009.
The TPU films provided in examples 1-7 and comparative examples 1-4 were tested according to the test methods described above and the test results are shown in table 1:
TABLE 1
Moisture permeability (g/m) 2 ·24h) 100% recovery from permanent elongation (%) Elongation at break (%)
Example 1 10500 98 490
Example 2 10460 98 485
Example 3 10360 96 481
Example 4 9400 93 470
Example 5 9380 90 471
Example 6 9800 92 472
Example 7 9050 90 468
Comparative example 1 9800 80 435
Comparative example 2 2800 90 468
Comparative example 3 5840 92 470
Comparative example 4 7680 87 468
As can be seen from the data in table 1, the TPU film provided by the present invention has superior elasticity and moisture permeability.
Specifically, examples 1 to 7 provided TPU films having a moisture permeability of 9050 to 10500g/m 2 24h; the recovery rate of 100% stretching is 90-98%; the elongation at break is 468-490%.
As can be seen from comparative example 1, comparative example 1 and comparative example 4, the 100% elongation recovery and elongation at break of the TPU film obtained by replacing the expanded silicone masterbatch with the silicone masterbatch (comparative example 1) or directly without adding the expanded silicone masterbatch (comparative example 4) are both drastically reduced.
As can be seen from comparative examples 1 and 2, the use of conventional polyether polyols instead of perfluoropolyether diols for the preparation of TPU materials resulted in a significant reduction in the moisture permeability of the TPU film.
As can be seen from comparative examples 1 and 3, the moisture permeability of the TPU film obtained by excessively low addition amount of polystyrene in the preparation raw material is greatly reduced.
Further comparing example 1 with examples 4 to 5, it was found that the silicone powder and TPU particles in the raw materials for the preparation of the expanded silicone master batch were outside or below the specific ranges set in the present invention, and the obtained TPU film had a reduced moisture permeability, elongation at break and 100% elongation recovery.
Further comparing example 1 with examples 6 to 7, it was found that when the particle size of the polystyrene added in the raw material for preparation was not within the set range, the moisture permeability, elongation at break and 100% elongation recovery of the finally obtained TPU film were all reduced.
The applicant states that the present invention, by way of the above examples, illustrates a high elasticity, high moisture vapor transmission TPU film and method of making the same, but the present invention is not limited to the above process steps, i.e., it is not meant that the present invention must rely on the above process steps to be practiced. It should be apparent to those skilled in the art that any modification of the present invention, equivalent substitution of selected raw materials, addition of auxiliary components, selection of specific modes, etc. fall within the scope of the present invention and the scope of disclosure.

Claims (27)

1. The high-elasticity and high-moisture-permeability TPU film is characterized by comprising the following raw materials in parts by weight:
Figure FDA0004142854980000011
the particle size of the polystyrene is 200-300 meshes;
the preparation raw materials of the foaming silicone master batch comprise the following components in parts by weight:
90-100 parts by weight of TPU particles;
2-10 parts by weight of a foaming agent;
80-90 parts of silicone powder.
2. The high elasticity, high moisture vapor transmission TPU film of claim 1 wherein said aliphatic diisocyanate comprises any one or a combination of at least two of hexamethylene diisocyanate, isophorone diisocyanate, dicyclohexylmethane-4, 4' -diisocyanate, or methylcyclohexane diisocyanate.
3. The high elasticity, high moisture vapor transmission TPU film of claim 1 wherein said chain extender comprises 1, 4-butanediol.
4. The high elasticity, high moisture vapor transmission TPU film of claim 1 wherein said catalyst comprises an organotin catalyst.
5. The high elasticity, high moisture vapor permeability TPU film of claim 1 wherein said TPU particles and silicone powder are present in a mass ratio of 1 (0.8 to 0.9).
6. The high elasticity, high moisture vapor permeation TPU film of claim 1 wherein said blowing agent comprises any one or a combination of at least two of carbon dioxide, nitrogen, propane, n-butane, isobutane, n-pentane, or isopentane.
7. The high elasticity, high moisture vapor transmission TPU film of claim 1 wherein said expanded silicone masterbatch is prepared by a process comprising: and mixing TPU particles, a foaming agent and silicone powder, and extruding to obtain the foaming silicone master batch.
8. The high elasticity, high moisture vapor transmission TPU film of claim 1 wherein said abrasion resistant additive comprises any one or a combination of at least two of polytetrafluoroethylene fibers, molybdenum disulfide, graphite, or polyimide fibers.
9. The high elasticity, high moisture vapor transmission TPU film of claim 8 wherein said abrasion resistant additive is polytetrafluoroethylene fiber and/or polyimide fiber.
10. The high elasticity, high moisture vapor transmission TPU film of claim 1 wherein said UV resistant agent comprises any one or a combination of at least two of a salicylate-based UV resistant agent, a benzophenone-based UV resistant agent, a benzotriazole-based UV resistant agent, a substituted acrylonitrile-based UV resistant agent, a triazine-based UV resistant agent, or a hindered amine-based UV resistant agent.
11. The high elasticity, high moisture vapor transmission TPU film of claim 1 further comprising any one or a combination of at least two of an antioxidant, a slip agent, or a pigment.
12. The high elasticity, high moisture vapor transmission TPU film of claim 11 wherein said antioxidant comprises pentaerythritol tetrakis [ beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate ].
13. The high elasticity, high moisture vapor transmission TPU film of claim 11 wherein the antioxidant is present in the starting material for the preparation of the high elasticity, high moisture vapor transmission TPU film in an amount of 1 to 5 parts by weight.
14. The high elasticity, high moisture vapor transmission TPU film of claim 11 wherein said high elasticity, high moisture vapor transmission TPU film is prepared from a slip agent in an amount of 0.5 to 2 parts by weight.
15. The high elasticity, high moisture vapor transmission TPU film of claim 11 wherein said slip agent comprises any one or a combination of at least two of erucamide, oleamide, C wax, or montan wax.
16. The high elasticity, high moisture vapor transmission TPU film of claim 11 wherein said high elasticity, high moisture vapor transmission TPU film is prepared from pigment in an amount of 0.5 to 2 parts by weight.
17. The high elasticity, high moisture vapor transmission TPU film of claim 11 wherein said pigment comprises any one or a combination of at least two of phthalocyanine red, phthalocyanine blue, phthalocyanine green, sun fast scarlet, macromolecular red, macromolecular yellow, permanent violet, or azo red.
18. A process for the preparation of a high elasticity, high moisture vapor transmission TPU film according to any one of claims 1 to 17, comprising the steps of:
(1) Reacting perfluoropolyether dihydric alcohol, aliphatic diisocyanate and a catalyst to obtain a prepolymer;
(2) Reacting the prepolymer obtained in the step (1) with a chain extender, and extruding to obtain TPU resin;
(3) And (3) carrying out melt extrusion, cooling and stretching on the TPU resin, the polystyrene, the foaming silicone master batch, the wear-resistant additive, the UV resistant agent, the optional antioxidant, the optional slipping agent and the optional pigment obtained in the step (2) to obtain the high-elasticity and high-moisture permeability TPU film.
19. The process of claim 18, wherein the temperature of the reaction in step (1) is 70 to 80 ℃.
20. The method of claim 18, wherein the reaction time in step (1) is 2 to 3 hours.
21. The process of claim 18, wherein the temperature of the reaction in step (2) is 40-60 ℃.
22. The method of claim 18, wherein the reaction time in step (2) is from 6 to 12 hours.
23. The method of claim 18, wherein the melt extrusion in step (3) is performed at a temperature of 170 to 200 ℃.
24. The method according to claim 18, wherein the pressure of the melt extrusion in the step (3) is 10 to 20MPa.
25. The method of claim 18, wherein the melt extrusion of step (3) is performed by a single screw extruder.
26. The method of claim 25, wherein the single screw extruder is rotated at 20 to 100rpm.
27. The method of preparation according to claim 18, characterized in that the method of preparation comprises the steps of:
(1) Reacting perfluoropolyether dihydric alcohol, aliphatic diisocyanate and a catalyst at 70-80 ℃ for 2-3 hours to obtain a prepolymer;
(2) Reacting the prepolymer obtained in the step (1) with a chain extender at 40-60 ℃ for 6-12 hours, and extruding to obtain TPU resin;
(3) And (3) carrying out melt extrusion, cooling and stretching on the TPU resin, the polystyrene, the foaming silicone master batch, the wear-resistant additive, the UV resistant agent, the optional antioxidant, the optional slipping agent and the optional pigment obtained in the step (2) at 170-200 ℃ by a single screw extruder with the rotating speed of 20-100 rpm to obtain the high-elasticity and high-moisture permeability TPU film.
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