CN112358726A - Novel curtain coating coiling middle-permeation waterproof moisture-permeable TPU film - Google Patents
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
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- C08J2381/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing sulfur with or without nitrogen, oxygen, or carbon only; Polysulfones; Derivatives of such polymers
- C08J2381/06—Polysulfones; Polyethersulfones
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- C08J2409/00—Characterised by the use of homopolymers or copolymers of conjugated diene hydrocarbons
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- C08J2423/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
- C08J2423/02—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers not modified by chemical after treatment
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- C08J2427/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers
- C08J2427/02—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers not modified by chemical after-treatment
- C08J2427/12—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers not modified by chemical after-treatment containing fluorine atoms
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- C08J2475/00—Characterised by the use of polyureas or polyurethanes; Derivatives of such polymers
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- C08J2483/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen, or carbon only; Derivatives of such polymers
- C08J2483/04—Polysiloxanes
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Abstract
The invention discloses a novel cast winding intermediate-permeability waterproof moisture-permeable TPU film, which comprises the following raw materials in parts by weight: 20-40 parts of diphenylmethane diisocyanate, 10-20 parts of polytetrahydrofuran, 20-40 parts of butanediol, 10-15 parts of antioxidant, 10-15 parts of ethylene propylene diene monomer, 12-18 parts of methyl vinyl silicon, 5-10 parts of styrene butadiene rubber, 15-30 parts of polytetrafluoroethylene, 30-65 parts of polyether sulfone resin and a plurality of parts of purified water. The invention improves the multipurpose use of the whole TPU film, the added methyl vinyl silicone rubber can improve the whole high temperature resistance, the polystyrene has better corrosion resistance and solvent resistance, and the added styrene butadiene rubber further improves the wear resistance, heat resistance and aging resistance of the whole TPU film.
Description
Technical Field
The invention relates to a manufacturing method of a spraying material, in particular to a novel curtain coating coiling middle-permeation waterproof moisture-permeable TPU film, and belongs to the technical field of spraying materials.
Background
The TPU thermoplastic TPU elastomer is prepared by extruding and mixing MDI containing NCO functional groups, POLYOL containing OH functional groups and 1.4BG, and is widely used for processing modes such as injection, extrusion, calendering and solution type resin and the like due to good elasticity, good physical properties and good mechanical strength, and is a plastic material frequently used by plastic processing manufacturers, and the prepared product covers the range of industrial application and civil necessities.
Most of the existing waterproof moisture-permeable TPU films are used in a production process to be adhered with cloth for shoe materials so as to achieve the waterproof moisture-permeable effect, and the TPU films are used in the shoe materials, wherein the wear resistance and the ductility temperature resistance are low, so that the TPU films have the defects of short service life, poor quality effect and no multipurpose use purpose in the process of using the TPU films for shoe sole materials.
Disclosure of Invention
The invention mainly aims to provide a novel cast reeling waterproof moisture-permeable TPU film, and solves the problems of poor wear resistance, poor ductility and poor pressure resistance of the traditional waterproof moisture-permeable TPU film in the production process.
In order to achieve the purpose, the invention provides the following technical scheme:
a novel curtain coating coiling intermediate-permeation waterproof moisture-permeable TPU film is characterized by comprising the following raw materials in parts by weight: 20-40 parts of diphenylmethane diisocyanate, 10-20 parts of polytetrahydrofuran, 20-40 parts of butanediol, 10-15 parts of antioxidant, 10-15 parts of ethylene propylene diene monomer, 12-18 parts of methyl vinyl silicon, 5-10 parts of styrene butadiene rubber, 15-30 parts of polytetrafluoroethylene, 30-65 parts of polyether sulfone resin and a plurality of parts of purified water;
the novel cast winding intermediate-permeability waterproof moisture-permeable TPU film comprises the following steps:
the method comprises the following steps: 20-40 parts of polyether sulfone (PES) resin is placed in a melting furnace at 290-320 ℃ for melting, then the solution is poured into a container A, after a small part of purified water is added, the temperature of the container A is raised to 100-120 ℃, the stirring speed is 100r/min, and the stirring time is 5 min;
step two: then, the mixture in the first step is dehydrated for 2 to 3 hours in vacuum, so that the water content in the solution is less than 0.05 percent;
step three: then the vacuum state is released, and a small amount of nitrogen is introduced for standing for 3 min;
step four: melting 20-40 parts of diphenylmethane diisocyanate and 10-20 parts of polytetrahydrofuran at the temperature of 100-150 ℃, introducing into a container B, heating to the temperature of 60-70 ℃, stirring at the speed of 100r/min, and stirring for 5 min;
step five: vacuum degassing the solution obtained in the fourth step for 0.5-1h, removing the vacuum state, introducing nitrogen and standing for 3 min;
step six: adding 20-40 parts of butanediol into a container C, heating to 30-50 ℃, stirring at a speed of 100r/min, adding a small amount of water while stirring for 8min, and then performing ultraviolet irradiation drying at a drying temperature of 85 ℃ for 1-1.5 h;
step seven: vacuum dehydrating the solution obtained in the sixth step for 0.5-1h to ensure that the water content of the container C is less than 0.08%, then releasing the vacuum state, introducing nitrogen, and standing for three minutes;
step eight: injecting the solution in the container A into a container B, mixing and stirring at the stirring speed of 200-300r/min, injecting 10-15 parts of antioxidant and 10-15 parts of ethylene propylene diene after stirring for 2min, then continuing stirring at the speed for 5min, and controlling the temperature at 30-35 ℃ to obtain a mixed solution a;
step nine: injecting the mixture in the step six into the solution A in the step four, stirring at the stirring speed of 200-;
step ten: and E, extruding the mixed material obtained in the step nine by an automatic double-screw extruder to form a thin film to obtain the TPU film.
Preferably, the antioxidant in the first step is one of Butylated Hydroxyanisole (BHA), Butylated Hydroxytoluene (BHT), Propyl Gallate (PG) and tert-butylhydroquinone (TBHQ).
Preferably, the vacuum dehydration pressure in the second step is 0.5 Mpa.
Preferably, the double-screw reaction extruder in the step ten is an LSF-68 type (nine-section temperature-adjusting cylinder), the center distance of the screws is 60mm, the length-diameter ratio of the screws is 45, and the gap between the screws and the cylinder is less than or equal to 0.02 mm.
Preferably, the antioxidant accounts for 0.3-0.5% of the total solution by mass.
Preferably, the temperature of the head of the double-screw extruder in the step ten is controlled at 140-180 ℃.
Compared with the prior art, the invention provides a novel method for casting and coiling a middle-permeation waterproof and moisture-permeable TPU film, which has the following beneficial effects:
the designed polyether type TPU film has strong low-temperature flexibility and hydrolysis resistance, the integral quality of the TPU film is improved, the added polytetrafluoroethylene can well realize waterproof, breathable and dustproof effects, and the use of the integral TPU film in multiple purposes is improved.
According to the TPU film obtained by the invention, the added methyl vinyl silicone rubber has high temperature resistance, so that the overall high temperature resistance is improved, the polystyrene has good corrosion resistance and solvent resistance, and meanwhile, the added styrene butadiene rubber further improves the wear resistance, heat resistance and aging resistance of the overall TPU film.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
A novel curtain coating coiling intermediate-permeation waterproof moisture-permeable TPU film comprises the following raw materials in parts by weight: 20 parts of diphenylmethane diisocyanate, 10 parts of polytetrahydrofuran, 20 parts of butanediol, 10-15 parts of antioxidant, 10 parts of ethylene propylene diene monomer, 12 parts of methyl vinyl silicon, 5 parts of styrene butadiene rubber, 15 parts of polytetrafluoroethylene, 30 parts of polyether sulfone resin and a plurality of parts of purified water.
The novel cast winding intermediate-permeability waterproof moisture-permeable TPU film comprises the following steps:
the method comprises the following steps: and (3) melting 20 parts of polyether sulfone resin (PES) in a melting furnace at 290 ℃, pouring the solution into a container A, adding a small part of purified water, heating the container A to 100 ℃, and stirring at the speed of 100r/min for 5 min.
Step two: and then, carrying out vacuum dehydration on the mixture in the step one for 2 hours, so that the water content in the solution is less than 0.05 percent.
Step three: then the vacuum state is released, and a small amount of nitrogen is introduced for standing for 3 min.
Step four: melting 20 parts of diphenylmethane diisocyanate and 10 parts of polytetrahydrofuran at 100 ℃, introducing into a container B, heating to 60 ℃, stirring at a speed of 100r/min, and stirring for 5 min.
Step five: and (4) carrying out vacuum degassing on the solution obtained in the fourth step for 0.5-1h, relieving the vacuum state, introducing nitrogen and standing for 3 min.
Step six: adding 20 parts of butanediol into a container C, heating to 30 ℃, stirring at the speed of 100r/min, adding a small amount of water while stirring, stirring for 8min, and then performing ultraviolet irradiation drying at the drying temperature of 85 ℃, wherein the irradiation drying time is 1 h.
Step seven: and (5) dehydrating the solution in the sixth step for 0.5h in vacuum to ensure that the water content of the container C is less than 0.08%, and then releasing the vacuum state, introducing nitrogen and standing for three minutes.
Step eight: and (3) injecting the solution in the container A into the container B, mixing and stirring at the stirring speed of 200r/min, injecting 10 parts of antioxidant and 10 parts of ethylene propylene diene after stirring for 2min, then continuing stirring at the speed for 5min, and controlling the temperature at 30 ℃ to obtain a mixed solution a.
Step nine: and C, injecting the mixture in the step six into the solution A in the step four, stirring at the stirring speed of 200r/min for 3min, injecting 10 parts of ethylene propylene diene, 12 parts of methyl vinyl silicon, 5 parts of styrene butadiene rubber and 15 parts of polytetrafluoroethylene, continuously stirring and mixing in a forward rotation mode and a reverse rotation mode at the speed of 300r/min, and finally obtaining the TPU film raw material.
Step ten: and E, extruding the mixed material obtained in the step nine by an automatic double-screw extruder to form a thin film to obtain the TPU film.
Through control to carry out ultraviolet irradiation drying after the same industry wherein, can carry out effectual sterilization and the whole tensile properties of former solution, because the former solution carries out high-efficient dehydration after for holistic former solution density can increase, then can to a great extent fuse and improve holistic stretch-proofing performance when middle mixing process
Example 2
A novel curtain coating coiling intermediate-permeation waterproof moisture-permeable TPU film is characterized by comprising the following raw materials in parts by weight: 20-40 parts of diphenylmethane diisocyanate, 10-20 parts of polytetrahydrofuran, 20-40 parts of butanediol, 10-15 parts of antioxidant, 10-15 parts of ethylene propylene diene monomer, 12-18 parts of methyl vinyl silicon, 5-10 parts of styrene butadiene rubber, 15-30 parts of polytetrafluoroethylene, 30-65 parts of polyether sulfone resin and a plurality of parts of purified water.
The novel cast winding intermediate-permeability waterproof moisture-permeable TPU film comprises the following steps:
the method comprises the following steps: 30 parts of polyether sulfone resin (PES) are put in a melting furnace at 305 ℃ for melting, then the solution is poured into a container A, after a small part of purified water is added, the temperature of the container A is raised to 110 ℃, the stirring speed is 100r/min, and the stirring time is 5 min.
Step two: and then, the mixture in the step one is subjected to vacuum dehydration for 2.5 hours, so that the water content in the solution is less than 0.05 percent.
Step three: then the vacuum state is released, and a small amount of nitrogen is introduced for standing for 3 min.
Step four: melting diphenylmethane diisocyanate parts and 15 parts of polytetrahydrofuran at 125 ℃, introducing into a container B, heating to 65 ℃, stirring at a speed of 100r/min, and stirring for 5 min.
Step five: and (4) carrying out vacuum degassing on the solution obtained in the fourth step for 0.8h, relieving the vacuum state, introducing nitrogen and standing for 3 min.
Step six: adding 30 parts of butanediol into a container C, heating to 40 ℃, stirring at the speed of 100r/min, adding a small amount of water while stirring, stirring for 8min, and then performing ultraviolet irradiation drying at the drying temperature of 85 ℃, wherein the irradiation drying time is 1.25 h.
Step seven: and (5) dehydrating the solution in the sixth step for 0.8h in vacuum to ensure that the water content of the container C is less than 0.08%, and then releasing the vacuum state, introducing nitrogen and standing for three minutes.
Step eight: and (3) injecting the solution in the container A into the container B, mixing and stirring at the stirring speed of 250r/min, injecting 12.5 parts of antioxidant and 12.5 parts of ethylene propylene diene after stirring for 2min, then continuing stirring at the speed for 5min, and controlling the temperature at 32.5 ℃ to obtain a mixed solution a.
Step nine: and C, injecting the mixture in the step six into the solution A in the step four, stirring at the stirring speed of 250r/min, injecting 12.5 parts of ethylene propylene diene monomer, 15 parts of methyl vinyl silicon, 7.5 parts of butadiene styrene rubber and 20 parts of polytetrafluoroethylene after stirring for 3min, continuously stirring and mixing in forward rotation and reverse rotation at the speed of 400r/min, and finally obtaining the TPU film raw material.
Step ten: and E, extruding the mixed material obtained in the step nine by an automatic double-screw extruder to form a thin film to obtain the TPU film.
The polytetrafluoroethylene arranged has the characteristic of high temperature resistance, the friction coefficient of the polytetrafluoroethylene is extremely low, the abrasion is reduced, the temperature resistance of the whole TPU film is improved, and the TPU film can be uniformly fused and has higher efficiency through the stirring and mixing of forward rotation and reverse rotation.
EXAMPLE III
A novel curtain coating coiling intermediate-permeation waterproof moisture-permeable TPU film is characterized by comprising the following raw materials in parts by weight: 40 parts of diphenylmethane diisocyanate, 20 parts of polytetrahydrofuran, 40 parts of butanediol, 15 parts of antioxidant, 15 parts of ethylene propylene diene, 18 parts of methyl vinyl silicon, 10 parts of styrene-butadiene rubber, 30 parts of polytetrafluoroethylene, 65 parts of polyether sulfone and a plurality of parts of purified water.
The novel cast winding intermediate-permeability waterproof moisture-permeable TPU film comprises the following steps:
the method comprises the following steps: 40 parts of polyether sulfone resin (PES) are put in a melting furnace at 320 ℃ for melting, then the solution is poured into a container A, after a small part of purified water is added, the temperature of the container A is raised to 120 ℃, the stirring speed is 100r/min, and the stirring time is 5 min.
Step two: and then, carrying out vacuum dehydration on the mixture in the step one for 3 hours, so that the water content in the solution is less than 0.05 percent.
Step three: then the vacuum state is released, and a small amount of nitrogen is introduced for standing for 3 min.
Step four: 40 parts of diphenylmethane diisocyanate and 20 parts of polytetrahydrofuran are melted at 150 ℃ and then introduced into a container B, and then heated to 70 ℃, stirred at the speed of 100r/min and stirred for 5 min.
Step five: and (4) carrying out vacuum degassing on the solution obtained in the fourth step for 1h, relieving the vacuum state, introducing nitrogen and standing for 3 min.
Step six: adding 40 parts of dices into a container C, heating to 50 ℃, stirring at the speed of 100r/min, adding a small amount of water while stirring, stirring for 8min, and then performing ultraviolet irradiation drying at the drying temperature of 85 ℃, wherein the irradiation drying time is 1.5 h.
Step seven: and (5) dehydrating the solution obtained in the sixth step for 0.5-1h in vacuum to ensure that the water content of the container C is less than 0.08%, then releasing the vacuum state, introducing nitrogen, and standing for three minutes.
Step eight: and injecting the solution in the container A into a container B, mixing and stirring at the stirring speed of 200-300r/min, injecting 15 parts of antioxidant and 15 parts of ethylene propylene diene after stirring for 2min, then continuing stirring at the speed for 5min, and controlling the temperature at 35 ℃ to obtain a mixed solution a.
Step nine: and C, injecting the mixture in the step six into the solution A in the step four, stirring at the stirring speed of 300r/min for 3min, injecting 15 parts of ethylene propylene diene, 18 parts of methyl vinyl silicon, 10 parts of styrene butadiene rubber and 30 parts of polytetrafluoroethylene, continuously stirring and mixing in a forward rotation mode and a reverse rotation mode at the speed of 500r/min, and finally obtaining the TPU film raw material.
Step ten: and E, extruding the mixed material obtained in the step nine by an automatic double-screw extruder to form a thin film to obtain the TPU film.
Experimental example 1
The TPU film obtained by the invention has strong low-temperature flexibility and hydrolysis resistance, the overall quality of the TPU film is improved, the added polytetrafluoroethylene can well perform waterproof, breathable and dustproof effects, the multipurpose use of the overall TPU film is improved, meanwhile, the added methyl vinyl silicone rubber has high temperature resistance and improves the overall high-temperature resistance because of high temperature resistance, the polystyrene has better corrosion resistance and solvent resistance, and meanwhile, the wear resistance, heat resistance and aging resistance of the overall TPU film are further improved through the added styrene butadiene rubber
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (6)
1. A novel curtain coating coiling intermediate-permeation waterproof moisture-permeable TPU film is characterized by comprising the following raw materials in parts by weight: 20-40 parts of diphenylmethane diisocyanate, 10-20 parts of polytetrahydrofuran, 20-40 parts of butanediol, 10-15 parts of antioxidant, 10-15 parts of ethylene propylene diene monomer, 12-18 parts of methyl vinyl silicon, 5-10 parts of styrene butadiene rubber, 15-30 parts of polytetrafluoroethylene, 30-65 parts of polyether sulfone resin and a plurality of parts of purified water;
the novel cast winding intermediate-permeability waterproof moisture-permeable TPU film comprises the following steps:
the method comprises the following steps: 20-40 parts of polyether sulfone (PES) resin is placed in a melting furnace at 290-320 ℃ for melting, then the solution is poured into a container A, after a small part of purified water is added, the temperature of the container A is raised to 100-120 ℃, the stirring speed is 100r/min, and the stirring time is 5 min;
step two: then, the mixture in the first step is dehydrated for 2 to 3 hours in vacuum, so that the water content in the solution is less than 0.05 percent;
step three: then the vacuum state is released, and a small amount of nitrogen is introduced for standing for 3 min;
step four: melting 20-40 parts of diphenylmethane diisocyanate and 10-20 parts of polytetrahydrofuran at the temperature of 100-150 ℃, introducing into a container B, heating to the temperature of 60-70 ℃, stirring at the speed of 100r/min, and stirring for 5 min;
step five: vacuum degassing the solution obtained in the fourth step for 0.5-1h, removing the vacuum state, introducing nitrogen and standing for 3 min;
step six: adding 20-40 parts of butanediol into a container C, heating to 30-50 ℃, stirring at a speed of 100r/min, adding a small amount of water while stirring for 8min, and then performing ultraviolet irradiation drying at a drying temperature of 85 ℃ for 1-1.5 h;
step seven: vacuum dehydrating the solution obtained in the sixth step for 0.5-1h to ensure that the water content of the container C is less than 0.08%, then releasing the vacuum state, introducing nitrogen, and standing for three minutes;
step eight: injecting the solution in the container A into a container B, mixing and stirring at the stirring speed of 200-300r/min, injecting 10-15 parts of antioxidant and 10-15 parts of ethylene propylene diene after stirring for 2min, then continuing stirring at the speed for 5min, and controlling the temperature at 30-35 ℃ to obtain a mixed solution a;
step nine: injecting the mixture in the step six into the solution A in the step four, stirring at the stirring speed of 200-;
step ten: and E, extruding the mixed material obtained in the step nine by an automatic double-screw extruder to form a thin film to obtain the TPU film.
2. A novel cast mid-roll waterproof moisture permeable TPU film as described in claim 1 wherein the antioxidant in step one is selected from the group consisting of Butylated Hydroxyanisole (BHA), Butylated Hydroxytoluene (BHT), Propyl Gallate (PG), and Tertiary Butyl Hydroquinone (TBHQ).
3. A novel cast roll-to-roll waterproof moisture permeable TPU film as described in claim 1 wherein the vacuum dewatering pressure in step two is 0.5 Mpa.
4. A novel casting reeling waterproof and moisture permeable TPU film as claimed in claim 1, wherein the twin-screw reaction extruder in step ten is LSF-68 type (nine sections of temperature-adjusting barrel), the center distance between screws is 60mm, the length-diameter ratio of screws is 45, and the gap between screws and barrel is less than or equal to 0.02 mm.
5. A novel cast, mid-roll, water-permeable, moisture-permeable TPU film as claimed in claim 1 where the antioxidant is present in an amount of 0.3% to 0.5% by weight of the total solution.
6. A novel casting reeling waterproof and moisture permeable TPU film as claimed in claim 1, wherein the head temperature of the twin-screw extruder in the step ten is controlled at 140-180 ℃.
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| CN105111724A (en) * | 2015-09-07 | 2015-12-02 | 苏州市雄林新材料科技有限公司 | High-water-permeability TPU (thermoplastic polyurethane) film and preparation method thereof |
| CN106117493A (en) * | 2016-06-27 | 2016-11-16 | 张勇 | A kind of preparation method of heat resistant type TPU film |
| CN107057021A (en) * | 2017-03-22 | 2017-08-18 | 上海恒安聚氨酯股份有限公司 | High permeation waterproof humidity-permeant TPUE of heat-resistance type and preparation method thereof |
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