CN106496628A - A kind of preparation method of thermoplastic polyurethane foam's film - Google Patents
A kind of preparation method of thermoplastic polyurethane foam's film Download PDFInfo
- Publication number
- CN106496628A CN106496628A CN201611002667.0A CN201611002667A CN106496628A CN 106496628 A CN106496628 A CN 106496628A CN 201611002667 A CN201611002667 A CN 201611002667A CN 106496628 A CN106496628 A CN 106496628A
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- tpu
- film
- thermoplastic polyurethane
- preparation
- polyurethane foam
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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
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/36—After-treatment
-
- 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
- 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
- C08J9/122—Hydrogen, oxygen, CO2, nitrogen or noble gases
-
- 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
- C08J2203/00—Foams characterized by the expanding agent
- C08J2203/06—CO2, N2 or noble gases
-
- 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
- C08J2203/00—Foams characterized by the expanding agent
- C08J2203/08—Supercritical fluid
-
- 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
- C08J2375/00—Characterised by the use of polyureas or polyurethanes; Derivatives of such polymers
- C08J2375/04—Polyurethanes
-
- 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
- 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
- C08J2427/16—Homopolymers or copolymers of vinylidene fluoride
-
- 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
- C08J2429/00—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 an alcohol, ether, aldehydo, ketonic, acetal, or ketal radical; Hydrolysed polymers of esters of unsaturated alcohols with saturated carboxylic acids; Derivatives of such polymer
- C08J2429/02—Homopolymers or copolymers of unsaturated alcohols
- C08J2429/04—Polyvinyl alcohol; Partially hydrolysed homopolymers or copolymers of esters of unsaturated alcohols with saturated carboxylic acids
Abstract
The invention discloses a kind of preparation method of thermoplastic polyurethane foam's film, TPU resins, gas barrier agent, compatilizer, nucleator are carried out dry-mixed, adopt extruder curtain coating to prepare the TPU laminated film coiled materials that thickness is for 0.4 millimeter；TPU laminated film coiled materials are inserted in autoclave body, implantation temperature is 30～60 DEG C, and pressure is the Compressed CO_2 fluid of 1 6MPa, process 1～12 hour, Compressed CO_2 fluid is diffused in TPU laminated film matrixes；TPU laminated films after by process are launched with the speed of 0.1～1.0 meter per second, by foamable in vapor groove that temperature is 80～150 degree, the TPU laminated films for expanding are obtained；The TPU laminated films of expansion are stretched for 130 160 DEG C of monoaxial stretching apparatus through excess temperature, stretching time is less than 15 seconds, and prepared thickness is the TPU foamed thin sheets of 0.1～0.5mm.Using above-mentioned technical proposal, the TPU foamed thin sheets that thickness is 0.1～0.5 millimeter can be prepared, and avoid that abscess-size is excessive, the defect that density of material is excessive.
Description
Technical field
The present invention relates to a kind of thermoplastic polyurethane（TPU）The preparation method of foamed thin sheet, more particularly to a kind of high pressure or
The method that person's supercritical fluid physical blowing prepares TPU foamed thin sheets.
Background technology
Artificial leather such as polyurethane（PU）Foam leather, polyvinyl chloride（PVC）Etc. foam leather as natural leather alternative materials,
Quickly grow in China.But, artificial leather in process of manufacture inevitably using poisonous and hazardous solvent in a large number and
Plasticizer.In recent years, with the volatile organic matter that the raising of people's environmental consciousness, artificial leather are present in use（VOC）
Problem has caused the attention of various circles of society and artificial leather industry.At present, American-European, Japan, China all successively put into effect the inspection of VOC
Survey regulation.
TPU have excellent wearability, chemical resistance, oil resistant, water-fast, high resiliency, antifatigue many advantages, such as, be
A kind of excellent performance, the environment-friendly materials for having price competitiveness.After TPU resins are prepared into foam films, also there is lightweight, softness, height
The advantages of resilience, can instead tradition PU, the novel environment friendly artificial leather of PVC artificial leather.
Chinese patent literature CN104861642A discloses one kind with CBA azodicarbonamide（AC）In conjunction with carbon
Sour hydrogen sodium be composite foamable agent, the method for preparing TPU foam films used for artificial leather, first by reaction raw materials mixed at high speed after, entrance
Screw extruder carries out reactive extrursion and makes TPU master batches, then begins to pratise to enter with foaming agent under two-roll mill in flakes TPU master batches
Row foaming.The AC foaming agents used by the method can not avoid the problem of VOC completely, and have that abscess-size is excessive, and material is close
Spend big problem.
High-pressure fluid such as high pressure CO2Fluid is a kind of cheap and colourless, nontoxic, odorless, harmless physical blowing
Agent, according to demand, high pressure CO2Fluid can be high-pressure gas flow body, highly pressurised liquid fluid and supercritical fluid.CO2Reach super facing
The condition of boundary's state is very gentle, only needs temperature more than 31.1 °C, pressure more than 7.38 MPa, CO2Will be changed into overcritical
CO2.CO2Fluid can be removed from product easily, the postprocessing working procedures of the completely left out complexity that is brought using conventional solvent, and
And can also realize to CO2Recycling.
Chinese patent literature CN103951965A is disclosed and is prepared as foaming agent with high-pressure fluid or supercritical fluid
The method of TPU foam sheets.Due to high-pressure fluid, in TPU matrixes, diffusion velocity is exceedingly fast, and the method is difficult to prepare thickness and is only
0.1～0.5 millimeter of foamed thin sheet material used for artificial leather, and the materials such as the larger shoe-pad of thickness can only be prepared.
Content of the invention
Therefore, it is an object of the invention to overcoming defect of the prior art, there is provided a kind of thermoplastic polyurethane foam is thin
The preparation method of film.
To achieve these goals, the preparation method of a kind of thermoplastic polyurethane foam's film of the invention, using following
The raw material of parts by weight：
100 parts of TPU resins；
Gas barrier agent is 5～10 parts；
Compatilizer is 1～3 part；
Nucleator is 1～5 part；
Comprise the following steps：
1）TPU resins, gas barrier agent, compatilizer, nucleator are carried out according to above-mentioned mass fraction dry-mixed, using extruder stream
Prolong the TPU laminated film coiled materials for preparing that thickness is 0.4 millimeter；
2）TPU laminated film coiled materials are inserted in autoclave body, implantation temperature is 30～60 DEG C, high pressure of the pressure for 1-6MPa
CO2 fluids, process 1～12 hour, Compressed CO_2 fluid is diffused in TPU laminated film matrixes；
3）TPU laminated films after by process are launched with the speed of 0.1～1.0 meter per second, by the water that temperature is 80～150 degree
Foamable in steam groove, is obtained the TPU laminated films of expansion；
4）The TPU laminated films of expansion are stretched for 130-160 DEG C of monoaxial stretching apparatus through excess temperature, stretching time does not surpass
15 seconds are spent, prepared thickness is the TPU foamed thin sheets of 0.1～0.5mm.
In the step 1, melting means of the TPU resins at 190 DEG C is 2.0-5.0g/10min.
In the step 1, gas barrier agent includes at least one in polyvinyl alcohol, Kynoar；The compatilizer bag
Include Hydrogenated thermoplastic's butadiene-styrene rubber-polyurethane grafting substrate, Hydrogenated thermoplastic's butadiene-styrene rubber-thermoplastic polyurethane copolymer, thermoplastic
At least one in property butadiene-styrene rubber-methyl methacrylate-grafted thing；The nucleator includes three dichloroxides, silica
In at least one.
In the step 1, the thickness of TPU laminated films coiled material is 0.2～0.6mm.
In the step 1, in TPU laminated films coiled material, the length of TPU laminated films is 50～150 meters
Preferably 80～150 meters of the length of TPU laminated films in TPU laminated films coiled material in the step 1.
TPU laminated films are wound TPU THIN COMPOSITE film rolls jointly with fabric diaphragm material with holes in the step 1
Material.High pressure or supercritical fluid CO due to TPU laminated films2Gas transmission rate is 1.0 × 10-7～10.0 × 10- 7cm2/ s, less than the 2.5 × 10 of pure TPU film-6cm2/ s, therefore in order to increase high pressure or supercritical fluid CO2Compound in TPU
Diffusion velocity in film, is tied with fabric diaphragm with holes between TPU laminated films.
In the step 3, in order that TPU laminated film controllable expansions, temperature successively elevated 2 can be set in water vapour groove
～3 compartments.TPU laminated films thermally equivalent and controllable expansion are made using pressure roller/guide roller groove combination in foaming process.
Due to high pressure or supercritical fluid CO2TPU complex matrixes can be quickly diffused out, cause TPU laminated films to foam
Multiplying power reduction even results in TPU laminated films and can not foam, in order to ensure TPU laminated films uniformly and stably can foam,
In the step 3, the development rate of TPU laminated films is preferably 0.2～0.8 meter per second.
In the step 4, monoaxial stretching apparatus have more than 1 group draw roll, and the draw ratio of draw roll is 1.2～2.0.
In the step 4, the density of obtained TPU foamed thin sheets is 0.2～0.5g/cm3.
In the step 4, the abscess-size of obtained TPU foamed thin sheets is 1～50 micron.
Using above-mentioned technical proposal, the preparation method of thermoplastic polyurethane foam's film of the present invention, from cleaning, honest and clean
Valency, eco-friendly supercritical fluid CO2For physical blowing agent, the committed step such as shape through physical blowing and first break draft, energy
Thickness is enough prepared for 0.1～0.5 millimeter, and density is 0.2～0.5g/cm3, and abscess-size is 1～50 micron of TPU foamed thin sheets
Material, and avoid that abscess-size is excessive, the defect that density of material is excessive.
Specific embodiment
Below by way of specific embodiment, the present invention is described in further detail.
Embodiment 1：
By the TPU resins that 100 parts of melting means are 3g/10min, 6 parts of gas barrier masterbatch for including polyvinyl alcohol, 2 parts compatible
Agent, 2 portions of nucleators are dry-mixed in agitator, and the melting extrusion of the extruded casting machine of compound obtains the TPU that thickness is 0.4 millimeter
TPU laminated films are wound the TPU THIN COMPOSITEs that length is 100 meters with fabric diaphragm material with holes by laminated film jointly
Film coiled material；TPU laminated film coiled materials are inserted in autoclave body, implantation temperature is 50 degree, high pressure CO of the pressure for 5MPa2Stream
Body, processing makes high pressure CO in 6 hours2Fluid is diffused in TPU laminated film matrixes；TPU laminated films coiled material is taken out and with 0.5
The speed of meter per second is launched, and foamable in the two temperatures section vapor groove that temperature is 80/100 degree, obtains length and width and expands
TPU film material, by the TPU film material of expansion through the uniaxial tension system that excess temperature is 150 degree, stretch through 2 groups of drawing-offs,
Cutting edge, obtains the uniform TPU foamed thin sheets of in uniform thickness, degrees of expansion.Test shows that the thickness of TPU foamed thin sheets is 0.3
Millimeter, density is 0.40g/cm3, average cell size is 30 microns.
Comparative example 1：
Except do not contain in TPU film raw material any dose auxiliary agent, other operations are same as Example 1.TPU foamed thin sheets only have 30
Rice has uniform and stable expansion, and density is 0.45g/cm3, and follow-up TPU foamed thin sheet expansion multiplying powers start constantly to reduce, 80 meters
The density of TPU foamed thin sheets afterwards rises to 0.6g/cm3.
Embodiment 2：
Except the melting means of TPU resins is 5 g/10min, the content of gas barrier masterbatch is 10 parts, and the content of compatilizer is 3 parts,
Other operations are same as Example 1, obtained the TPU foamed thin sheets of even inflation, and the density of foamed thin sheet is 0.32g/cm3,
Thickness is 0.3 millimeter, and average cell size is 25 microns.
Obviously, above-described embodiment is only intended to clearly illustrate example, and the not restriction to embodiment.For
For those of ordinary skill in the art, the change or change of other multi-forms can also be made on the basis of the above description
Dynamic.There is no need to be exhaustive to all of embodiment.And thus extended obvious change or change
Move among still in the protection domain of the invention.
Claims (8)
1. a kind of preparation method of thermoplastic polyurethane foam's film, it is characterised in that：Raw material using following parts by weight：
100 parts of TPU resins, gas barrier agent are 5～10 parts, and compatilizer is 1～3 part, and nucleator is 1～5 part；
Comprise the following steps：
1）TPU resins, gas barrier agent, compatilizer, nucleator are carried out according to above-mentioned mass fraction dry-mixed, using extruder stream
Prolong the TPU laminated film coiled materials for preparing that thickness is 0.4 millimeter；
2）TPU laminated film coiled materials are inserted in autoclave body, implantation temperature is 30～60 DEG C, high pressure of the pressure for 1-6MPa
CO2 fluids, process 1～12 hour, Compressed CO_2 fluid is diffused in TPU laminated film matrixes；
3）TPU laminated films after by process are launched with the speed of 0.1～1.0 meter per second, by the water that temperature is 80～150 degree
Foamable in steam groove, is obtained the TPU laminated films of expansion；
4）The TPU laminated films of expansion are stretched for 130～160 DEG C of monoaxial stretching apparatus through excess temperature, stretching time is not
More than 15 seconds, prepared thickness was the TPU foamed thin sheets of 0.1～0.5mm.
2. the preparation method of thermoplastic polyurethane foam's film as claimed in claim 1, it is characterised in that：In the step 1
Melting means of the TPU resins at 190 DEG C is 2.0-5.0g/10min.
3. the preparation method of thermoplastic polyurethane foam's film as claimed in claim 1, it is characterised in that：In the step 1
In the step 1, gas barrier agent includes at least one in polyvinyl alcohol, Kynoar；The compatilizer includes the heat of hydrogenation
Plasticity butadiene-styrene rubber-polyurethane grafting substrate, Hydrogenated thermoplastic's butadiene-styrene rubber-thermoplastic polyurethane copolymer, thermoplasticity butylbenzene rubber
At least one in glue-methyl methacrylate-grafted thing；The nucleator is included in three dichloroxides, silica at least
A kind of.
4. the preparation method of thermoplastic polyurethane foam's film as claimed in claim 1, it is characterised in that：In the step 1
The thickness of TPU laminated film coiled materials is 0.2～0.6mm.
5. the preparation method of thermoplastic polyurethane foam's film as claimed in claim 1, it is characterised in that：In the step 1
In TPU laminated film coiled materials, the length of TPU laminated films is 50～150 meters
The preparation method of thermoplastic polyurethane foam's film as claimed in claim 5, it is characterised in that：TPU in the step 1
In laminated film coiled material, the length of TPU laminated films is 80～150 meters.
6. the preparation method of thermoplastic polyurethane foam's film as claimed in claim 1, it is characterised in that：In the step 1
TPU laminated films are wound TPU laminated film coiled materials jointly with fabric diaphragm material with holes.
7. the preparation method of thermoplastic polyurethane foam's film as claimed in claim 1, it is characterised in that：In the step 3,
Temperature elevated 2～3 compartments successively are set in the water vapour groove.
8. the preparation method of thermoplastic polyurethane foam's film as claimed in claim 1, it is characterised in that：In the step 3
In, the development rate of TPU laminated films is preferably 0.2～0.8 meter per second.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611002667.0A CN106496628A (en) | 2016-11-15 | 2016-11-15 | A kind of preparation method of thermoplastic polyurethane foam's film |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611002667.0A CN106496628A (en) | 2016-11-15 | 2016-11-15 | A kind of preparation method of thermoplastic polyurethane foam's film |
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| CN106496628A true CN106496628A (en) | 2017-03-15 |
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| CN201611002667.0A Pending CN106496628A (en) | 2016-11-15 | 2016-11-15 | A kind of preparation method of thermoplastic polyurethane foam's film |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109401281A (en) * | 2018-09-11 | 2019-03-01 | 苏州市雄林新材料科技有限公司 | A kind of high-elastic TPU film and preparation method thereof |
| CN109438968A (en) * | 2018-09-11 | 2019-03-08 | 苏州市雄林新材料科技有限公司 | A kind of automotive headrest high-barrier TPU film and preparation method thereof |
| CN111808354A (en) * | 2019-04-10 | 2020-10-23 | 东莞市龙奕实业有限公司 | Production process of supercritical physical foaming coarse-pore sports equipment |
| CN115538187A (en) * | 2022-11-01 | 2022-12-30 | 张建春 | Preparation method of low-cost waterproof moisture-permeable fabric capable of blocking viruses |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103951965A (en) * | 2014-05-09 | 2014-07-30 | 晋江国盛鞋材有限公司 | Color TPU (thermoplastic polyurethane) foam material and preparation method and application thereof as well as method for preparing molding body, sheet and shoe material by using same |
| CN105714574A (en) * | 2016-03-07 | 2016-06-29 | 美瑞新材料股份有限公司 | Foaming thermoplastic polyurethane artificial leather and preparation method thereof |
-
2016
- 2016-11-15 CN CN201611002667.0A patent/CN106496628A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103951965A (en) * | 2014-05-09 | 2014-07-30 | 晋江国盛鞋材有限公司 | Color TPU (thermoplastic polyurethane) foam material and preparation method and application thereof as well as method for preparing molding body, sheet and shoe material by using same |
| CN105714574A (en) * | 2016-03-07 | 2016-06-29 | 美瑞新材料股份有限公司 | Foaming thermoplastic polyurethane artificial leather and preparation method thereof |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109401281A (en) * | 2018-09-11 | 2019-03-01 | 苏州市雄林新材料科技有限公司 | A kind of high-elastic TPU film and preparation method thereof |
| CN109438968A (en) * | 2018-09-11 | 2019-03-08 | 苏州市雄林新材料科技有限公司 | A kind of automotive headrest high-barrier TPU film and preparation method thereof |
| CN111808354A (en) * | 2019-04-10 | 2020-10-23 | 东莞市龙奕实业有限公司 | Production process of supercritical physical foaming coarse-pore sports equipment |
| CN115538187A (en) * | 2022-11-01 | 2022-12-30 | 张建春 | Preparation method of low-cost waterproof moisture-permeable fabric capable of blocking viruses |
| CN115538187B (en) * | 2022-11-01 | 2024-03-15 | 张建春 | Preparation method of low-cost waterproof moisture-permeable fabric for blocking viruses |
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Application publication date: 20170315 |
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