CN113896937B - Preparation method of light high-marble foam sole for high-end sports shoes - Google Patents
Preparation method of light high-marble foam sole for high-end sports shoes Download PDFInfo
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- CN113896937B CN113896937B CN202111306040.5A CN202111306040A CN113896937B CN 113896937 B CN113896937 B CN 113896937B CN 202111306040 A CN202111306040 A CN 202111306040A CN 113896937 B CN113896937 B CN 113896937B
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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
- C08J9/04—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
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- A—HUMAN NECESSITIES
- A43—FOOTWEAR
- A43B—CHARACTERISTIC FEATURES OF FOOTWEAR; PARTS OF FOOTWEAR
- A43B13/00—Soles; Sole-and-heel integral units
- A43B13/02—Soles; Sole-and-heel integral units characterised by the material
- A43B13/04—Plastics, rubber or vulcanised fibre
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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
- C08J2203/00—Foams characterized by the expanding agent
- C08J2203/06—CO2, N2 or noble gases
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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
- C08J2203/00—Foams characterized by the expanding agent
- C08J2203/08—Supercritical fluid
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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
- C08J2375/00—Characterised by the use of polyureas or polyurethanes; Derivatives of such polymers
- C08J2375/04—Polyurethanes
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids
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- Health & Medical Sciences (AREA)
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- Medicinal Chemistry (AREA)
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- Manufacture Of Porous Articles, And Recovery And Treatment Of Waste Products (AREA)
- Footwear And Its Accessory, Manufacturing Method And Apparatuses (AREA)
Abstract
The invention discloses a preparation method of a light high-marble foam sole for high-end sports shoes. The method comprises placing subcritical saturated solution with TPUx dissolved therein and TPUy particles into PTFE mold for shaping, then taking out oven-dried solvent, and selecting low-cost and environment-friendly CO 2 As a blowing agent, it is subjected to one-shot foam molding to form a TPU foam bead mixture. The invention provides a method for preparing TPU foaming bead mixture by combining solution compression molding and supercritical foaming technology, which does not need to use a steam bed to melt the surface of particles and then adhere the beads, can effectively improve the interfacial adhesion between TPU foaming beads, can eliminate unfoamed skin of the foaming beads, and realizes the secondary weight reduction of products.
Description
Technical Field
The invention relates to the field of polyurethane materials, in particular to a preparation method of a light high-marble foam sole for high-end sports shoes.
Background
Among the many elastomers, thermoplastic Polyurethane (TPU) has excellent physical properties such as abrasion resistance, toughness, tensile properties, and the like, and is a biodegradable material, and thus can replace many thermoplastic polymers. Since the institute of technology of the sesame-province first proposed the concept of microcellular foaming technology, more and more foaming materials are applied to actual production and life through the continuous perfection of the foaming technology and the improvement of the foaming products in the aspects of weight reduction, toughness enhancement, impact resistance, sound insulation and the like, and meanwhile, because the supercritical fluid foaming technology adopts CO 2 Or N 2 The production process is more environment-friendly and is more favored by people because the pollution-free gas is used as a foaming agent.
Thermoplastic polyurethane expanded beads (ETPU beads) have been widely used in the footwear industry due to their excellent light weight and high elastic properties. When TPU beads are prepared into soles, a two-step molding method is generally adopted, firstly, the TPU beads are put into a foaming kettle for foaming, then the foamed beads (ETPU beads) are taken out, and after the beads are not shrunk any more, the second-step molding process is carried out. Putting ETPU beads into a mould, introducing water vapor with a certain temperature, softening or melting the surfaces of the ETPU beads, and then performing compression molding, wherein in the compression molding process, the possibility that the interfaces of part of the beads cannot exhaust gas to cause trapping gas and holes appear. The uncompacted or fused bonded surfaces between the beads do not cool completely and open the mold causing gaps between the beads. Because the secondary steam mould pressing is to melt and weld the surfaces of ETPU beads together, cells near the surface skin are damaged, and the performance is affected. Meanwhile, the epidermis is not foamed, and further lightening of the product cannot be achieved. In the traditional steam molded product, a gap defect exists between two ETPU beads, an unfoamed skin layer exists (shown in figure 1), and a hole defect exists between three ETPU beads (shown in figure 2) through a field emission Scanning Electron Microscope (SEM), so that the mechanical properties of the product are affected.
Chinese patent application CN110126171a discloses an integrated foaming molding process of polymer particles, wherein a low-melting polymer is coated outside a high-melting polymer by two extruders to form a core-shell structure, and then underwater cutting and granulating are performed. And (3) placing the granulated particles into a mould for mould pressing and foaming, wherein the temperature is set at a temperature between the melting points of the two polymers, and melting the polymer shells with low melting points, so that the particles are mutually adhered, introducing a foaming agent, and releasing pressure and foaming after the particles are saturated for a certain time, and cooling to prepare the bead foam. However, the method has the requirement on the melting points of two polymers with core-shell structures (only a few polymers are used), and the polymer with a higher melting point can not be formed to cover the polymer with a lower melting point for compression molding foaming, so that the range of application of the method is limited. Because the method of melting the polymer with lower melting point is adopted to form the bead adhesion, if the melting point of the polymer is high, the use power of equipment is increased, the production cost is increased, and the type of the polymer is limited. In addition, the method has the defect that the interface adhesion is poor in the process of mutually fusing and bonding different core-shell particles, so that the mechanical and elastic properties of the product are affected.
Disclosure of Invention
The invention provides a preparation method of a lightweight high-elastic bead foam sole for high-end sports shoes, which is used for solving the interface problem among ETPU beads and realizing the aim of weight reduction again.
In order to achieve the above purpose, the invention adopts the following technical scheme:
a method for preparing a lightweight high-marble foam sole for high-end athletic shoes, comprising the following steps:
(1) Dissolving TPUx in N, N-Dimethylformamide (DMF) to obtain a TPUx subcritical saturated solution;
(2) Pouring the TPUx subcritical saturated solution into a PTFE (polytetrafluoroethylene) mould, and simultaneously putting TPUy particles;
(3) Putting the PTFE mould on a hot press for compression shaping;
(4) Taking out the TPU bead mixture after shaping from the PTFE mould, and putting the TPU bead mixture into an oven for drying to remove the solvent;
(5) And (3) putting the dried TPU bead mixture into a supercritical foaming kettle, heating, introducing supercritical gas for pressure maintaining, and then rapidly releasing pressure and cooling to obtain the TPU foaming bead mixture.
Further, TPUx, TPUy are different brands or same brands of TPU, which are dried to remove moisture prior to use.
In step (1), the dissolution is carried out in an oil bath at 80-82 ℃.
In the step (1), the weight ratio of TPUx to N, N-dimethylformamide is 2:2.8-3.2; the weight ratio of the TPUy in the step (2) to the TPUx in the step (1) is 5.8-6.2:1.
In the step (2), the concave die of the PTFE mold is attached with a groove of 10mm×10mm, the convex die is attached with a boss of 10mm×10mm×6mm, and the final molding size is a cuboid of 10mm×10mm×4mm.
In the step (3), the temperature of the hot press shaping is 80-82 ℃, the pressure is 5-5.5Mpa, and the shaping time is 30-35min.
In the step (5), CO is adopted as the supercritical gas 2 The foaming temperature is 90-92 ℃, the foaming pressure is 20-22Mpa, and the foaming time is 2-2.5 hours.
According to the invention, TPUx is dissolved in DMF through a solution method to form subcritical saturated solution, so that gel-like solid particles are formed, a certain amount of TPUy solid particles are placed in a self-made mold, a certain amount of subcritical saturated solution is poured into the mold to form a continuous phase (TPUx) and an island phase (TPUy), at the moment, unsaturated solvent in the subcritical saturated solution continuously dissolves the epidermis of a small amount of TPU particles, and the generation of holes or gaps among the beads is avoided. The original cell morphology is maintained after foaming, the cell damage to the nearby skin layer during steam mould pressing is avoided, and the bead skin layer disappears, so that the weight of the sample is reduced, the interface between the beads is also of a continuous cell structure, the cell morphology is adjustable, and therefore the sports sole with excellent mechanical properties, high elasticity, light weight, high performance and multifunction can be manufactured.
Compared with the polymer particle integrated foaming molding process disclosed in Chinese patent application CN110126171A, the method is not limited by the melting point of the polymer, and the polymer with high melting point can be used for coating the polymer with low melting point, and vice versa. The method expands the application range of bead foaming, is almost suitable for most thermoplastic polymer plastics, can prepare foam products with different purposes, and has wide application prospect.
The invention has the beneficial effects that:
1. the defect of interfaces among beads caused by the traditional secondary steam mould pressing is eliminated by a solution method, and the mechanical property of the product is improved;
3. according to the invention, the beads are adhered after the particle surfaces are melted by a vapor bed, so that the interfacial adhesion between TPU (thermoplastic polyurethane) foaming beads can be effectively improved, the unfoamed skin of the foaming beads can be eliminated, and the secondary weight reduction of the product is realized.
3. The invention eliminates the skin structure brought by melt molding, the interface bonding part between the beads is a continuous phase structure and is also in a foaming cell structure (big bubble or small bubble), the purpose of weight reduction again is realized, and the mechanical property of the product can be improved;
4. the equipment of the invention has low usage amount and cost;
5. the invention can realize the coating of the polymer with low melting point and the coating of the polymer with low melting point.
Drawings
FIG. 1 is a scanning electron microscope image of the interface between two ETPU beads in a foam prepared by conventional secondary steam molding.
FIG. 2 is a scanning electron microscope image of the interface between three ETPU beads in a foam prepared by conventional secondary steam molding.
FIG. 3 is a SEM image (200X) of the cross-sectional cell morphology of the TPU bead mixture foam prepared in example 3.
FIG. 4 is a SEM image (500X) of the cross-sectional cell morphology of the TPU bead mixture foam prepared in example 3.
FIG. 5 is a SEM image (2000X) of the cross-sectional cell morphology of the TPU bead mixture foam prepared in example 3.
FIG. 6 is a SEM image (5000X) of the cross-sectional cell morphology of the TPU bead mixture foam prepared in example 3.
Fig. 7 (a) is the 1 st and 50 th cycle compression curves of the TPU bead mixture foam prepared in example 3.
Fig. 7 (b) is the initial density and expansion ratio of the example 3 prepared TPU bead mixture foam.
Detailed Description
The invention is further illustrated by the following examples.
Example 1
A preparation method of a light high-elastic bead foam sole for high-end sports shoes comprises the steps of preparing raw materials of basf TPU1170A particles and N, N-dimethylformamide.
(1) The TPU1170A particles are put into a baking oven at 60 ℃ to be dried for 8 hours, and the moisture is removed;
(2) TPU1170A and N, N-dimethylformamide are poured into a beaker according to the weight ratio of 2:3, and then are put into an oil bath at 80 ℃ for dissolution, so as to obtain subcritical saturated solution;
(3) Pouring the subcritical saturated solution into a PTFE mold with molding size of 10mm multiplied by 4mm, then weighing a certain mass of TPU1170A particles, putting the TPU1170A particles into the PTFE mold, wherein the weight ratio of the TPU1170A particles in the step (3) to the TPU1170A particles in the step (2) is 6:1, and finally putting the PTFE mold into a hot press with the temperature of 80 ℃ and the pressure of 5MPa for 30 minutes to shape the TPU bead mixture;
(4) Taking out the shaped TPU bead mixture from the PTFE mold, and putting the TPU bead mixture into an oven at 60 ℃ for 48 hours to remove the N, N-dimethylformamide solvent;
(5) Taking out the dried TPU bead mixture, putting the TPU bead mixture into a foaming kettle, and using CO as supercritical fluid 2 The foaming temperature, pressure and time are 90 ℃, 20MPa and 2 hours respectively, and the foam is rapidly cooled and shaped in a cold water bath after pressure relief.
(6) And (3) soaking the TPU foaming bead mixture obtained in the step (5) in liquid nitrogen for 15 minutes, quenching, then carrying out surface metal spraying treatment, and observing the interface condition between the beads under a field emission scanning electron microscope.
Example 2
A preparation method of a light high-elastic bead foam sole for high-end sports shoes comprises the steps of raw materials including basf TPU1185A particles and N, N-dimethylformamide.
(1) Putting TPU1185A particles into a baking oven at 60 ℃ for drying for 8 hours, and removing water;
(2) TPU1185A and N, N-dimethylformamide are poured into a beaker according to the weight ratio of 2:3, and then are put into an oil bath at 80 ℃ for dissolution, so as to obtain subcritical saturated solution;
(3) Pouring the subcritical saturated solution into a PTFE mold with molding size of 10mm multiplied by 4mm, then weighing a certain mass of TPU1185A particles, putting the TPU1185A particles in the step (3) and the TPU1185A particles in the step (2) in a weight ratio of 6:1, and finally putting the PTFE mold into a hot press with the temperature of 80 ℃ and keeping the pressure of 5MPa for 30 minutes to shape the TPU bead mixture;
(4) Taking out the shaped TPU bead mixture from the PTFE mold, and putting the TPU bead mixture into an oven at 60 ℃ for 48 hours to remove the N, N-dimethylformamide solvent;
(5) Taking out the dried TPU bead mixture, putting the TPU bead mixture into a foaming kettle, and using CO as supercritical fluid 2 Foaming temperature, pressure and time are 90 ℃, 20MPa and 2 hours respectively, and unloading is carried outAnd after pressing, cooling and shaping in a cold water bath.
(6) The TPU foaming bead mixture in the step (5) is quenched after being soaked in liquid nitrogen for 15 minutes, then the surface is subjected to metal spraying treatment, and the interface condition among the beads is observed under a field emission scanning electron microscope.
Example 3
A preparation method of a light high-elastic bead foam sole for high-end sports shoes comprises the steps of preparing raw materials including basf TPU1170A particles, TPU1185A particles and N, N-Dimethylformamide (DMF).
(1) The TPU1170, A, TPU and 1185A particles are put into a baking oven at 60 ℃ to be dried for 8 hours, and the moisture is removed;
(2) TPU1185A and N, N-dimethylformamide are poured into a beaker according to the weight ratio of 2:3, and then are put into an oil bath at 80 ℃ for dissolution, so as to obtain subcritical saturated solution;
(3) Pouring the subcritical saturated solution into a PTFE mold with molding size of 10mm multiplied by 4mm, then weighing a certain mass of TPU1170A particles, putting the TPU1170A particles in the step (3) and the TPU1185A particles in the step (2) in a weight ratio of 6:1, and finally putting the PTFE mold into a hot press with the temperature of 80 ℃ and keeping the pressure of 5MPa for 30 minutes to shape the TPU bead mixture;
(4) Taking out the TPU bead mixture shaped in the step (3) from the PTFE mold, and putting the TPU bead mixture into an oven at 60 ℃ for 48 hours to remove the N, N-dimethylformamide solvent;
(5) Taking out the TPU bead mixture dried in the step (4), putting the TPU bead mixture into a foaming kettle, and adopting CO as a supercritical fluid 2 The foaming temperature, pressure and time are 90 ℃, 20MPa and 2 hours respectively, and the foam is rapidly cooled and shaped in a cold water bath after pressure relief.
(6) The TPU foaming bead mixture in the step (5) is quenched after being soaked in liquid nitrogen for 15 minutes, then the surface is subjected to metal spraying treatment, and the interface condition among the beads is observed under a field emission scanning electron microscope.
FIGS. 3-6 are scanning electron microscope images of cross-sections of TPU bead mixture foams prepared in this example at various magnifications (BASF TPU1170A bead phase, BASF TPU1185A subcritical solutionThe continuous foaming phase formed). FIG. 7 (a) is the 1 st and 50 th cycle compression curves of the TPU bead mixture foam prepared in this example; as can be seen from fig. 7 (a), after 50 cycles of compression, the maximum stress was reduced from 436KPa to 337KPa, the reduction was small, and the deviation of the compression and recovery curves was low, and the rebound and stability were excellent. Fig. 7 (b) is the initial density and expansion ratio of the TPU bead mixture foam prepared in this example. As can be seen from FIG. 7 (b), the bead mixture foam prepared in this way has a very low density (0.086 g/cm 3 ) And a higher expansion ratio (14.114). The results show that the TPU sole material prepared by the method has high elastic quality, light weight and excellent rebound resilience, and is suitable for the foam sole material of high-end sports shoes.
Example 4
A preparation method of a light high-elastic bead foam sole for high-end sports shoes, which comprises raw materials of basf TPU1170A particles, TPU1185A particles and N, N-dimethylformamide.
(1) The TPU1170, A, TPU and 1185A particles are put into a baking oven at 60 ℃ to be dried for 8 hours, and the moisture is removed;
(2) TPU1170A and N, N-dimethylformamide are poured into a beaker according to the volume ratio of 2:3, and then are put into an oil bath at 80 ℃ for dissolution, so as to obtain subcritical saturated solution;
(3) Pouring the subcritical saturated solution in the step (2) into a PTFE mold with molding size of 10mm multiplied by 4mm, then weighing a certain mass of TPU1185A particles, putting the TPU1185A particles in the step (3) and the TPU1170A particles in the step (2) in a weight ratio of 6:1, and finally putting the PTFE mold in a hot press with the temperature of 80 ℃ and keeping the pressure of 5MPa for 30 minutes to shape the TPU bead mixture;
(4) Taking out the shaped bead mixture in the step (3) from the PTFE mold, and putting the bead mixture into an oven at 60 ℃ for 48 hours to remove the N, N-dimethylformamide solvent;
(5) Taking out the TPU bead mixture dried in the step (4), putting the TPU bead mixture into a foaming kettle, and adopting CO as a supercritical fluid 2 Foaming temperature, pressure and time are 90 ℃, 20MPa and 2 hours respectivelyAnd after pressure relief, cooling and shaping in a cold water bath.
(6) The TPU foaming bead mixture in the step (5) is quenched after being soaked in liquid nitrogen for 15 minutes, then the surface is subjected to metal spraying treatment, and the interface condition among the beads is observed under a field emission scanning electron microscope.
The above embodiments are not intended to limit the form or style of the present invention, and any appropriate changes or modifications made by those skilled in the art should be construed as not departing from the scope of the present invention as claimed.
Claims (5)
1. A method for preparing a lightweight high-marble foam sole for a high-end athletic shoe, comprising the steps of:
(1) Dissolving TPUx in N, N-dimethylformamide to obtain a TPUx subcritical saturated solution;
the dissolution is carried out in an oil bath at 80-82 ℃, and the weight ratio of TPUx to N, N-dimethylformamide is 2:2.8-3.2;
(2) Pouring the TPUx subcritical saturated solution into a PTFE (polytetrafluoroethylene) mould, and simultaneously putting TPUy particles; TPUx and TPUy are TPU with different brands or the same brand, and the weight ratio of the TPUy to the TPUx is 5.8-6.2:1;
(3) Putting the PTFE mould on a hot press for compression shaping;
(4) Taking out the TPU bead mixture after shaping from the PTFE mould, and putting the TPU bead mixture into an oven for further drying to remove the solvent;
(5) And (3) putting the dried TPU bead mixture into a supercritical foaming kettle, heating, introducing supercritical gas for pressure maintaining, and then rapidly releasing pressure and cooling to obtain the TPU foaming bead mixture.
2. A method of making a lightweight high-marble foam sole for high-end athletic footwear according to claim 1, wherein the TPU is dried at 55-65 ℃ to remove moisture from 8-9 h prior to use.
3. The method for manufacturing a lightweight high-marble foam sole for high-end athletic shoes according to claim 1, wherein in the step (2), the molding size of the PTFE mold is 10mm x 4mm.
4. The method for preparing a lightweight high-marble foam sole for high-end athletic shoes according to claim 1, wherein in the step (3), the temperature of compression shaping is 80-82 ℃, the pressure is 5-5.5Mpa, and the shaping time is 30-35min.
5. The method for manufacturing a lightweight high-marble foam sole for high-end athletic shoes according to claim 1, wherein in step (5), supercritical gas is CO 2 The foaming temperature is 90-92 ℃, the foaming pressure is 20-22Mpa, and the gas soaking time is 2-2.5 hours.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105218850A (en) * | 2014-06-06 | 2016-01-06 | 茂泰(福建)鞋材有限公司 | The preparation method of a kind of high-elastic thermoplastic polyurethane foam's particle and formed body thereof |
| CN107283711A (en) * | 2017-07-12 | 2017-10-24 | 青岛中诚高分子科技有限公司 | A kind of thermoplastic polymer expanded bead formed body and preparation method thereof |
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| CN108081652B (en) * | 2018-01-08 | 2020-10-27 | 晋江兴迅新材料科技有限公司 | Preparation process of supercritical foaming sole |
| CN108559057B (en) * | 2018-05-03 | 2021-02-12 | 东莞市雄林新材料科技股份有限公司 | Novel composite foam material and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105218850A (en) * | 2014-06-06 | 2016-01-06 | 茂泰(福建)鞋材有限公司 | The preparation method of a kind of high-elastic thermoplastic polyurethane foam's particle and formed body thereof |
| CN107283711A (en) * | 2017-07-12 | 2017-10-24 | 青岛中诚高分子科技有限公司 | A kind of thermoplastic polymer expanded bead formed body and preparation method thereof |
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