CN113527754A - Preparation method of double-crosslinked aerogel material - Google Patents
Preparation method of double-crosslinked aerogel material Download PDFInfo
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- CN113527754A CN113527754A CN202010311741.7A CN202010311741A CN113527754A CN 113527754 A CN113527754 A CN 113527754A CN 202010311741 A CN202010311741 A CN 202010311741A CN 113527754 A CN113527754 A CN 113527754A
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- 239000004964 aerogel Substances 0.000 title claims abstract description 45
- 239000000463 material Substances 0.000 title claims abstract description 25
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims abstract description 24
- IMNFDUFMRHMDMM-UHFFFAOYSA-N N-Heptane Chemical compound CCCCCCC IMNFDUFMRHMDMM-UHFFFAOYSA-N 0.000 claims abstract description 21
- 238000001035 drying Methods 0.000 claims abstract description 17
- 239000002904 solvent Substances 0.000 claims abstract description 17
- WGTYBPLFGIVFAS-UHFFFAOYSA-M tetramethylammonium hydroxide Chemical compound [OH-].C[N+](C)(C)C WGTYBPLFGIVFAS-UHFFFAOYSA-M 0.000 claims abstract description 16
- 238000006243 chemical reaction Methods 0.000 claims abstract description 15
- 238000001723 curing Methods 0.000 claims abstract description 15
- 238000006116 polymerization reaction Methods 0.000 claims abstract description 12
- 238000004132 cross linking Methods 0.000 claims abstract description 8
- 238000002156 mixing Methods 0.000 claims abstract description 8
- 239000002243 precursor Substances 0.000 claims abstract description 8
- LSXWFXONGKSEMY-UHFFFAOYSA-N di-tert-butyl peroxide Chemical compound CC(C)(C)OOC(C)(C)C LSXWFXONGKSEMY-UHFFFAOYSA-N 0.000 claims abstract description 7
- ZLNAFSPCNATQPQ-UHFFFAOYSA-N ethenyl-dimethoxy-methylsilane Chemical compound CO[Si](C)(OC)C=C ZLNAFSPCNATQPQ-UHFFFAOYSA-N 0.000 claims abstract description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000003999 initiator Substances 0.000 claims abstract description 5
- 239000000203 mixture Substances 0.000 claims abstract description 5
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims abstract description 5
- ZFSFDELZPURLKD-UHFFFAOYSA-N azanium;hydroxide;hydrate Chemical compound N.O.O ZFSFDELZPURLKD-UHFFFAOYSA-N 0.000 claims abstract description 3
- 238000001816 cooling Methods 0.000 claims abstract description 3
- 238000007789 sealing Methods 0.000 claims abstract description 3
- 238000003756 stirring Methods 0.000 claims abstract description 3
- 238000000034 method Methods 0.000 claims description 12
- 230000009977 dual effect Effects 0.000 claims description 8
- 238000011415 microwave curing Methods 0.000 claims description 5
- 125000000956 methoxy group Chemical group [H]C([H])([H])O* 0.000 claims description 2
- 238000000352 supercritical drying Methods 0.000 claims description 2
- 238000007086 side reaction Methods 0.000 abstract description 2
- 229920002554 vinyl polymer Polymers 0.000 abstract description 2
- GRVDJDISBSALJP-UHFFFAOYSA-N methyloxidanyl Chemical group [O]C GRVDJDISBSALJP-UHFFFAOYSA-N 0.000 abstract 1
- 239000011148 porous material Substances 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 238000006467 substitution reaction Methods 0.000 description 2
- 239000004965 Silica aerogel Substances 0.000 description 1
- 150000001336 alkenes Chemical group 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000010382 chemical cross-linking Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000001879 gelation Methods 0.000 description 1
- 230000003301 hydrolyzing effect Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229920000620 organic polymer Polymers 0.000 description 1
- 238000006068 polycondensation reaction Methods 0.000 description 1
- -1 polyethylene chains Polymers 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 230000002787 reinforcement Effects 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
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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
- C08J9/28—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof by elimination of a liquid phase from a macromolecular composition or article, e.g. drying of coagulum
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F130/00—Homopolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and containing phosphorus, selenium, tellurium or a metal
- C08F130/04—Homopolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and containing phosphorus, selenium, tellurium or a metal containing a metal
- C08F130/08—Homopolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and containing phosphorus, selenium, tellurium or a metal containing a metal containing silicon
-
- 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
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/24—Crosslinking, e.g. vulcanising, of macromolecules
-
- 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
- C08J2201/00—Foams characterised by the foaming process
- C08J2201/04—Foams characterised by the foaming process characterised by the elimination of a liquid or solid component, e.g. precipitation, leaching out, evaporation
- C08J2201/05—Elimination by evaporation or heat degradation of a liquid phase
- C08J2201/0502—Elimination by evaporation or heat degradation of a liquid phase the liquid phase being organic
-
- 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
- C08J2205/00—Foams characterised by their properties
- C08J2205/02—Foams characterised by their properties the finished foam itself being a gel or a gel being temporarily formed when processing the foamable composition
- C08J2205/026—Aerogel, i.e. a supercritically dried gel
-
- 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
- C08J2343/00—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 containing boron, silicon, phosphorus, selenium, tellurium or a metal; Derivatives of such polymers
- C08J2343/04—Homopolymers or copolymers of monomers containing silicon
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- Chemical & Material Sciences (AREA)
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- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
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- Materials Engineering (AREA)
- Processes Of Treating Macromolecular Substances (AREA)
- Silicon Polymers (AREA)
Abstract
The invention discloses a preparation method of a double-crosslinking aerogel material, which comprises the following steps: vinyl polymerization, namely mixing and stirring a precursor methyl vinyl dimethoxysilane and an initiator di-tert-butyl peroxide, then pouring the mixture into a high-temperature reaction kettle for reaction, and cooling the product along with the reaction kettle and then sealing and storing the product; polymerization, curing and drying of methoxyl, evenly mixing the product obtained in the last step, water and tetramethyl ammonium hydroxide, and then curing; adding isopropanol into the obtained gel to perform solvent replacement, wherein the solvent replacement is performed at least twice; adding n-heptane into the gel after isopropanol replacement to perform solvent replacement at least twice; and drying the gel again to obtain the double-crosslinked aerogel. In such a way, compared with the traditional aerogel, the aerogel product prepared by the preparation method disclosed by the invention has high elasticity and high transparency; and the preparation process is simple and clear, and the occurrence of side reaction is effectively avoided.
Description
Technical Field
The invention relates to a preparation method of a double-crosslinking aerogel material.
Background
The double-crosslinked aerogel is an aerogel which uses only one precursor to initiate the precursor to perform polymerization reaction or directly perform polymerization reaction with each other. Because the whole process comprises two times of polymerization reactions, the structure of the double-crosslinked aerogel has a more concise and ordered three-dimensional network structure than the traditional aerogel, so that the double-crosslinked aerogel has higher elasticity and better transparency than the traditional aerogel.
In general, silica aerogels have poor mechanical properties, and polymerization of precursors containing olefin groups is another effective way to improve the mechanical properties of aerogels. Polymerization of vinyl groups in the polyvinylsilsesquioxane gel network also results in mechanically reinforced aerogels. Up to now, the polymerization reinforcement on silica-based aerogels has mostly been as a post-gelation process, and the polyethylene chains connecting the siloxane bonds in the network provide flexibility to the hybrid gel. In addition, the organic polymer gel with a double-network structure, high mechanical strength and strong flexibility can be synthesized through vinyl polymerization, the obtained gel comprises two interpenetrating polymer networks, and no chemical crosslinking exists between the two networks. Such networks can be obtained by polymerization of the various groups, followed by hydrolytic polycondensation of the organoalkoxysilanes of the particular olefinic group. However, there is no report on the preparation of aerogels by this method.
Disclosure of Invention
The invention mainly solves the technical problem of providing a method for manufacturing a double-crosslinking aerogel material which is different from the traditional aerogel material and has the characteristics of high elasticity, high transparency and the like.
In order to solve the technical problems, the invention adopts a technical scheme that: the preparation method of the double-crosslinking aerogel material comprises the following steps:
1) polymerisation of vinyl groups
Mixing and stirring a precursor methylvinyldimethoxysilane and an initiator di-tert-butyl peroxide, then pouring the mixture into a high-temperature reaction kettle for reaction, and cooling the product along with the reaction kettle and then sealing and storing the product;
2) polymerization, curing and drying of methoxy groups
Uniformly mixing the product obtained in the step 1), water and tetramethylammonium hydroxide, and then curing; adding isopropanol into the obtained gel to perform solvent replacement, wherein the solvent replacement is performed at least twice; adding n-heptane into the gel after isopropanol replacement to perform solvent replacement at least twice; and drying the gel again to obtain the double-crosslinked aerogel.
In a preferred embodiment of the invention, the ratio of the precursor methylvinyldimethoxysilane to the initiator di-tert-butyl peroxide in the step 1) is 600: 1.
In a preferred embodiment of the present invention, the ratio of water to tetramethylammonium hydroxide in step 2) is 16: 1.
in a preferred embodiment of the present invention, the curing in step 2) comprises oven curing or microwave curing.
In a preferred embodiment of the present invention, the dehumidifying rate of the microwave curing is 20%, the microwave power is 250W, and the curing time is 5 min.
In a preferred embodiment of the present invention, the drying includes atmospheric drying, microwave drying or supercritical drying.
In a preferred embodiment of the present invention, the microwave power of the microwave dryer is 700 w, the drying time is 18min, and the dehumidifying rate is 90%.
In a preferred embodiment of the present invention, in step 2), the temperature for solvent replacement by adding isopropanol to the gel is 60 ℃, and the replacement time is 12 h.
In a preferred embodiment of the present invention, in step 2), the temperature at which the solvent substitution is carried out by adding n-heptane to the gel is 60 ℃ and the substitution time is 12 hours.
The invention has the beneficial effects that: compared with the traditional aerogel, the aerogel product prepared by the preparation method has high elasticity and high transparency; and the preparation process is simple and clear, and the occurrence of side reaction is effectively avoided.
Drawings
In order to more clearly illustrate the technical solutions in the embodiments of the present invention, the drawings needed to be used in the description of the embodiments are briefly introduced below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and other drawings can be obtained by those skilled in the art without inventive efforts, wherein:
FIG. 1 is an SEM photograph of a dual cross-linked aerogel material prepared in example 1;
FIG. 2 is an SEM photograph of a dual cross-linked aerogel material prepared in example 2;
FIG. 3 is an SEM photograph of a dual cross-linked aerogel material prepared by a comparative example.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are some, but not all, embodiments of the present invention. The components of embodiments of the present invention generally described and illustrated in the figures herein may be arranged and designed in a wide variety of different configurations.
Thus, the following detailed description of the embodiments of the present invention, presented in the figures, is not intended to limit the scope of the invention, as claimed, but is merely representative of selected embodiments of the invention. 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.
It should be noted that: like reference numbers and letters refer to like items in the following figures, and thus, once an item is defined in one figure, it need not be further defined and explained in subsequent figures.
In the description of the present invention, it should be noted that the terms "front" and "back" and the like indicate orientations and positional relationships based on orientations and positional relationships shown in the drawings or orientations and positional relationships where the products of the present invention are conventionally placed in use, and are used for convenience in describing the present invention and simplifying the description, but do not indicate or imply that the devices or elements to be referred must have a specific orientation, be constructed in a specific orientation, and be operated, and thus should not be construed as limiting the present invention. Furthermore, the terms "first," "second," and the like are used merely to distinguish one description from another, and are not to be construed as indicating or implying relative importance.
In the description of the present invention, it should also be noted that, unless otherwise explicitly specified or limited, the terms "disposed" and "connected" are to be interpreted broadly, e.g., as being either fixedly connected, detachably connected, or integrally connected; can be mechanically or electrically connected; they may be connected directly or indirectly through intervening media, or they may be interconnected between two elements. The specific meanings of the above terms in the present invention can be understood in specific cases to those skilled in the art.
In the present invention, unless otherwise expressly stated or limited, the first feature may be present on or under the second feature in direct contact with the first and second feature, or may be present in the first and second feature not in direct contact but in contact with another feature between them. Also, the first feature being above, on or above the second feature includes the first feature being directly above and obliquely above the second feature, or merely means that the first feature is at a higher level than the second feature. A first feature that underlies, and underlies a second feature includes a first feature that is directly under and obliquely under a second feature, or simply means that the first feature is at a lesser level than the second feature.
The embodiment of the invention comprises the following steps:
example 1: a preparation method of a double-crosslinking aerogel material comprises the following steps:
1) 60 mL of methylvinyldimethoxysilane and 0.1 mL of di-tert-butyl peroxide are mixed and stirred, then poured into a high-temperature reaction kettle for reaction for 48 hours, and the product is sealed and stored after being cooled down along with the reaction kettle.
2) Mixing the product obtained in the first step with 40g of water and 2.5g of tetramethylammonium hydroxide, and then placing the mixture in a microwave heating chamber for microwave curing, wherein the dehumidifying rate is set to be 20%, the microwave power is 250W, and the curing time is 5 min; adding isopropanol into the obtained gel to perform solvent replacement, wherein the temperature is 60 ℃, the replacement time is 12 hours, and the replacement is performed twice; adding n-heptane into the gel after isopropanol replacement to perform solvent replacement, wherein the temperature is 60 ℃, the replacement time is 12 h, and the replacement is performed twice. And (3) placing the gel in a microwave heating chamber for microwave drying, wherein the dehumidifying rate is set to be 90%, the microwave power is set to be 700W, and the drying time is set to be 18min, so that the double-crosslinked aerogel is prepared, as shown in figure 1.
The double-crosslinked aerogel material prepared by the embodiment has the advantages of rich pores, uniform appearance, high elasticity and high transparency.
Example 2: a preparation method of a double-crosslinking aerogel material comprises the following steps:
1) 120 mL of methyl vinyl dimethoxy silane and 0.2 mL of di-tert-butyl peroxide are mixed and stirred, then poured into a high-temperature reaction kettle for reaction for 48 hours, and the product is sealed and stored after being cooled down along with the reaction kettle.
2) Mixing the product obtained in the first step with 32g of water and 2g of tetramethylammonium hydroxide, and then placing the mixture in an oven for curing, wherein the temperature of the oven is set to be 120 ℃, and the curing time is set to be 5 min; adding isopropanol into the obtained gel to perform solvent replacement, wherein the temperature is 60 ℃, the replacement time is 12 hours, and the replacement is performed for three times; adding n-heptane into the gel after isopropanol replacement to perform solvent replacement, wherein the temperature is 60 ℃, the replacement time is 12 h, and the replacement is performed three times in total. Drying the gel at normal pressure for 60min to obtain the double-crosslinked aerogel, as shown in FIG. 2.
The double-crosslinked aerogel material prepared by the embodiment has the advantages of rich pores, uniform appearance, high elasticity and high transparency.
Example 3: a preparation method of a double-crosslinked aerogel material is to change the mass of tetramethylammonium hydroxide in the step (2) in the example 1 into 3.0g, and the rest is the same as the example 1 to prepare the double-crosslinked aerogel, as shown in figure 3.
The double-crosslinked aerogel material prepared by the embodiment has the advantages of rare pores, uniform appearance, no elasticity and low transparency.
The above description is only an embodiment of the present invention, and not intended to limit the scope of the present invention, and all modifications of equivalent structures and equivalent processes, which are made by the present specification, or directly or indirectly applied to other related technical fields, are included in the scope of the present invention.
Claims (9)
1. A preparation method of a double-crosslinking aerogel material is characterized by comprising the following steps:
1) polymerisation of vinyl groups
Mixing and stirring a precursor methylvinyldimethoxysilane and an initiator di-tert-butyl peroxide, then pouring the mixture into a high-temperature reaction kettle for reaction, and cooling the product along with the reaction kettle and then sealing and storing the product;
2) polymerization, curing and drying of methoxy groups
Uniformly mixing the product obtained in the step 1), water and tetramethylammonium hydroxide, and then curing; adding isopropanol into the obtained gel to perform solvent replacement, wherein the solvent replacement is performed at least twice; adding n-heptane into the gel after isopropanol replacement to perform solvent replacement at least twice; and drying the gel again to obtain the double-crosslinked aerogel.
2. The preparation method of the double-crosslinking aerogel material as claimed in claim 1, wherein the ratio of the precursor methylvinyldimethoxysilane to the initiator di-tert-butyl peroxide in the step 1) is 600: 1.
3. The method for preparing a double-crosslinked aerogel material according to claim 1, wherein the ratio of water to tetramethylammonium hydroxide in step 2) is 16: 1.
4. the method for preparing a dual crosslinked aerogel material according to claim 1, wherein the curing in step 2) comprises oven curing or microwave curing.
5. The method for preparing a dual crosslinked aerogel material according to claim 4, wherein the microwave curing has a dehumidifying rate of 20%, a microwave power of 250W, and a curing time of 5 min.
6. The method of preparing a dual crosslinked aerogel material of claim 1, wherein drying comprises atmospheric drying, microwave drying, or supercritical drying.
7. The method for preparing a dual crosslinked aerogel material according to claim 6, wherein the microwave power of the microwave dryer is 700 w, the drying time is 18min, and the dehumidifying rate is 90%.
8. The method for preparing the double-crosslinked aerogel material according to claim 1, wherein the temperature for solvent replacement by adding isopropanol into the gel in the step 2) is 60 ℃, and the replacement time is 12 h.
9. The method of preparing a dual crosslinked aerogel material according to claim 1,
in the step 2), the temperature of adding n-heptane into the gel for solvent replacement is 60 ℃, and the replacement time is 12 h.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115449118A (en) * | 2022-10-24 | 2022-12-09 | 晋江市民富鞋材有限公司 | Light wear-resistant polyurethane sole and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109485905A (en) * | 2018-11-26 | 2019-03-19 | 淮阴工学院 | A kind of double cross-linked network silica-based aerogels and preparation method thereof |
| CN109796018A (en) * | 2019-01-29 | 2019-05-24 | 同济大学 | A kind of preparation method of elasticity double cross connection aeroge |
| CN110945064A (en) * | 2017-08-25 | 2020-03-31 | 国立大学法人京都大学 | Low density gel and method of making same |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110945064A (en) * | 2017-08-25 | 2020-03-31 | 国立大学法人京都大学 | Low density gel and method of making same |
| CN109485905A (en) * | 2018-11-26 | 2019-03-19 | 淮阴工学院 | A kind of double cross-linked network silica-based aerogels and preparation method thereof |
| CN109796018A (en) * | 2019-01-29 | 2019-05-24 | 同济大学 | A kind of preparation method of elasticity double cross connection aeroge |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115449118A (en) * | 2022-10-24 | 2022-12-09 | 晋江市民富鞋材有限公司 | Light wear-resistant polyurethane sole and preparation method thereof |
| CN115449118B (en) * | 2022-10-24 | 2024-01-02 | 浙江佰顺鞋业有限公司 | Light wear-resistant polyurethane sole and preparation method thereof |
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Application publication date: 20211022 |