CN115057987A - Formula and preparation method of low-temperature-resistant transparent TPU film - Google Patents
Formula and preparation method of low-temperature-resistant transparent TPU film Download PDFInfo
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- CN115057987A CN115057987A CN202210785402.1A CN202210785402A CN115057987A CN 115057987 A CN115057987 A CN 115057987A CN 202210785402 A CN202210785402 A CN 202210785402A CN 115057987 A CN115057987 A CN 115057987A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/65—Low-molecular-weight compounds having active hydrogen with high-molecular-weight compounds having active hydrogen
- C08G18/66—Compounds of groups C08G18/42, C08G18/48, or C08G18/52
- C08G18/6666—Compounds of group C08G18/48 or C08G18/52
- C08G18/667—Compounds of group C08G18/48 or C08G18/52 with compounds of group C08G18/32 or polyamines of C08G18/38
- C08G18/6674—Compounds of group C08G18/48 or C08G18/52 with compounds of group C08G18/32 or polyamines of C08G18/38 with compounds of group C08G18/3203
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/30—Low-molecular-weight compounds
- C08G18/32—Polyhydroxy compounds; Polyamines; Hydroxyamines
- C08G18/3203—Polyhydroxy compounds
- C08G18/3206—Polyhydroxy compounds aliphatic
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/40—High-molecular-weight compounds
- C08G18/48—Polyethers
- C08G18/4854—Polyethers containing oxyalkylene groups having four carbon atoms in the alkylene group
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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
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
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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
- C08J2375/08—Polyurethanes from polyethers
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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
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A40/00—Adaptation technologies in agriculture, forestry, livestock or agroalimentary production
- Y02A40/10—Adaptation technologies in agriculture, forestry, livestock or agroalimentary production in agriculture
- Y02A40/25—Greenhouse technology, e.g. cooling systems therefor
Abstract
The application relates to a formula of a low-temperature-resistant transparent TPU film and a preparation method thereof. The formula comprises the following components in percentage by weight: 25% -35% of aliphatic isocyanate; 60% -70% polytetrahydrofuran ether glycol; 0 to 15 percent of micromolecule chain extender. The preparation method comprises the following steps: (a) weighing the raw materials according to the formula; (b) dehydrating polytetrahydrofuran ether glycol in vacuum; (c) uniformly mixing aliphatic isocyanate and dehydrated polytetrahydrofuran ether glycol, and heating and stirring to obtain a first material; (d) heating the micromolecule chain extender to obtain a second material; (e) mixing the first material and the second material, and stirring until the mixture is clear to obtain a castable; (f) pouring the casting material into a mould, solidifying at high temperature in stages, and removing the mould to obtain the low-temperature-resistant transparent TPU film which has better flexibility at the temperature of minus 20 ℃ and still has lower hardness at the temperature of minus 50 ℃.
Description
Technical Field
The application relates to a TPU film, in particular to a formula of a low-temperature-resistant transparent TPU film and a preparation method thereof.
Background
The Thermoplastic polyurethane elastomer rubber (TPU) film is a Thermoplastic polyurethane functional film, has the characteristics of high strength, good toughness, cold resistance, oil resistance, aging resistance, environmental protection, no toxicity, degradability and the like, and can be widely applied to various fields.
In the process of implementing the present application, the applicant finds that the hardness of the existing TPU film can be greatly improved at a low temperature, and in order to reduce the hardness of the TPU film at the low temperature, a common method is to add a plasticizer, a softener, etc. in the preparation process of the TPU film, but the effect of the prepared TPU film at the low temperature is not obvious, so that a TPU film capable of maintaining a certain physical property (higher hardness) at the low temperature is urgently needed.
Disclosure of Invention
The embodiment of the application provides a formula of a low-temperature-resistant transparent TPU film and a preparation method thereof, and solves the problem that the existing TPU film is high in hardness at low temperature.
In order to solve the above technical problem, the present application is implemented as follows:
in a first aspect, a formula of a low temperature resistant transparent TPU film is provided, which comprises the following components in percentage by weight: 25% -35% of aliphatic isocyanate; 60% -70% polytetrahydrofuran ether glycol; 0 to 15 percent of micromolecule chain extender.
In a first possible implementation of the first aspect, the aliphatic isocyanate comprises one or more of isophorone diisocyanate, dicyclohexylmethane diisocyanate, hexamethylene diisocyanate, hydrogenated m-xylylene isocyanate.
In a second possible implementation form of the first aspect, the polytetrahydrofuran ether glycol has a molecular weight of 1000.
In a third possible implementation of the first aspect, the small molecule chain extender comprises one or more of ethylene glycol, propylene glycol, 1, 4-butanediol, diethylene glycol, 1, 3-butanediol, 1, 5-pentanediol, methyl propylene glycol, or diethylene glycol (diethylene glycol).
In a second aspect, a preparation method of a low temperature resistant transparent TPU film is provided, which comprises the following steps: (a) weighing the raw materials according to the formula of the low-temperature-resistant transparent TPU film in any one of the first aspect; (b) dehydrating polytetrahydrofuran ether glycol in vacuum to ensure that the mass fraction of water is less than or equal to 0.05 percent; (c) uniformly mixing aliphatic isocyanate and dehydrated polytetrahydrofuran ether glycol, and heating and stirring to obtain a first material; (d) heating the micromolecule chain extender to obtain a second material; (e) mixing the first material and the second material, and stirring until the mixture is clear to obtain a castable; (f) pouring the casting material into a mold, curing at high temperature in stages, and removing the mold to obtain the low-temperature-resistant transparent TPU film.
In a first possible implementation manner of the second aspect, in the step (b), during vacuum dehydration, the polytetrahydrofuran ether glycol is added into a three-neck flask provided with a stirrer and a thermometer, and the polytetrahydrofuran ether glycol is heated and stirred for dehydration.
With reference to the first possible implementation manner of the second aspect, in a second possible implementation manner of the second aspect, the heating temperature of the polytetrahydrofuran ether glycol is 100-.
In a third possible implementation manner of the second aspect, in the step (c), the heating and stirring temperature of the aliphatic isocyanate and the polytetrahydrofuran ether glycol is 120 ℃ and the time is 2-3 h.
In a fourth possible implementation manner of the second aspect, in the step (d), the heating temperature of the small molecule chain extender is 120 ℃.
In a fifth possible implementation manner of the second aspect, in the step (f), during the step of high-temperature stage curing, the curing is performed in stages by heating 120 ℃ and keeping the temperature for 4 hours, heating 160 ℃ and keeping the temperature for 6 hours, heating 80 ℃ and keeping the temperature for 12 hours.
Compared with the prior art, the application has the advantages that:
according to the formula and the preparation method of the low-temperature-resistant transparent TPU film, the prepared low-temperature-resistant transparent TPU film has good flexibility at the temperature of-20 ℃ and still has low hardness at the temperature of-50 ℃.
Drawings
The accompanying drawings, which are included to provide a further understanding of the application and are incorporated in and constitute a part of this application, illustrate embodiment(s) of the application and together with the description serve to explain the application and not to limit the application. In the drawings:
fig. 1 is a flow chart illustrating the steps of a method for preparing a low temperature resistant transparent TPU film according to an embodiment of the present application. .
Detailed Description
To make the objects, technical solutions and advantages of the present application more clear, embodiments of the present application will be described in further detail below with reference to the accompanying drawings.
Example 1
Weighing the following components in percentage by weight: 31% of diisocyanate; 65% polytetrahydrofuran ether glycol 1000; 2% of 1, 4-butanediol and 2% of ethylene glycol.
Please refer to fig. 1, which is a flowchart illustrating steps of a method for manufacturing a low temperature resistant transparent TPU film according to an embodiment of the present application. The preparation method S of the low-temperature-resistant transparent TPU film comprises the following steps S1 to S5. Wherein:
in step S1, polytetrahydrofuran ether glycol is dehydrated in vacuum so that the mass fraction of water is 0.05% or less. Specifically, the polytetrahydrofuran ether glycol 1000 is added into a three-neck flask provided with a stirrer and a thermometer, heated to 110 ℃, dehydrated for 2-3h under vacuum, the mass fraction of water in the polytetrahydrofuran ether glycol 1000 is not higher than 0.05 percent, and cooled to 100 ℃ for standby.
In step S2, the aliphatic isocyanate and the dehydrated polytetrahydrofuran ether glycol are uniformly mixed, heated and stirred to obtain a first material. Specifically, adding the dehydrated polytetrahydrofuran ether glycol 1000 obtained in the step S1 into metered diisocyanate, keeping the temperature at 120 ℃, heating and stirring for reaction for 2-3 hours, and obtaining a first material for later use after the theoretical NCO content is reached.
In step S3, the small molecule chain extender is heated to obtain the second material. Specifically, 1, 4-butanediol and ethylene glycol are mixed and heated at 120 ℃ to obtain a second material for later use.
In step S4, the first material and the second material are mixed and stirred until they are clear, so as to obtain the castable. Specifically, the second material and the first material are added into a three-neck flask, and the first material and the second material are stirred by a stirrer in the three-neck flask until the materials are clear, so that the castable is obtained.
In step S5, the casting material is poured into a mold, and the mold is cured at high temperature, and then the low temperature resistant transparent TPU film is obtained after the mold is removed. Specifically, pouring the casting material into a flat plate-shaped mold, solidifying stage by stage according to the modes of heating at 120 ℃, preserving heat for 4h, heating at 160 ℃, preserving heat for 6h, heating at 80 ℃ and preserving heat for 12h, cooling and demolding to obtain the low-temperature-resistant transparent TPU film.
The performance of the low temperature resistant transparent TPU film prepared by the method is tested, and the test data is as follows:
1. the light transmittance of the low-temperature-resistant transparent TPU film is 91%, the hardness is 62A, the bonding strength is 5Mpa, the tensile strength is 11Mpa, and the TPU film is not broken when stretched to an extreme position;
2. the hardness of the low-temperature-resistant transparent TPU film is 68A, the tensile strength is 4MPa, and the TPU film is not broken when stretched to a limit position at the temperature of-20 ℃;
3. the hardness of the low-temperature resistant transparent TPU film is 92A at the temperature of-50 ℃.
Example 2
Weighing the following components in percentage by weight: 31% of diisocyanate; 65% polytetrahydrofuran ether glycol 1000; 2% of 1, 5-pentanediol and 2% of ethylene glycol.
Please refer to fig. 1, which is a flowchart illustrating steps of a method for manufacturing a low temperature resistant transparent TPU film according to an embodiment of the present application. The preparation method S of the low-temperature-resistant transparent TPU film comprises the following steps S1 to S5. Wherein:
in step S1, polytetrahydrofuran ether glycol is dehydrated in vacuum so that the mass fraction of water is 0.05% or less. Specifically, the polytetrahydrofuran ether glycol 1000 is added into a three-neck flask provided with a stirrer and a thermometer, heated to 110 ℃, dehydrated for 2-3h under vacuum, the mass fraction of water in the polytetrahydrofuran ether glycol 1000 is not higher than 0.05 percent, and cooled to 100 ℃ for standby.
In step S2, the aliphatic isocyanate and the dehydrated polytetrahydrofuran ether glycol are uniformly mixed, heated and stirred to obtain a first material. Specifically, adding the dehydrated polytetrahydrofuran ether glycol 1000 obtained in the step S1 into metered diisocyanate, keeping the temperature at 120 ℃, heating and stirring for reaction for 2-3 hours, and obtaining a first material for later use after the theoretical NCO content is reached.
In step S3, the small molecule chain extender is heated to obtain the second material. Specifically, 1, 5-pentanediol and ethylene glycol are mixed and heated at 120 ℃ to obtain a second material for later use.
In step S4, the first material and the second material are mixed and stirred until they are clear, so as to obtain the castable. Specifically, the second material and the first material are added into a three-neck flask, and the first material and the second material are stirred by a stirrer in the three-neck flask until the materials are clear, so that the castable is obtained.
In step S5, the casting material is poured into a mold, and the mold is cured at high temperature, and then the low temperature resistant transparent TPU film is obtained after the mold is removed. Specifically, pouring the casting material into a flat plate-shaped mold, solidifying stage by stage according to the modes of heating at 120 ℃, preserving heat for 4h, heating at 160 ℃, preserving heat for 6h, heating at 80 ℃ and preserving heat for 12h, cooling and demolding to obtain the low-temperature-resistant transparent TPU film.
The performance of the low temperature resistant transparent TPU film prepared by the method is tested, and the test data is as follows:
1. the light transmittance of the low-temperature-resistant transparent TPU film is 91%, the hardness is 57A, the tensile strength is 5Mpa, and the TPU film is not broken when stretched to a limit position;
2. the hardness of the low-temperature-resistant transparent TPU film is 66A at the temperature of minus 20 ℃;
3. the hardness of the low-temperature resistant transparent TPU film is 94A at the temperature of-50 ℃.
By combining the test results of the above example 1 and example 2, it can be seen that the low temperature resistant transparent TPU film prepared according to the formula and the preparation method of the low temperature resistant transparent TPU film of the present application has good physical properties at room temperature, good flexibility at-20 ℃, and still has low hardness at-50 ℃.
In summary, the application provides a formula of a low-temperature-resistant transparent TPU film and a preparation method thereof. The low-temperature-resistant transparent TPU film prepared by the method has good flexibility at the temperature of-20 ℃ and still has low hardness at the temperature of-50 ℃.
It should be noted that, in this document, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus. Without further limitation, an element defined by the phrase "comprising an … …" does not exclude the presence of other like elements in a process, method, article, or apparatus that comprises the element.
While the present embodiments have been described with reference to the accompanying drawings, it is to be understood that the invention is not limited to the precise embodiments described above, which are meant to be illustrative and not restrictive, and that various changes may be made therein by those skilled in the art without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (10)
1. The formula of the low-temperature-resistant transparent TPU film is characterized by comprising the following components in percentage by weight:
25% -35% of aliphatic isocyanate;
60% -70% polytetrahydrofuran ether glycol;
0 to 15 percent of micromolecule chain extender.
2. The formulation of low temperature resistant transparent TPU film according to claim 1, wherein the aliphatic isocyanate comprises one or more of isophorone diisocyanate, dicyclohexylmethane diisocyanate, hexamethylene diisocyanate, hydrogenated m-xylylene isocyanate.
3. The formulation of low temperature resistant transparent TPU film according to claim 1 where the polytetrahydrofuran ether glycol has a molecular weight of 1000.
4. The formulation of low temperature resistant transparent TPU film according to claim 1, where the small molecule chain extender comprises one or more of ethylene glycol, propylene glycol, 1, 4-butanediol, diethylene glycol, 1, 3-butanediol, 1, 5-pentanediol, methyl propylene glycol, or diethylene glycol (diethylene glycol).
5. A preparation method of a low-temperature-resistant transparent TPU film is characterized by comprising the following steps:
(a) weighing the raw materials according to the formula of the low-temperature-resistant transparent TPU film as defined in any one of claims 1 to 4;
(b) dehydrating the polytetrahydrofuran ether glycol in vacuum to ensure that the mass fraction of water is less than or equal to 0.05 percent;
(c) uniformly mixing the aliphatic isocyanate and the dehydrated polytetrahydrofuran ether glycol, and heating and stirring to obtain a first material;
(d) heating the micromolecule chain extender to obtain a second material;
(e) mixing the first material and the second material, and stirring until the mixture is clear to obtain a castable;
(f) and pouring the castable into a mold, curing at high temperature in stages, and removing the mold to obtain the low-temperature-resistant transparent TPU film.
6. The method for preparing a low temperature resistant transparent TPU film according to claim 5, wherein in the step (b), the polytetrahydrofuran ether glycol is added to a three-neck flask equipped with a stirrer and a thermometer during vacuum dehydration, and the polytetrahydrofuran ether glycol is heated and stirred for dehydration.
7. The method for preparing the low temperature resistant transparent TPU film as claimed in claim 6, wherein the polytetrahydrofuran ether glycol is heated at a temperature of 100 ℃ and 110 ℃ and the vacuum dehydration time is 2-3 h.
8. The method for preparing a low temperature resistant transparent TPU film of claim 5, wherein in step (c), the heating and stirring temperature of the aliphatic isocyanate and the polytetrahydrofuran ether glycol is 120 ℃ for 2-3 h.
9. The method for preparing a low temperature resistant transparent TPU film as claimed in claim 5, wherein in step (d), the heating temperature of the small molecule chain extender is 120 ℃.
10. The method for preparing a low temperature resistant transparent TPU film according to claim 5, wherein in the step (f), the step of high temperature curing is carried out by heating at 120 ℃ for 4 hours, heating at 160 ℃ for 6 hours, heating at 80 ℃ for 12 hours.
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| CN202210785402.1A CN115057987B (en) | 2022-07-05 | 2022-07-05 | Formula of low-temperature-resistant transparent TPU film and preparation method thereof |
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| CN202210785402.1A CN115057987B (en) | 2022-07-05 | 2022-07-05 | Formula of low-temperature-resistant transparent TPU film and preparation method thereof |
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| CN115057987B CN115057987B (en) | 2023-05-23 |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20090104449A1 (en) * | 2005-12-09 | 2009-04-23 | Hani Farah | Low Haze Thermoplastic Polyurethane Using Co-Chain Extenders |
| CN108047415A (en) * | 2018-01-10 | 2018-05-18 | 中国航发北京航空材料研究院 | A kind of optical grade thermoplastic polyurethane elastomer and preparation method thereof |
| CN113943538A (en) * | 2021-11-30 | 2022-01-18 | 江苏铁锚玻璃股份有限公司 | Formula and preparation method of low-melting-temperature transparent TPU film |
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- 2022-07-05 CN CN202210785402.1A patent/CN115057987B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20090104449A1 (en) * | 2005-12-09 | 2009-04-23 | Hani Farah | Low Haze Thermoplastic Polyurethane Using Co-Chain Extenders |
| CN108047415A (en) * | 2018-01-10 | 2018-05-18 | 中国航发北京航空材料研究院 | A kind of optical grade thermoplastic polyurethane elastomer and preparation method thereof |
| CN113943538A (en) * | 2021-11-30 | 2022-01-18 | 江苏铁锚玻璃股份有限公司 | Formula and preparation method of low-melting-temperature transparent TPU film |
Non-Patent Citations (2)
| Title |
|---|
| CHUANJUAN WEI等: "Dipentaerythritol-Derived Hyperbranched Polyurethane Elastomers and Their Applications in Flexible Strain Sensors" * |
| 李海柱 等: "柔性透明聚氨酯弹性体制备及性能" * |
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