CN115057987B - Formula of low-temperature-resistant transparent TPU film and preparation method thereof - Google Patents
Formula of low-temperature-resistant transparent TPU film and preparation method thereof Download PDFInfo
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- CN115057987B CN115057987B CN202210785402.1A CN202210785402A CN115057987B CN 115057987 B CN115057987 B CN 115057987B CN 202210785402 A CN202210785402 A CN 202210785402A CN 115057987 B CN115057987 B CN 115057987B
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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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- 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
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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% of polytetrahydrofuran ether glycol; 0% -15% of small molecule chain extender. The preparation method comprises the following steps: (a) weighing raw materials according to the formula; (b) vacuum dehydrating polytetrahydrofuran ether glycol; (c) Uniformly mixing aliphatic isocyanate and dehydrated polytetrahydrofuran ether glycol, and heating and stirring to obtain a first material; (d) heating the small molecule 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 castable; (f) Pouring the castable into a mold, curing at a high temperature, and removing the mold to obtain the low-temperature-resistant transparent TPU film, wherein the low-temperature-resistant transparent TPU film has better flexibility at a temperature of-20 ℃ and still has lower hardness at a temperature of-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 (Thermoplastic polyurethanes, 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, decomposability and the like, and can be widely applied to various fields.
In the process of realizing the application, the applicant finds that the hardness of the conventional 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 plasticizers, softeners and the like in the preparation process of the TPU film, but the effect of the TPU film prepared in the way is not obvious at the low temperature, so that a TPU film capable of maintaining certain physical properties (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, which solve the problem that the conventional TPU film has larger hardness at low temperature.
In order to solve the technical problems, the application is realized in the following way:
in a first aspect, a formulation for a low temperature resistant transparent TPU film is provided, comprising the following components in weight percent: 25% -35% of aliphatic isocyanate; 60% -70% of polytetrahydrofuran ether glycol; 0% -15% of small molecule 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 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, methylpropanediol, or diethylene glycol (diethylene glycol).
In a second aspect, a method for preparing a low temperature resistant transparent TPU film is provided, comprising the steps of: (a) Weighing raw materials according to the formula of the low-temperature-resistant transparent TPU film in any one of the first aspects; (b) Vacuum dehydrating polytetrahydrofuran ether glycol to make the mass fraction of water less than or equal to 0.05%; (c) Uniformly mixing aliphatic isocyanate and dehydrated polytetrahydrofuran ether glycol, and heating and stirring to obtain a first material; (d) heating the small molecule 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 castable; (f) Pouring the castable into a mold, curing at a high temperature, 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 the vacuum dehydration, the polytetrahydrofuran ether glycol is added into a three-neck flask equipped with a stirrer and a thermometer, and the polytetrahydrofuran ether glycol is heated, stirred and dehydrated.
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 100-110 ℃, and the vacuum dehydration time is 2-3h.
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 ℃ for 2-3h.
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), the step of curing at a high temperature is performed in a manner of heating at 120 ℃, keeping the temperature for 4 hours, heating at 160 ℃, keeping the temperature for 6 hours, heating at 80 ℃ and keeping the temperature for 12 hours.
Compared with the prior art, the application has the advantages that:
the formula of the low-temperature-resistant transparent TPU film and the preparation method thereof have the advantages that the prepared low-temperature-resistant transparent TPU film has better flexibility at the temperature of minus 20 ℃ and still has lower hardness at the temperature of minus 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 embodiments of the application and together with the description serve to explain the application and do not constitute an undue limitation to the application. In the drawings:
FIG. 1 is a flow chart of the steps of a method of making a low temperature resistant transparent TPU film according to one embodiment of the present application. .
Detailed Description
For the purpose of making the objects, technical solutions and advantages of the present application more apparent, the embodiments of the present application will be described in further detail below with reference to the accompanying drawings.
Example 1
The weight percentages of the components in the formula are respectively weighed: 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 preparing 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 the step S1, polytetrahydrofuran ether glycol is dehydrated in vacuum, so that the mass fraction of water is less than or equal to 0.05%. Specifically, the polytetrahydrofuran ether glycol 1000 is added into a three-neck flask with a stirrer and a thermometer, heated to 100-110 ℃, dehydrated for 2-3h under vacuum, the mass fraction of water in the polytetrahydrofuran ether glycol 1000 is not higher than 0.05%, and cooled to 100 ℃ for standby.
In the step S2, the aliphatic isocyanate and the dehydrated polytetrahydrofuran ether glycol are uniformly mixed, heated and stirred to obtain a first material. Specifically, the dehydrated polytetrahydrofuran ether glycol 1000 in the step S1 is added into metered diisocyanate, and is heated and stirred at 120 ℃ for 2-3 hours to react, and after the theoretical NCO content is reached, a first material is obtained for standby.
In step S3, the small molecule chain extender is heated to obtain a second material. Specifically, 1, 4-butanediol and ethylene glycol are mixed and heated at 120 ℃ to obtain a second material for standby.
In step S4, the first material and the second material are mixed and stirred until the mixture is clear, and the castable is obtained. Specifically, a second material and a 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 first material and the second material are clarified, so that castable is obtained.
In the step S5, pouring the castable into a mold, curing at a high temperature in stages, and removing the mold to obtain the low-temperature-resistant transparent TPU film. Specifically, pouring the castable into a flat plate-shaped mold, heating to 120 ℃, preserving heat for 4 hours, heating to 160 ℃, preserving heat for 6 hours, heating to 80 ℃ and preserving heat for 12 hours, cooling and demolding to obtain the low-temperature-resistant transparent TPU film.
The properties of the prepared low temperature resistant transparent TPU film were tested, and the test data are as follows:
1. the 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 film is stretched to the limit position without breaking;
2. the low-temperature-resistant transparent TPU film has the hardness of 68A and the tensile strength of 4MPa at the temperature of minus 20 ℃ and is stretched to the limit position without breaking;
3. the hardness of the low-temperature-resistant transparent TPU film is 92A at the temperature of minus 50 ℃.
Example 2
The weight percentages of the components in the formula are respectively weighed: 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 preparing 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 the step S1, polytetrahydrofuran ether glycol is dehydrated in vacuum, so that the mass fraction of water is less than or equal to 0.05%. Specifically, the polytetrahydrofuran ether glycol 1000 is added into a three-neck flask with a stirrer and a thermometer, heated to 100-110 ℃, dehydrated for 2-3h under vacuum, the mass fraction of water in the polytetrahydrofuran ether glycol 1000 is not higher than 0.05%, and cooled to 100 ℃ for standby.
In the step S2, the aliphatic isocyanate and the dehydrated polytetrahydrofuran ether glycol are uniformly mixed, heated and stirred to obtain a first material. Specifically, the dehydrated polytetrahydrofuran ether glycol 1000 in the step S1 is added into metered diisocyanate, and is heated and stirred at 120 ℃ for 2-3 hours to react, and after the theoretical NCO content is reached, a first material is obtained for standby.
In step S3, the small molecule chain extender is heated to obtain a second material. Specifically, 1, 5-pentanediol and ethylene glycol are mixed and heated at 120 ℃ to obtain a second material for standby.
In step S4, the first material and the second material are mixed and stirred until the mixture is clear, and the castable is obtained. Specifically, a second material and a 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 first material and the second material are clarified, so that castable is obtained.
In the step S5, pouring the castable into a mold, curing at a high temperature in stages, and removing the mold to obtain the low-temperature-resistant transparent TPU film. Specifically, pouring the castable into a flat plate-shaped mold, heating to 120 ℃, preserving heat for 4 hours, heating to 160 ℃, preserving heat for 6 hours, heating to 80 ℃ and preserving heat for 12 hours, cooling and demolding to obtain the low-temperature-resistant transparent TPU film.
The properties of the prepared low temperature resistant transparent TPU film were tested, and the test data are as follows:
1. the transmittance of the low-temperature-resistant transparent TPU film is 91%, the hardness is 57A, the tensile strength is 5Mpa, and the film is stretched to the limit position without breaking;
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 minus 50 ℃.
As can be seen from the test results of the above examples 1 and 2, the low temperature resistant transparent TPU film prepared according to the formula and the preparation method of the low temperature resistant transparent TPU film has good physical properties at normal temperature, good flexibility at-20 ℃ and 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 application has better flexibility at the temperature of minus 20 ℃ and still has lower hardness at the temperature of minus 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 one … …" does not exclude the presence of other like elements in a process, method, article, or apparatus that comprises the element.
The embodiments of the present application have been described above with reference to the accompanying drawings, but the present application is not limited to the above-described embodiments, which are merely illustrative and not restrictive, and many forms may be made by those of ordinary skill in the art without departing from the spirit of the present application and the scope of the claims, which are also within the protection of the present application.
Claims (3)
1. The preparation method of the low-temperature-resistant transparent TPU film is characterized by comprising the following steps of:
(a) Weighing raw materials according to a formula of the low-temperature-resistant transparent TPU film, wherein the formula comprises 31% of aliphatic isocyanate, 65% of polytetrahydrofuran ether glycol and 4% of small molecular chain extender, wherein the aliphatic isocyanate is diisocyanate, the polytetrahydrofuran ether glycol is polytetrahydrofuran ether glycol 1000,4% of the small molecular chain extender is 2% of 1, 4-butanediol and 2% of ethylene glycol or 2% of 1, 5-pentanediol and 2% of ethylene glycol;
(b) Vacuum dehydrating the polytetrahydrofuran ether glycol to ensure that the mass fraction of water is less than or equal to 0.05%;
(c) Uniformly mixing the aliphatic isocyanate and the dehydrated polytetrahydrofuran ether glycol, and heating and stirring to obtain a first material, wherein the heating and stirring temperature of the aliphatic isocyanate and the polytetrahydrofuran ether glycol is 120 ℃ and the time is 2-3h;
(d) Heating the small molecular chain extender to obtain a second material, wherein the heating temperature of the small molecular chain extender is 120 ℃;
(e) Mixing the first material with the second material, and stirring until the mixture is clear to obtain castable;
(f) And pouring the castable into a mold, curing at a stage of high temperature, and removing the mold to obtain the low temperature-resistant transparent TPU film, wherein the low temperature-resistant transparent TPU film is cured at a stage of high temperature according to the modes of heating to 120 ℃, preserving heat for 4 hours, heating to 160 ℃, preserving heat for 6 hours, heating to 80 ℃ and preserving heat for 12 hours.
2. The method for producing a low temperature resistant transparent TPU film according to claim 1, wherein in said step (b), said polytetrahydrofuran ether glycol is added to a three-necked flask equipped with a stirrer and a thermometer during vacuum dehydration, and said polytetrahydrofuran ether glycol is heated and dehydrated with stirring.
3. The method for preparing the low temperature resistant transparent TPU film according to claim 2, wherein the heating temperature of the polytetrahydrofuran ether glycol is 100-110 ℃, and the vacuum dehydration time is 2-3h.
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| 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 |
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