Anti-aging PET (Polyethylene Terephthalate) film and preparation method of anti-aging process of PET film

Abstract

The invention relates to an anti-aging PET (polyethylene terephthalate) film and a preparation method of an anti-aging process of the PET film, the anti-aging PET film comprises a PET layer, an anti-aging layer and an adhesive layer, the anti-aging layer is arranged on the PET layer through the adhesive layer, the anti-aging layer takes trifluoropropyl trimethyl cyclotrisiloxane, octamethylcyclotetrasiloxane and tetramethyldihydrodisiloxane as raw materials, and the anti-aging layer and the adhesive layer are arranged on the PET layer through the adhesive layer. And carrying out ring-opening polycondensation, hydrosilylation and hydrolysis copolycondensation reaction to obtain the product. The adhesive layer is prepared by taking polyterephthalic acid-3-methyl-1, 5-pentanediol ester glycol and polyethylene glycol as soft segments and taking isophorone diisocyanate, diethylene glycol and 2, 2-dimethylolpropionic acid as hard segments. According to the prepared adhesive layer, the mechanical property and the water resistance of the PET film are greatly improved, the thermal stability is improved, meanwhile, the PET layer and the anti-aging layer are fixed through the adhesive layer, the PET layer and the anti-aging layer can be well bonded, and the bonding strength is good; in addition, the prepared anti-aging layer is low in aging stripping force.

Description

Technical Field

[0001] The invention relates to the technical field of PET films, and in particular to an electric actuator. Background Art

[0002] PET film is widely used in packaging, electronics, optics and other fields due to its excellent mechanical properties, optical properties and chemical stability. However, during long-term use, PET film is affected by environmental factors such as light, temperature and humidity, and is prone to aging, such as yellowing, brittleness, and decreased mechanical properties, which seriously limits its service life and application range. The PET film currently on the market has limited aging resistance and is difficult to meet application scenarios with high requirements for material durability. Therefore, it is of great practical significance to develop a PET film with good aging resistance and a preparation method thereof. Summary of the invention

[0003] The object of the present invention is to provide an anti-aging PET film and a method for preparing the anti-aging process of the PET film.

[0004] To achieve the above object, the present invention provides the following technical solutions:

[0005] A kind of aging-resistant PET film, characterized in that it comprises a PET layer, an aging-resistant layer and an adhesive layer, wherein the aging-resistant layer is arranged on the PET layer through the adhesive layer, wherein the aging-resistant layer is made of trifluoropropyltrimethylcyclotrisiloxane, octamethylcyclotetrasiloxane and tetramethyldihydrodisiloxane as raw materials, and is prepared through ring-opening polycondensation, hydrosilylation and co-condensation reaction; the adhesive layer is made of poly(3-methyl-1,5-pentanediol terephthalate) diol and polyethylene glycol as soft segments, and isophorone diisocyanate, diethylene glycol and 2,2-dihydroxymethylpropionic acid as hard segments.

[0006] The present invention also provides a method for preparing an anti-aging process of a PET film, which is characterized by comprising the following steps:

[0007] S100, prepare an adhesive layer, place polyethylene glycol and poly(3-methyl-1,5-pentanediol terephthalate) in a mass ratio of 1-4:1-3 in a stirring device for stirring, and control the heating temperature, then perform vacuum dehydration, cool down to half of the heating temperature after dehydration, then add isophorone diisocyanate and 2,2-dihydroxymethyl propionic acid, raise its temperature to 80-85 degrees Celsius, control the reaction time to 2-3 hours, cool down to half of the heating temperature, add diethylene glycol to react for at least 1 hour, control the temperature to 60-70 degrees Celsius, cool down to half of the heating temperature again, add a catalyst, heat up to 60 degrees Celsius again, the reaction time is 3-4 hours, and hydroxypropyl methylcellulose is used to adjust the viscosity during the reaction. Cool down after the reaction, pour the prepolymer in the flask into an emulsification barrel, add a quantitative triethylamine, and neutralize and stir. Then, a proper amount of water is slowly added under high-speed shearing of the mixer to emulsify and obtain an adhesive layer;

[0008] S200, prepare the aging-resistant layer, add trifluoropropyl trimethyl cyclotrisiloxane and octamethyl cyclotetrasiloxane in a molar ratio of 1-3:1-5 to a stirring device for uniform stirring, react until the temperature inside the device reaches 40-50 degrees Celsius, add a certain amount of catalyst, react at a constant temperature for 1-1.5 hours, and add the end-capping agent D2 H After a certain reaction time, anhydrous sodium carbonate is used for neutralization, filtering, and vacuum distillation is used to remove low-boiling substances to obtain a colorless, transparent, low-viscosity oily liquid as the first product, which is fluorine-containing and hydrogen-containing silicone oil;

[0009] The first product and vinyl triethoxysilane (VTES) are added to a stirring device in a substance ratio of 1:1 and mixed evenly. After the system is heated to 90°C and stirred for a certain period of time, a chloroplatinic acid catalyst is added, and the reaction is continued at a constant temperature for 4 hours to obtain a second product, which is an alkoxy-modified fluorinated polysiloxane intermediate; the synthesized oxy-modified fluorinated polysiloxane intermediate, tetraethyl orthosilicate (TEOS) and octyl triethoxysilane (OTES) are added to anhydrous ethanol in a substance ratio of 4:2:1 and mixed evenly. When the internal temperature is heated to 60°C, hydrochloric acid is added to adjust the pH to 3-4. After reacting for 30 minutes, co-hydrolysis and polycondensation are performed for 5-6 hours to obtain an organic-inorganic hybrid modified fluorosilicone resin;

[0010] S300. During the stretching and extrusion process of preparing the PET film, the PET layer is coated with an adhesive layer and then an anti-aging layer through an online coating process, and then stretched, and placed in an oven to form an anti-aging layer on the surface of the PET layer after the solvent of the anti-aging layer is dried and volatilized.

[0011] The present invention further provides that the mass ratio of the polyethylene glycol to the poly(3-methyl-1,5-pentanediol terephthalate) is 1:1.

[0012] The present invention further provides that the molar ratio of the fluoropropyltrimethylcyclotrisiloxane to the octamethylcyclotetrasiloxane is 2:3.

[0013] The present invention further provides that the heating temperature is at least 100 degrees Celsius.

[0014] Beneficial effects of the present invention:

[0015] The adhesive layer prepared in the present invention greatly increases the mechanical properties and water resistance of the PET film, improves the thermal stability, and at the same time, the PET layer and the aging-resistant layer are fixed by the adhesive layer, which can well bond the PET layer and the aging-resistant layer to have good bonding strength; in addition, the prepared aging-resistant layer has low aging peeling force. DETAILED DESCRIPTION

[0016] The following will explain the implementation methods of the present application in detail with reference to examples, so that the implementation process of how the present application uses technical means to solve technical problems and achieve technical effects can be fully understood and implemented accordingly.

[0017] Embodiment 1:

[0018] The present embodiment provides an aging-resistant PET film, comprising a PET layer, an aging-resistant layer and an adhesive layer, wherein the aging-resistant layer is arranged on the PET layer through the adhesive layer, wherein the aging-resistant layer is made of trifluoropropyltrimethylcyclotrisiloxane, octamethylcyclotetrasiloxane, and tetramethyldihydrodisiloxane as raw materials, and is prepared through ring-opening polycondensation, hydrosilylation, and hydrolysis co-condensation reactions; the adhesive layer is made of poly(3-methyl-1,5-pentanediol terephthalate) diol and polyethylene glycol as soft segments, and isophorone diisocyanate, diethylene glycol, and 2,2-dihydroxymethylpropionic acid as hard segments.

[0019] The present invention also provides a method for preparing an anti-aging process of a PET film, which is characterized by comprising the following steps:

[0020] S100, prepare an adhesive layer, place polyethylene glycol and poly(3-methyl-1,5-pentanediol terephthalate) in a mass ratio of 1-4:1-3 in a stirring device for stirring, and control the heating temperature, then perform vacuum dehydration, cool down to half of the heating temperature after dehydration, then add isophorone diisocyanate and 2,2-dihydroxymethyl propionic acid, raise its temperature to 80-85 degrees Celsius, control the reaction time to 2-3 hours, cool down to half of the heating temperature, add diethylene glycol to react for at least 1 hour, control the temperature to 60-70 degrees Celsius, cool down to half of the heating temperature again, add a catalyst, heat up to 60 degrees Celsius again, the reaction time is 3-4 hours, and hydroxypropyl methylcellulose is used to adjust the viscosity during the reaction. Cool down after the reaction, pour the prepolymer in the flask into an emulsification barrel, add a quantitative triethylamine, and neutralize and stir. Then, a proper amount of water is slowly added under high-speed shearing of the mixer to emulsify and obtain an adhesive layer;

[0021] S200, prepare the aging-resistant layer, add trifluoropropyl trimethyl cyclotrisiloxane and octamethyl cyclotetrasiloxane in a molar ratio of 1-3:1-5 to a stirring device for uniform stirring, react until the temperature inside the device reaches 40-50 degrees Celsius, add a certain amount of catalyst, react at a constant temperature for 1-1.5 hours, and add the end-capping agent D2 H After a certain reaction time, anhydrous sodium carbonate is used for neutralization, filtering, and vacuum distillation is used to remove low-boiling substances to obtain a colorless, transparent, low-viscosity oily liquid as the first product, which is fluorine-containing and hydrogen-containing silicone oil;

[0022] The first product and vinyl triethoxysilane (VTES) are added to a stirring device in a substance ratio of 1:1 and mixed evenly. After the system is heated to 90°C and stirred for a certain period of time, a chloroplatinic acid catalyst is added, and the reaction is continued at a constant temperature for 4 hours to obtain a second product, which is an alkoxy-modified fluorinated polysiloxane intermediate; the synthesized oxy-modified fluorinated polysiloxane intermediate, tetraethyl orthosilicate (TEOS) and octyl triethoxysilane (OTES) are added to anhydrous ethanol in a substance ratio of 4:2:1 and mixed evenly. When the internal temperature is heated to 60°C, hydrochloric acid is added to adjust the pH to 3-4. After reacting for 30 minutes, co-hydrolysis and polycondensation are performed for 5-6 hours to obtain an organic-inorganic hybrid modified fluorosilicone resin;

[0023] S300. During the stretching and extrusion process of preparing the PET film, the PET layer is coated with an adhesive layer and then an anti-aging layer through an online coating process, and then stretched, and placed in an oven to form an anti-aging layer on the surface of the PET layer after the solvent of the anti-aging layer is dried and volatilized.

[0024] The present invention further provides that the mass ratio of the polyethylene glycol to the poly(3-methyl-1,5-pentanediol terephthalate) is 1:1.

[0025] The present invention further provides that the molar ratio of the fluoropropyltrimethylcyclotrisiloxane to the octamethylcyclotetrasiloxane is 2:3.

[0026] The present invention further provides that the heating temperature is at least 100 degrees Celsius.

[0027] The adhesive layer prepared in the present invention greatly increases the mechanical properties and water resistance of the PET film, improves the thermal stability, and at the same time, the PET layer and the aging-resistant layer are fixed by the adhesive layer, which can well bond the PET layer and the aging-resistant layer to have good bonding strength; in addition, the prepared aging-resistant layer has low aging peeling force.

[0028] The peel strength test was performed after combining the aging-resistant layer, adhesive layer and PET layer:

[0029] The test method is as follows: 0.5% (accounting for the mass of the adhesive layer) of the thickener is added dropwise to the prepared adhesive layer and stirred evenly with a glass rod. A certain amount of the adhesive layer is evenly applied to a PET film strip (10mm×200mm), and the same mass of the aging-resistant layer is applied to the adhesive layer. Dry at room temperature. After drying, hot press at 80°C. The peel strength is tested using a SANS microcomputer-controlled electronic universal testing machine with a tensile speed of 200mm / min, measured 3 times, and the average value is taken. When preparing the adhesive layer, the mass ratio of the polyethylene glycol and the poly(3-methyl-1,5-pentanediol terephthalate) is 1:1.

[0030] The comparative example is: using epoxy adhesive layer to bond the aging-resistant layer and the adhesive layer;

[0031] The data are shown in Table 1:

[0032] Bonding strength Comparative Example 1.28N / 25mm Experimental example 4.55N / 25mm

[0033] The thermal stability test of the comparative example and experimental example is as follows: under N2 protection, the test is performed using a thermogravimetric analyzer (TGA), the test range is 25-800°C, and the heating rate is 10°C / min. The following data are obtained: Comparative example:

[0034]

[0035] According to the above data, the experimental example has good thermal stability and is not prone to aging when exposed to high temperatures.

[0036] For example, certain words are used in the specification and claims to refer to specific components. Those skilled in the art should understand that hardware manufacturers may use different terms to refer to the same component. This specification and claims do not use differences in names as a way to distinguish components, but use differences in the functions of components as the criteria for distinction. For example, "including" mentioned throughout the specification and claims is an open term, so it should be interpreted as "including but not limited to". "Approximately" means that within an acceptable error range, those skilled in the art can solve technical problems within a certain error range and basically achieve technical effects.

[0037] It should be noted that the terms "include", "comprises" or any other variations thereof are intended to cover non-exclusive inclusion, so that a product or system including a series of elements includes not only those elements, but also other elements not explicitly listed, or also includes elements inherent to such product or system. In the absence of more restrictions, the elements defined by the sentence "comprises a ..." do not exclude the existence of other identical elements in the product or system including the elements.

[0038] The above description shows and describes several preferred embodiments of the present invention, but as before, it should be understood that the present invention is not limited to the form disclosed herein, and should not be regarded as excluding other embodiments, but can be used in various other combinations, modifications and environments, and can be modified within the scope of the invention concept of this article through the above teachings or the technology or knowledge of the relevant field. And the changes and modifications made by those skilled in the art do not depart from the spirit and scope of the present invention, and should be within the scope of protection of the claims attached to the present invention.

Claims

1. An aging-resistant PET film, characterized in that: The invention comprises a PET layer, an aging-resistant layer and an adhesive layer, wherein the aging-resistant layer is arranged on the PET layer through the adhesive layer, wherein the aging-resistant layer is made of trifluoropropyltrimethylcyclotrisiloxane, octamethylcyclotetrasiloxane and tetramethyldihydrodisiloxane as raw materials, and is prepared through ring-opening polycondensation, hydrosilylation and co-condensation reaction; the adhesive layer is made of poly(3-methyl-1,5-pentanediol terephthalate) glycol and polyethylene glycol as soft segments, and isophorone diisocyanate, diethylene glycol and 2,2-dihydroxymethylpropionic acid as hard segments.

2. A method for preparing an anti-aging process for a PET film, characterized in that: The steps include: S100, preparing an adhesive layer, placing polyethylene glycol and poly(3-methyl-1,5-pentanediol terephthalate) in a mass ratio of 1-4:1-3 in a stirring device for stirring, and controlling the heating temperature, then performing vacuum dehydration, cooling to half of the heating temperature after dehydration, and then adding isophorone diisocyanate and 2,2-dihydroxymethylpropionic acid, raising the temperature to 80-85 degrees Celsius, controlling the reaction time to 2-3 hours, cooling to half of the heating temperature, adding diethylene glycol to react for at least 1 hour, and controlling the temperature to 60-70 degrees Celsius, cooling again to half of the heating temperature, adding a catalyst, and heating again to 60 degrees Celsius, and the reaction time is 3-4 hours. During the reaction, hydroxypropyl methylcellulose is used to adjust the viscosity. After the reaction is finished, cool down, pour the prepolymer in the flask into the emulsification barrel, add a certain amount of triethylamine, neutralize and stir. Then slowly add an appropriate amount of water under high-speed shearing of the mixer, emulsify, and obtain an adhesive layer; S200, prepare the aging-resistant layer, add trifluoropropyl trimethyl cyclotrisiloxane and octamethyl cyclotetrasiloxane in a molar ratio of 1-3:1-5 to a stirring device for uniform stirring, react until the temperature inside the device reaches 40-50 degrees Celsius, add a certain amount of catalyst, react at a constant temperature for 1-1.5 hours, and add the end-capping agent D2 H After a certain reaction time, anhydrous sodium carbonate is used for neutralization, filtering, and vacuum distillation is used to remove low-boiling substances to obtain a colorless, transparent, low-viscosity oily liquid as the first product, which is fluorine-containing and hydrogen-containing silicone oil; The first product and vinyl triethoxysilane (VTES) are added to a stirring device in a substance ratio of 1:1 and mixed evenly. After the system is heated to 90°C and stirred for a certain period of time, a chloroplatinic acid catalyst is added, and the reaction is continued at a constant temperature for 4 hours to obtain a second product, which is an alkoxy-modified fluorinated polysiloxane intermediate; the synthesized oxy-modified fluorinated polysiloxane intermediate, tetraethyl orthosilicate (TEOS) and octyl triethoxysilane (OTES) are added to anhydrous ethanol in a substance ratio of 4:2:1 and mixed evenly. When the internal temperature is heated to 60°C, hydrochloric acid is added to adjust the pH to 3-4. After reacting for 30 minutes, co-hydrolysis and polycondensation are performed for 5-6 hours to obtain an organic-inorganic hybrid modified fluorosilicone resin; S300. During the stretching and extrusion process of preparing the PET film, the PET layer is coated with an adhesive layer and then an anti-aging layer through an online coating process, and then stretched, and placed in an oven to form an anti-aging layer on the surface of the PET layer after the solvent of the anti-aging layer is dried and volatilized.

3. The method for preparing an anti-aging process of a PET film according to claim 2, characterized in that: The mass ratio of the polyethylene glycol to the poly(3-methyl-1,5-pentanediol terephthalate) is 1:

1.

4. The method for preparing an anti-aging process of a PET film according to claim 2, characterized in that: The molar ratio of the fluoropropyltrimethylcyclotrisiloxane to octamethylcyclotetrasiloxane is 2:

3.

5. The method for preparing an anti-aging process of a PET film according to claim 2, characterized in that: The heating temperature is at least 100 degrees Celsius.

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