Antistatic polyester release film and preparation method thereof

Abstract

The invention relates to a preparation method of an antistatic polyester release film, which is characterized by comprising the following steps: adding a proper amount of AZO powder into 250mL of polyethylene glycol to prepare a polyethylene glycol solution of AZO; the preparation method comprises the following steps: preheating a reaction kettle, adding a polyethylene glycol solution of AZO, then adding terephthalic acid for multiple times, adjusting the stirring rotating speed to be 50Hz, and stirring for 5-10 minutes; inert gas is slowly filled into the reaction kettle to 150 kPa, the pressure is relieved after 10 seconds, the process is repeated twice, inert gas is filled again to 100 kPa for pressure maintaining, and the temperature of a jacket of the reaction kettle is set to 260 DEG C. Maintaining the pressure of the reaction kettle at 360-400 kPa, ending the esterification stage when the esterification water reaches 80% of a theoretical value and the pressure is reduced to 300 kPa or below, and slowly releasing the pressure; the PET / AZO composite material is prepared. AZO is used as the conductive filler, so that the antistatic property of PET can be effectively improved.

Description

Technical Field

[0001] The invention relates to the technical field of antistatic release films, and in particular to an antistatic polyester release film and a preparation method thereof. Background Art

[0002] During the transportation or use of products such as glass, high-grade plates, and electronic products, the surface is easily contaminated or scratched by contact, so a protective film is used to cover the surface to avoid contamination or damage. Generally, plastic film is used, but the dielectric constant of plastic film is small, it is a non-conductor, and the insulation performance is high, so static electricity will be generated. However, static charge accumulates on the surface of plastic film, which is easy to cause dust adsorption on the surface, and even cause discharge, causing fire. Therefore, in order to avoid static electricity accumulation on the surface of plastic film, plastic film is usually treated with antistatic to enhance its conductive properties. Conventional antistatic treatment is to coat plastic film with antistatic agent, but with current technology, the antistatic performance of treated plastic film is not stable enough and the retention time is short. Especially when the ambient humidity decreases, the antistatic performance of plastic film will deteriorate, that is, the conductivity will decrease or even fail. Summary of the invention

[0003] The purpose of the present invention is to provide a method for preparing an antistatic polyester release film to solve the above technical problems.

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

[0005] A method for preparing an antistatic polyester release film, characterized in that it comprises the following steps:

[0006] Add an appropriate amount of AZO powder into 250 mL of polyethylene glycol, stir, and then put it into an ultrasonic crusher for ultrasonic crushing to prepare an AZO polyethylene glycol solution;

[0007] After preheating the reactor, add the polyethylene glycol solution of AZO, then add terephthalic acid several times, adjust the stirring speed to 50 Hz, and stir for 5 to 10 minutes;

[0008] The reactor was slowly filled with inert gas to 150 kPa, and the pressure was released after 10 seconds. This was repeated twice, and the inert gas was filled again to 100 kPa to maintain the pressure. The jacket temperature of the reactor was set to 260°C.

[0009] Maintain the reactor pressure at 360-400 kPa. When the esterified water reaches 80% of the theoretical value and the pressure drops below 300 kPa, the esterification stage ends and the pressure is slowly released.

[0010] After the pressure in the autoclave is determined to be 0, the esterification channel is closed, the polycondensation channel is opened, and the polyethylene glycol solution of AZO, triphenyl phosphite and antimony trioxide are added multiple times;

[0011] After reacting for 5 to 10 minutes, adjust the micro-vacuum valve to -100 kPa and set the reactor jacket temperature to 270 °C;

[0012] The casting head temperature was set at 260°C, and the speed was adjusted to 25 Hz when the reactor power reached 90 W. When the power dropped to 80 W, the agitator and vacuum pump were turned off, and the material was discharged after the inert gas was filled and the pressure was reduced to 0 to obtain a PET / AZO composite material.

[0013] The present invention further provides that the contents of terephthalic acid, polyethylene glycol, antimony trioxide and triphenyl phosphite are added in the amount of substance, and the ratio thereof is 1:1.4:0.001:0.001.

[0014] The present invention further provides that the preparation method of AZO powder is as follows: dissolve ZnCl2 and Al(NO3)3·9H2O in deionized water, add PEG-2000, and stir for 0.5h. Prepare a mixed alkaline solution as a precipitant according to n(NaOH):n(Na2CO3)=2:1, add the precipitant and the salt solution dropwise into distilled water under magnetic stirring, ensure that pH=8 during the reaction, and react at 60°C for 2.5h to obtain a white hydrothermal product; after the reaction is complete, the hydrothermal product is allowed to stand for aging for 2h, filtered by a water circulation filter, washed with deionized water and then with anhydrous ethanol, and dried at 100°C to obtain a white AZO precursor powder; the AZO precursor powder is placed in a tubular furnace, kept warm at 300°C for 2h, and kept warm at 800°C for 2h to obtain an AZO nano powder.

[0015] The present invention further provides that the mass of PEG-2000 is 1.5% of ZnCl2.

[0016] The present invention further provides that the number of times of washing with deionized water is 5-10 times.

[0017] The present invention further provides that the number of washing times with anhydrous ethanol is 1 time or 2 times.

[0018] The beneficial effects of the present invention are as follows: in the process of preparing PET / AZO nanocomposite materials, when the filling amount is less than 0.005%, the surface resistivity decreases with the increase of the filler content, and when the filling amount exceeds 0.005%, the surface resistivity increases. When the filling amount is 0.005%, the surface resistivity of the composite material is the lowest, reaching 1.16×1010Ω / sq, and the material is transformed from an insulator to an electrostatic dissipator. Using AZO as a conductive filler can effectively improve the antistatic property of PET. DETAILED DESCRIPTION

[0019] 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.

[0020] The present invention provides a method for preparing an antistatic polyester release film, comprising the following steps:

[0021] Add an appropriate amount of AZO powder into 250 mL of polyethylene glycol, stir, and then put it into an ultrasonic crusher for ultrasonic crushing to prepare an AZO polyethylene glycol solution;

[0022] After preheating the reactor, add the polyethylene glycol solution of AZO, then add terephthalic acid several times, adjust the stirring speed to 50 Hz, and stir for 5 to 10 minutes;

[0023] The reactor was slowly filled with inert gas to 150 kPa, and the pressure was released after 10 seconds. This was repeated twice, and the inert gas was filled again to 100 kPa to maintain the pressure. The jacket temperature of the reactor was set to 260°C.

[0024] Maintain the reactor pressure at 360-400 kPa. When the esterified water reaches 80% of the theoretical value and the pressure drops below 300 kPa, the esterification stage ends and the pressure is slowly released.

[0025] After the pressure in the autoclave is determined to be 0, the esterification channel is closed, the polycondensation channel is opened, and the polyethylene glycol solution of AZO, triphenyl phosphite and antimony trioxide are added multiple times;

[0026] After reacting for 5 to 10 minutes, adjust the micro-vacuum valve to -100 kPa and set the reactor jacket temperature to 270 °C;

[0027] The casting head temperature was set at 260°C, and the speed was adjusted to 25 Hz when the reactor power reached 90 W. When the power dropped to 80 W, the agitator and vacuum pump were turned off, and the material was discharged after the inert gas was filled and the pressure was reduced to 0 to obtain a PET / AZO composite material.

[0028] The present invention further provides that the contents of terephthalic acid, polyethylene glycol, antimony trioxide and triphenyl phosphite are added in the amount of substance, and the ratio thereof is 1:1.4:0.001:0.001.

[0029] The present invention further provides that the preparation method of AZO powder is as follows: dissolve ZnCl2 and Al(NO3)3·9H2O in deionized water, add PEG-2000, and stir for 0.5h. Prepare a mixed alkaline solution as a precipitant according to n(NaOH):n(Na2CO3)=2:1, add the precipitant and the salt solution dropwise into distilled water under magnetic stirring, ensure that pH=8 during the reaction, and react at 60°C for 2.5h to obtain a white hydrothermal product; after the reaction is complete, the hydrothermal product is allowed to stand for aging for 2h, filtered by a water circulation filter, washed with deionized water and then with anhydrous ethanol, and dried at 100°C to obtain a white AZO precursor powder; the AZO precursor powder is placed in a tubular furnace, kept warm at 300°C for 2h, and kept warm at 800°C for 2h to obtain an AZO nano powder.

[0030] The present invention further provides that the mass of PEG-2000 is 1.5% of ZnCl2.

[0031] The present invention further provides that the number of times of washing with deionized water is 5-10 times.

[0032] The present invention further provides that the number of washing times with anhydrous ethanol is 1 time or 2 times.

[0033] The antistatic properties of PET / AZO nanocomposites were tested using the following method:

[0034] AZO powder with 2% Al doping was selected as the conductive filler to study the effect of AZO filler content on the surface resistivity of PET. The results are shown in the following table. The AZO powder filling amounts of samples 1#, 2#, 3#, 4#, 5#, and 6# are 0.001%, 0.002%, 0.003%, 0.005%, 0.01%, and 0.05%, respectively.

[0035]

[0036] The surface resistivity measurement results show that when the filling amount is less than 0.005%, the surface resistivity decreases with the increase of filler content. When the filling amount exceeds 0.005%, the surface resistivity increases. When the filling amount is 0.005%, the surface resistivity of the composite material is the lowest, reaching 1.16×10 10 Ω / m 2. The surface resistivity of the composite material decreases sharply within the AZO content range of 0 to 0.005%, indicating that a connected structure has been formed when the AZO content is below 0.005%. The electro-percolation threshold of the PET / AZO composite material appears below 0.005%, and the material is transformed from an insulator to an electrostatic dissipator. When the addition amount exceeds 0.005%, a certain increase in the surface resistivity of the material is observed. Therefore, in the process of preparing PET / AZO nanocomposites, when the filling amount is less than 0.005%, the surface resistivity decreases with the increase of the filler content. When the filling amount exceeds 0.005%, the surface resistivity increases. When the filling amount is 0.005%, the surface resistivity of the composite material is the lowest, reaching 1.16×1010Ω / sq, and the material is transformed from an insulator to an electrostatic dissipator. Using AZO as a conductive filler can effectively improve the antistatic properties of PET.

[0037] 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.

[0038] 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.

[0039] 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. A method for preparing an antistatic polyester release film, characterized in that: The steps include: Add an appropriate amount of AZO powder into 250 mL of polyethylene glycol, stir, and then put it into an ultrasonic crusher for ultrasonic crushing to prepare an AZO polyethylene glycol solution; After preheating the reactor, add the polyethylene glycol solution of AZO, then add terephthalic acid several times, adjust the stirring speed to 50 Hz, and stir for 5 to 10 minutes; Slowly fill the reactor with inert gas to 150 kPa, release the pressure after 10 seconds, repeat twice, fill the reactor with inert gas again to 100 kPa and maintain the pressure. Set the reactor jacket temperature to 260 °C; Maintain the reactor pressure at 360-400 kPa. When the esterified water reaches 80% of the theoretical value and the pressure drops below 300 kPa, the esterification stage ends and the pressure is slowly released. After the pressure in the autoclave is determined to be 0, the esterification channel is closed, the polycondensation channel is opened, and the polyethylene glycol solution of AZO, triphenyl phosphite and antimony trioxide are added multiple times; After reacting for 5 to 10 minutes, adjust the micro-vacuum valve to -100 kPa and set the jacket temperature of the reactor to 270 °C; The casting head temperature was set at 260°C, and the speed was adjusted to 25 Hz when the reactor power reached 90 W. When the power dropped to 80 W, the agitator and vacuum pump were turned off, and the material was discharged after the inert gas was filled and the pressure was reduced to 0 to obtain a PET / AZO composite material.

2. The method for preparing an antistatic polyester release film according to claim 2, characterized in that: The contents of terephthalic acid, polyethylene glycol, antimony trioxide and triphenyl phosphite are added in the amount of substance, and the ratio thereof is 1:1.4:0.001:0.

001.

3. The method for preparing an antistatic polyester release film according to claim 2, characterized in that: The preparation method of AZO powder is as follows: dissolve ZnCl2 and Al(NO3)3·9H2O in deionized water, add PEG-2000, and stir for 0.5h. Prepare a mixed alkaline solution as a precipitant according to n(NaOH):n(Na2CO3)=2:1, add the precipitant and the salt solution dropwise into distilled water under magnetic stirring, ensure that pH=8 during the reaction, and react at 60℃ for 2.5h to obtain a white hydrothermal product; after the reaction is complete, the hydrothermal product is allowed to stand for 2h, filtered by a water circulation filter, washed with deionized water and then with anhydrous ethanol, and dried at 100℃ to obtain a white AZO precursor powder; the AZO precursor powder is placed in a tubular furnace, kept at 300℃ for 2h, and kept at 800℃ for 2h to obtain AZO nanopowder.

4. The method for preparing an antistatic polyester release film according to claim 3, characterized in that: The mass of PEG-2000 is 1.5% of ZnCl2.

5. The method for preparing an antistatic polyester release film according to claim 3, characterized in that: The number of washing times with deionized water is 5-10 times.

6. The method for preparing an antistatic polyester release film according to claim 3, characterized in that: The number of washings with anhydrous ethanol was 1 or 2 times.

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