CN117841397A - Preparation method of PET-TPU composite film - Google Patents
Preparation method of PET-TPU composite film Download PDFInfo
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- 238000010438 heat treatment Methods 0.000 claims description 16
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- 229920000570 polyether Polymers 0.000 claims description 6
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 5
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- 239000010408 film Substances 0.000 abstract description 229
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Abstract
The application relates to the technical field of electron optical films, in particular to a preparation method of a PET-TPU composite film. A preparation method of a PET-TPU composite film comprises the steps of carrying out electrostatic dust removal pretreatment on a PET base film, drying, carrying out hot-pressing compounding on a TPU casting film and the PET base film, and carrying out stretching treatment, shaping and plasma treatment to obtain the PET-TPU composite film. The PET-TPU composite film prepared by the method has high hardness, light transmittance, anti-fog performance and excellent TPU ink printability. Meanwhile, the preparation method is simple and feasible, low in cost and suitable for large-scale production.
Description
Technical Field
The application relates to the technical field of electron optical films, in particular to a preparation method of a PET-TPU composite film.
Background
Polyethylene terephthalate (PET) has excellent optical properties such as good transparency, low haze and high glossiness in addition to excellent physical and mechanical properties of a general polyester film, and is generally used as a base material for high-end electron optical functional films such as a hard coat film, a diffusion film, a brightness enhancing film, an antireflection film and the like.
The TPU film is a high molecular elastic material, and is a novel environment-friendly material. Its special molecular structure gives it excellent physical properties such as: high elasticity, wear resistance, high strength, hardness, ductility, water resistance, air permeability, oil resistance and mold resistance. Because of its excellent performance and environmental protection concepts, there is an increasing interest in it, and its application breadth and depth are also expanding.
The existing PET-TPU composite film has the problem of poor printing performance due to higher optical property requirement, so that a new PET-TPU composite film with excellent printing performance needs to be developed.
Disclosure of Invention
The application aims at overcoming the defects of the prior art and providing a preparation method of a PET-TPU composite film.
The application provides a preparation method of a PET-TPU composite film, which adopts the following technical scheme:
the preparation method of the PET-TPU composite film comprises the following steps:
s1, carrying out electrostatic dust removal pretreatment on the PET base film, and drying to obtain the PET base film with a clean surface.
S2, casting the TPU casting film onto a PET base film with a clean surface, and then carrying out hot-pressing compounding on the TPU casting film and the PET base film to form a composite base film; the raw materials for preparing the TPU casting film are polyether type TPU particles with the average molecular weight of 33000-36000;
s3, heating the composite base film obtained in the step S2, performing stretching treatment, wherein the longitudinal stretching multiplying power is 5-10 times, the transverse stretching multiplying power is 5-10 times, heating and shaping, cooling to obtain a composite film with the film thickness of 0.01-0.04mm, and performing plasma treatment on the TPU film surface of the composite film to obtain the PET-TPU composite film.
By adopting the technical scheme, in the preparation method of the application, each step plays an indispensable role, and the steps are mutually cooperated, so that the PET-TPU composite film with excellent performance is finally prepared. In the step S1, dust and impurities on the surface of the PET base film are removed through electrostatic dust removal pretreatment and drying, so that the surface of the base film is ensured to be clean, and a good foundation is provided for subsequent casting and hot pressing. In step S2, the TPU casting film is cast on the PET base film with a clean surface, and hot-pressing compounding is carried out, so that the PET-TPU composite base film is formed. The key of the step is to select proper TPU raw materials, and firmly combine the PET base film and the TPU film together through hot-pressing compounding, so as to form the composite base film with higher hardness and light transmittance. In the step S3, the composite base film is subjected to heating and then stretching treatment to generate stretching deformation in the longitudinal direction and the transverse direction, and after heating setting and cooling, the composite film with the film thickness of 0.01-0.04mm is obtained. The treatment ensures that the film layer is more uniform and compact, and improves the strength and stability of the film layer. Finally, in step S3, plasma treatment is performed on the TPU film surface of the composite film to make the dyne value of the surface reach 60 or more. The treatment ensures that the surface of the film has better surface energy and lipophilicity, and obviously improves the printing performance and anti-fog performance of the TPU ink, and in sum, each step plays an indispensable role in preparing the PET-TPU composite film and cooperates with each other, so that the PET-TPU composite film with high hardness, light transmittance, anti-fog performance and excellent printing performance of the TPU ink is finally prepared. Meanwhile, the preparation method is simple and feasible, has low cost and is suitable for mass production.
Preferably, in step S1, the drying temperature is 40-60 ℃ for 3-5 minutes.
Preferably, in step S2, the pressure of the thermocompression bonding is set to 0.1-0.3Mpa, and the temperature of the thermocompression bonding is 130-190 ℃.
By adopting the technical scheme, in the step S2, the pressure of the hot-pressing compounding is set to be 0.1-0.3Mpa, and the setting of the temperature of the hot-pressing compounding to be 130-190 ℃ plays the following roles: by applying pressure, good contact is formed between the PET base film and the TPU casting film, and the contact area of the PET base film and the TPU casting film is increased, so that molecular diffusion and combination between the PET base film and the TPU casting film are promoted. Meanwhile, the thickness of the composite base film can be uniform by proper pressure, and uneven thick films or bubbles are avoided. The temperature of the hot press compounding plays a critical role in the melting of the TPU particles. At the appropriate temperature, the TPU particles may melt to form an adhesive that is intimately bonded to the PET-based film. At the same time, temperature also affects the properties of the composite base film, such as light transmittance and hardness. Through reasonable setting of the pressure and the temperature of hot-pressing compounding, the firm combination of the PET base film and the TPU casting film can be realized, and the PET-TPU composite film with higher hardness, light transmittance, anti-fog performance and excellent TPU ink printing performance is formed.
Preferably, in step S3, the stretching process includes the steps of:
s41, longitudinally stretching the composite base film at 160-300 ℃;
s42, transversely stretching the longitudinally stretched composite base film at 180-200 ℃.
Preferably, the stretching treatment is performed in a state that the PET base film of the composite base film is facing upward and the TPU film is facing downward.
By adopting the above technical scheme, in step S3, the stretching treatment is performed on the compounded base film to change its physical properties and structure, thereby obtaining a composite film having desired properties. Specifically, the method comprises the following steps: s41, longitudinal stretching: the composite base film was placed in a heating apparatus to a suitable temperature of 160-300 c, and then was stretched longitudinally with the PET base film facing upward and the TPU film facing downward. The longitudinal stretching multiplying power is 5-10 times, namely, the composite base film is stretched along the longitudinal direction in the stretching process, so that the length direction of the composite base film is prolonged. S42, transverse stretching: and placing the longitudinally stretched composite base film in heating equipment to reach a proper temperature of 180-200 ℃, and then transversely stretching the composite base film in a state that the PET base film faces upwards and the TPU film faces downwards. The transverse stretching multiplying power is 5-10 times, namely the composite base film is stretched along the transverse direction in the stretching process, so that the width direction of the composite base film is stretched and widened. The two steps aim to change the molecular structure of the composite film through stretching treatment, so that the composite film has more uniform distribution in the longitudinal and transverse directions, and the mechanical property, the light transmission property and the anti-fog property of the film are improved. The stretching treatment can also control the thickness and surface smoothness of the composite film, so that the composite film is more uniform and flexible, and is beneficial to subsequent plasma treatment. Through the series of processing steps, the obtained PET-TPU composite film has higher hardness and light transmittance.
Preferably, in step S41, the surface temperature of the TPU film is controlled not to exceed 205 ℃ during the machine direction stretching.
By adopting the above technical solution, in step S41, the purpose of controlling the surface temperature of the TPU film not to exceed 205 ℃ is to avoid exceeding the heat distortion temperature of the TPU, preventing melting of the material and damage to the shape. The specific actions are as follows: avoiding thermal deformation and shape distortion: exceeding the heat distortion temperature of the TPU may result in melting and shape distortion of the TPU material, which in turn affects the overall performance of the composite film. By controlling the TPU surface temperature to not exceed 205 ℃, the shape stability of the TPU can be maintained during stretching, ensuring the uniformity and flatness of the composite film. Avoiding material damage and quality problems: exceeding the heat distortion temperature of TPU also results in structural failure of the material, such as breakage and crosslinking of molecular chains, and the like, thereby affecting the physical and chemical properties of the composite film. By controlling the TPU surface temperature, the material damage and quality problems can be avoided, and the stability and reliability of the composite film are ensured. Control surface properties: the control of the TPU film surface temperature can also affect the surface properties of the composite film, such as gloss, flatness, and printability. The surface characteristics of the composite film can be optimized by properly controlling the surface temperature, and the requirements of required hardness, light transmittance, anti-fog performance, printing performance and the like are met.
Preferably, in step S3, the setting temperature is set to 260-350 ℃, and the setting time is set to 4-8S.
By adopting the technical scheme, in the step S3, setting of the setting temperature and setting time plays a key role in the performance of the composite membrane. The specific actions are as follows: setting temperature: the sizing temperature is selected to melt and recrystallize the TPU molecules in the composite film, thereby improving the wear resistance, tensile properties and thermal stability of the film. Higher setting temperatures can increase the hardness and heat distortion temperature of the composite film, but excessively high temperatures can cause the film to deform or melt. The proper shaping temperature is selected within the range of 260-350 ℃, so that the composite film can achieve balance among hardness, light transmittance, anti-fog performance and printing performance. Setting time: the shaping time is selected to ensure that the composite film maintains shape and performance stability after stretching. Shorter setting times may result in stress relaxation during stretching, thereby allowing the film to return to its original dimensions, while longer setting times may result in shrinkage and deformation of the film. Proper time is selected within the setting time range of 4-8 seconds, so that the required film thickness and performance stability of the composite film can be ensured after stretching.
Preferably, in step S3, the process conditions of the plasma treatment are as follows: the air pressure is 10-30Pa, the power of the plasma power supply is 500-1000W, and the time is 0.5-5min.
Preferably, the gas used for the plasma treatment includes at least one of pure nitrogen gas, pure helium gas and pure oxygen gas.
Preferably, the gas adopted by the plasma treatment is a combination of pure helium and pure oxygen according to the volume ratio of 1:5-8.
By adopting the technical scheme, in the step S3, the plasma treatment means that plasma excitation treatment is carried out on the TPU film surface of the composite film, and plasma is generated by ionizing gas so as to change the chemical property and the surface property of the surface of the composite film, thereby improving the printing performance and the coating performance of TPU ink. Specifically, the process conditions of the plasma treatment are as follows: air pressure: 10-30Pa, which means the pressure of the gas chamber controlled during plasma treatment, generally the lower the gas pressure, the better the treatment effect. Plasma power supply power: 500-1000W, means that the higher the power the more active the plasma is, the power required to provide plasma excitation. Time: 0.5-5min, refers to the duration of the plasma treatment, i.e. the time required to complete the plasma treatment. The gas used for the plasma treatment includes at least one of pure nitrogen gas, pure helium gas, and pure oxygen gas. The preferred gas combination is pure helium and pure oxygen in a ratio of 1:5-8 by volume. This combination of gases can provide higher plasma activity, which is beneficial to improving the chemical properties and surface characteristics of the composite film surface. The surface of the composite film can be smoother and smoother through plasma treatment, and the wettability and coverage of the composite film are enhanced, so that the adhesive force and the printing performance of TPU ink are improved. In addition, the plasma treatment can also change the energy state and chemical adsorption performance of the surface of the composite film, increase the interaction between the composite film and TPU ink, and improve the stability and accuracy of the printed pattern.
In summary, the beneficial technical effects of the present application are:
1. the hardness of the composite film is improved: the TPU curtain coating film and the PET base film are compounded by hot pressing, and the composite film has higher hardness through stretching treatment and shaping, so that better wear resistance and scratch resistance can be provided.
2. The light transmittance and the antifogging performance of the composite film are improved: the PET base film has good transparency, and the transmittance of the composite film is further improved through compounding and treatment with the TPU casting film, so that the composite film is more transparent.
3. Excellent TPU ink printing performance: after plasma treatment, the dyne value of the TPU film surface of the composite film reaches more than 54mN/m, and the interaction between the TPU film surface and TPU ink is remarkably improved, so that the adhesive force and the printing quality of the ink are improved.
4. The preparation process is simple, the cost is low, and the method is suitable for large-scale production: the whole preparation process comprises the steps of base film pretreatment, tape casting compounding, stretching treatment, plasma treatment and the like, and is simple and easy to operate, and complex equipment and conditions are not needed. And the cost of the required raw materials is relatively low, so that the method is suitable for large-scale production, and the preparation cost can be reduced.
Detailed Description
Embodiments of the present application will be described in detail below with reference to examples, but it will be understood by those skilled in the art that the following examples are only for illustration of the present application and should not be construed as limiting the scope of the present application. The specific conditions are not noted in the examples and are carried out according to conventional conditions or conditions recommended by the manufacturer. The reagents or apparatus used were conventional products commercially available without the manufacturer's attention.
Example 1:
the preparation method of the PET-TPU composite film comprises the following steps:
s1, carrying out electrostatic dust removal pretreatment on a PET base film, and drying at 40 ℃ for 5 minutes to obtain the PET base film with a clean surface, wherein the thickness of the PET base film is 0.50mm.
S2, casting a TPU casting film with the thickness of 0.50mm onto a PET base film with a clean surface, and then carrying out hot pressing compounding on the TPU casting film and the PET base film, wherein the pressure is set to be 0.1Mpa, and the temperature is 190 ℃ to form a compound base film; the raw materials for preparing the TPU casting film are polyether type TPU particles with the average molecular weight of 33000;
s3, heating the composite base film obtained in the step S2, and then stretching the composite base film, wherein the stretching is performed under the condition that the PET base film of the composite base film faces upwards and the TPU film faces downwards, and the composite base film is longitudinally stretched at 160 ℃; transversely stretching the longitudinally stretched composite base film at 180 ℃, wherein the longitudinal stretching multiplying power is 5 times, the transverse stretching multiplying power is 10 times, and the surface temperature of the TPU film is controlled to be 200 ℃; and then heating and shaping, wherein the temperature is set to 260 ℃ and the time is 8s, cooling to prepare a composite film with the film thickness of 0.02mm, and carrying out plasma treatment on the TPU film surface of the composite film, wherein the process conditions are as follows: the air pressure is 10Pa, the power of a plasma power supply is 500W, the time is 5min, and the gas adopted by the plasma treatment is pure nitrogen, so that the PET-TPU composite film is obtained.
Example 2:
the preparation method of the PET-TPU composite film comprises the following steps:
s1, carrying out electrostatic dust removal pretreatment on a PET base film, drying at 60 ℃ for 3 minutes to obtain the PET base film with a clean surface, wherein the thickness of the PET base film is 0.50mm.
S2, casting a TPU casting film with the thickness of 0.50mm onto a PET base film with a clean surface, and then carrying out hot pressing compounding on the TPU casting film and the PET base film, wherein the pressure is set to be 0.3Mpa, and the temperature is 130 ℃ to form a compound base film; the raw materials for preparing the TPU curtain coating film are polyether type TPU particles with the average molecular weight of 36000;
s3, heating the composite base film obtained in the step S2, and then stretching the composite base film, wherein the stretching is performed under the condition that the PET base film of the composite base film faces upwards and the TPU film faces downwards, and the composite base film is longitudinally stretched at 300 ℃; transversely stretching the longitudinally stretched composite base film at 200 ℃, wherein the longitudinal stretching multiplying power is 5 times, the transverse stretching multiplying power is 10 times, and the surface temperature of the TPU film is controlled to be 205 ℃; and then heating and shaping, wherein the temperature is set to 350 ℃, the time is set to 4s, the composite film with the film thickness of 0.02mm is prepared after cooling, and the TPU film surface of the composite film is subjected to plasma treatment, and the process conditions are as follows: the air pressure is 30Pa, the power of a plasma power supply is 1000W, the time is 5min, and the gas adopted by plasma treatment is pure helium, so that the PET-TPU composite film is obtained.
Example 3:
the preparation method of the PET-TPU composite film comprises the following steps:
s1, carrying out electrostatic dust removal pretreatment on a PET base film, and drying at 50 ℃ for 4 minutes to obtain the PET base film with a clean surface, wherein the thickness of the PET base film is 0.50mm.
S2, casting a TPU casting film with the thickness of 0.50mm onto a PET base film with a clean surface, and then carrying out hot pressing compounding on the TPU casting film and the PET base film, wherein the pressure is set to be 0.2Mpa, and the temperature is 150 ℃ to form a compound base film; the raw materials for preparing the TPU curtain coating film are polyether type TPU particles with the average molecular weight of 34000;
s3, heating the composite base film obtained in the step S2, and then stretching the composite base film, wherein the stretching is performed under the condition that the PET base film of the composite base film faces upwards and the TPU film faces downwards, and the composite base film is longitudinally stretched at 250 ℃; transversely stretching the longitudinally stretched composite base film at 190 ℃, wherein the longitudinal stretching multiplying power is 10 times, the transverse stretching multiplying power is 10 times, and the surface temperature of the TPU film is controlled to be 205 ℃; and then heating and shaping, wherein the temperature is set to 300 ℃ for 5 seconds, cooling to prepare a composite film with the film thickness of 0.01mm, and carrying out plasma treatment on the TPU film surface of the composite film, wherein the process conditions are as follows: the air pressure is 20Pa, the power of a plasma power supply is 800W, the time is 1min, and the gas adopted by the plasma treatment is pure oxygen, so that the PET-TPU composite film is obtained.
Example 4:
the preparation method of the PET-TPU composite film comprises the following steps:
s1, carrying out electrostatic dust removal pretreatment on a PET base film, and drying at 50 ℃ for 4 minutes to obtain the PET base film with a clean surface, wherein the thickness of the PET base film is 0.50mm.
S2, casting a TPU casting film with the thickness of 0.50mm onto a PET base film with a clean surface, and then carrying out hot pressing compounding on the TPU casting film and the PET base film, wherein the pressure is set to be 0.2Mpa, and the temperature is 160 ℃ to form a compound base film; the raw materials for preparing the TPU curtain coating film are polyether type TPU particles with the average molecular weight of 35000;
s3, heating the composite base film obtained in the step S2, and then stretching the composite base film, wherein the stretching is performed under the condition that the PET base film of the composite base film faces upwards and the TPU film faces downwards, and the composite base film is longitudinally stretched at 250 ℃; transversely stretching the longitudinally stretched composite base film at 190 ℃, wherein the longitudinal stretching multiplying power is 5 times, the transverse stretching multiplying power is 5 times, and the surface temperature of the TPU film is controlled to be 205 ℃; and then heating and shaping, wherein the temperature is set to 300 ℃ for 5 seconds, cooling to prepare a composite film with the film thickness of 0.04mm, and carrying out plasma treatment on the TPU film surface of the composite film, wherein the process conditions are as follows: the air pressure is 20Pa, the power of a plasma power supply is 800W, the time is 1min, the gas adopted by plasma treatment is a composition of pure helium and pure oxygen according to the volume ratio of 1:6.5, and the PET-TPU composite film is obtained.
Example 5
The same as in example 4, except that in step S3, the plasma treatment was performed using a composition of pure helium and pure oxygen in a volume ratio of 1:8.
Example 6
The same as in example 4, except that in step S3, the plasma treatment was performed using a composition of pure helium and pure oxygen in a volume ratio of 1:5.
Comparative example 1
The same as in example 4, except that in step S3, there is no plasma treatment.
Performance testing
The PET-TPU composite films prepared in examples 1 to 6 and comparative example 1 were subjected to performance tests, and the test results are shown in Table 1: pencil hardness test: according to the method of standard GB/T6739-1996, a film hardness tester by pencil scratch [ Shanghai Pushen chemical machinery Co., ltd; model "BY" ] measures pencil hardness;
haze: measured according to the method specified in GB/T25273;
transmittance: measured according to the method specified in GB/T2410;
definition: sharpness was tested using a haze meter BYK AT-4725;
the value of dyne: the smart 100-type dyne pen is used for testing, and is used for indicating whether the printing performance of the TPU ink is good or not, and the higher the numerical value is, the better the printing performance of the TPU ink is.
TABLE 1
Dyne value/mN/m | Hardness of | Haze/% | Transmittance/% | Definition/% | |
Example 1 | 54 | HB | 0.7 | 93 | 100 |
Example 2 | 56 | HB | 0.8 | 92 | 100 |
Example 3 | 58 | HB | 0.7 | 93 | 100 |
Example 4 | 65 | HB | 0.6 | 94 | 100 |
Example 5 | 63 | HB | 0.6 | 93 | 100 |
Example 6 | 64 | HB | 0.6 | 94 | 100 |
Comparative example 1 | 33 | HB | 0.7 | 92 | 100 |
From Table 1, it is clear that the PET-TPU composite films prepared in examples 1 to 6 have high hardness, light transmittance, antifogging property and excellent TPU ink printing property, and from numerical comparison analysis of the dyne values of the PET-TPU composite films prepared in examples 4 to 6 and examples 2 to 3, it is clear that the gas used in the plasma treatment is a composition of pure helium and pure oxygen in a volume ratio of 1:5 to 8, and the synergistic effect between them is utilized to obtain a PET-TPU composite film which has a higher dyne value and excellent TPU ink printing property.
As can be seen from Table 1, the performance comparison analysis of the PET-TPU composite film prepared in example 4 and comparative example 1 shows that the plasma treatment technology is adopted in the method, so that the PU ink printing performance of the PET-TPU composite film is remarkably improved.
The foregoing embodiments are merely for illustrating the technical solution of the present application and are not intended to be limiting, and although the foregoing embodiments specifically illustrate the present application, it should be understood by those skilled in the relevant art that modifications and equivalents can be made to the specific embodiments of the present application without departing from the spirit and scope of the present application.
Claims (10)
1. The preparation method of the PET-TPU composite film is characterized by comprising the following steps of:
s1, carrying out electrostatic dust removal pretreatment on a PET (polyethylene terephthalate) base film, and drying to obtain the PET base film with a clean surface;
s2, casting the TPU casting film onto a PET base film with a clean surface, and then carrying out hot-pressing compounding on the TPU casting film and the PET base film to form a composite base film; the raw materials for preparing the TPU casting film are polyether type TPU particles with the average molecular weight of 33000-36000;
s3, heating the composite base film obtained in the step S2, performing stretching treatment, wherein the longitudinal stretching multiplying power is 5-10 times, the transverse stretching multiplying power is 5-10 times, heating and shaping, cooling to obtain a composite film with the film thickness of 0.01-0.04mm, and performing plasma treatment on the TPU film surface of the composite film to obtain the PET-TPU composite film.
2. The method of producing a PET-TPU composite film according to claim 1, wherein in step S1, the drying temperature is 4060 ℃ for 3-5 minutes.
3. The method of producing a PET-TPU composite film according to claim 1, wherein in step S2, the pressure of the thermocompression bonding is set to 0.1-0.3MPa, and the temperature is 130-190 ℃.
4. The method for producing a PET-TPU composite film according to claim 1, wherein in step S3, the stretching process comprises the steps of:
s41, longitudinally stretching the composite base film at 160-300 ℃;
s42, transversely stretching the longitudinally stretched composite base film at 180-200 ℃.
5. The method for producing a PET-TPU composite film according to claim 4, wherein the stretching treatment is performed in a state where a PET base film of the composite base film faces upward and a TPU film faces downward.
6. The method according to claim 4, wherein in step S41, the surface temperature of the TPU film is controlled to be not higher than 205 ℃.
7. The method of producing a PET-TPU composite film according to claim 1, wherein in step S3, the setting temperature is set to 260 to 350 ℃ and the setting time is set to 4 to 8S.
8. The method for producing a PET-TPU composite film according to claim 1, wherein in step S3, the process conditions of the plasma treatment are: the air pressure is 10-30Pa, the power of the plasma power supply is 500-1000W, and the time is 0.5-5min.
9. The method for producing a PET-TPU composite film according to claim 8, wherein the gas used for the plasma treatment includes at least one of pure nitrogen gas, pure helium gas, and pure oxygen gas.
10. The method for preparing a PET-TPU composite film according to claim 9, wherein the gas adopted by the plasma treatment is a composition of pure helium and pure oxygen according to a volume ratio of 1:5-8.
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