CN106867012B - Method for modifying PET film by electron beam pre-irradiation grafting - Google Patents
Method for modifying PET film by electron beam pre-irradiation grafting Download PDFInfo
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- C08J7/18—Chemical modification with polymerisable compounds using wave energy or particle radiation
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Abstract
The invention discloses a method for modifying a PET film by electron beam pre-irradiation grafting. The invention provides a method for modifying a PET film by electron beam pre-irradiation grafting, which comprises the following steps: step 1: at room temperature, the PET film is radiated under 0.5 MeV-1.5 MeV electron beams, the radiation dose rate is 8-70 kGy/h, and the absorbed dose is 30-230 kGy, so as to obtain the radiated PET film; step 2: and (2) under the protection of inert gas, in a solvent and in the presence of a monomer polymerization inhibitor, carrying out a grafting reaction on the irradiated PET film obtained in the step (1) and a monomer to obtain an electron beam pre-irradiation grafting modified PET film. The surface modification process of the PET film is simple and easy to implement, high in efficiency and wide in applicability, and the prepared PET film is good in surface hydrophilicity, biocompatibility and printability and beneficial to industrial production.
Description
Technical Field
The invention relates to a method for grafting and modifying a PET film by electron beam pre-irradiation.
Background
The 21 st century is an age of rapid development of polymer materials, various polymer materials exist in almost every aspect of daily life of people, a film product is a very typical material, and the trace of a polymer film can be found in various fields in social production and life. Polyethylene terephthalate (PET) films not only have good barrier properties and solvent resistance, but also have very excellent optical and mechanical properties, and are widely used in the fields of medicine, optics, electronics, packaging and the like. However, the PET film has low surface free energy, and thus has relatively poor properties such as surface wettability and printability, and thus the application of the PET film is limited. Therefore, to expand the range of applications of PET films, it is required to improve the surface hydrophilicity thereof.
Currently, studies on modification of the surface hydrophilicity of a PET film by UV, plasma, gamma-ray radiation, and the like have been conducted more. (Ping X, Wang M Z, Ge X W. the term on patterning composition of n-butyl acrylate and styrene on poly (ethylene terephthalate) film by gamma-ray induced polymerization. radial Phys Chem,2010,79(9):941 946; Song Y W, Do H S, jo H S, et al. Effect of acrylic acid on PET film by irradiation of the PSAs. J adhesives science technique, 2006,20(12): 1357-1365; n J, Suo L, Sun S, et al. Effect of coating composition and injection of coating film by irradiation of PET film by irradiation of PSAs. J adhesives technique, 20(12): 1357-1365; n J, Suo L, Sun S, et al. irradiation of coating composition and coating film by irradiation of PET film by irradiation of coating film 358. PET film coating composition of coating film by irradiation of PET film by irradiation of coating method of PET film coating technique, 2. sub. irradiation of coating film by irradiation of PET film coating technique, 2. sub. 2. irradiation of coating film coating composition of coating film by irradiation of PET film coating method of coating film coating: the UV treatment efficiency is low, the requirements of plasma on treatment atmosphere and equipment are high, the gamma-ray radiation effect is good, but the gamma-ray radiation effect is generally co-radiation grafting, the reaction control is difficult, the gamma-ray device is large in volume, and the shielding requirement is very high, so that the continuous online production of the gamma-ray radiation technology is difficult to realize. Although there are reports occasionally on modification of PET films or sheets with electron beams (Chumakov M K, Shahamat L, Weaver A, et al. Electron beam induced grafting of N-isopyralacetylamide to a poly (ethylene-tert-halate) membrane for rapid cell death benefit. radial Phys Chem,2011,80(2): 182. 189; He C, Gu Z Y. study on the electron beam irradiated and acrylic acid grafted PET M [ J ]. radial Phys Chem,2003,68(5): 873. high.), the electron beam step-wise radiation grafting process is complicated, has low efficiency or employs radiation absorbers (750kGy or so), easily affects performance and does not adversely affect practicality. Therefore, the search for a simple process for modifying the surface hydrophilicity of the PET film is a technical problem which needs to be solved urgently at present.
Disclosure of Invention
The invention aims to overcome the defects of poor surface hydrophilicity, complex modification process, inconvenience for industrial production and the like of a PET film in the prior art and provides a method for modifying the PET film by electron beam pre-irradiation grafting. The surface modification process of the PET film is simple and easy to implement, high in efficiency and wide in applicability, and the prepared PET film is good in surface hydrophilicity, biocompatibility and printability and beneficial to industrial production.
The invention provides a method for modifying a PET film by electron beam pre-irradiation grafting, which comprises the following steps:
step 1: at room temperature, the PET film is radiated under 0.5 MeV-1.5 MeV electron beams, the radiation dose rate is 8-70 kGy/h, and the absorbed dose is 30-230 kGy, so as to obtain the radiated PET film;
step 2: and (2) under the protection of inert gas, in a solvent and in the presence of a monomer polymerization inhibitor, carrying out a grafting reaction on the irradiated PET film obtained in the step (1) and a monomer to obtain an electron beam pre-irradiation grafting modified PET film.
In step 1, the irradiation may be a method and conditions conventional in the art for such operations, and in the present invention, it is particularly preferable to carry out the irradiation in air or an inert atmosphere under normal pressure. The inert atmosphere may be an inert gas as is conventional in the art, preferably nitrogen and/or argon.
In step 1, the electron beam is preferably obtained by an electron accelerator.
In step 1, the PET film is preferably 100 parts, and the thickness of the PET film of 100 parts is preferably 3 to 120 μm, more preferably 15 to 80 μm, for example 35, 50 or 70 μm.
In step 1, the current of the electron beam is preferably 0.9 mA-6.0 mA, such as 2.7mA or 4.0 mA.
In step 1, the kinetic energy of the electron beam is preferably 1.40MeV to 1.50MeV, for example 1.46MeV or 1.48 MeV.
In step 1, the radiation dose rate is preferably 9kGy/h to 70kGy/h, such as 30kGy/h or 50 kGy/h.
In step 1, the absorbed dose is preferably 36kGy to 210kGy, for example 200 kGy.
In the step 1, the irradiated PET film is stored in the air at room temperature for no more than 1 hour.
In step 2, the solvent can be a conventional solvent for such grafting reaction in the field, and water and/or alcohol solvents are particularly preferred in the invention; the water is preferably deionized water; the alcohol solvent is preferably methanol.
In the step 2, the mass fraction ratio of the solvent to the irradiated PET film obtained in the step 1 is preferably 20 to 35, more preferably 20 to 32, for example 25 or 30.
In step 2, the monomer can be a water-soluble monomer which is conventional in the field of such grafting reaction, and one or more of an acrylic acid monomer, an acrylamide monomer and an N-isopropylacrylamide monomer are particularly preferred in the invention.
In the step 2, the mass fraction ratio of the monomer to the irradiated PET film obtained in the step 1 is preferably 15-30, more preferably 18-25, for example 20.
In step 2, the monomer polymerization inhibitor can be a conventional monomer polymerization inhibitor for the grafting reaction of the type in the art, and Mohr's salt is particularly preferred in the present invention.
In the step 2, the mass fraction ratio of the monomeric polymerization inhibitor to the irradiated PET film obtained in the step 1 is preferably 0.01 to 0.06, more preferably 0.02 to 0.05, for example, 0.04 or 0.045.
In step 2, the temperature of the grafting reaction may be a temperature conventional in the art for such grafting reactions, and in the present invention, a temperature of 50 ℃ to 70 ℃, for example 65 ℃, is particularly preferred.
In step 2, the time of the grafting reaction can be monitored by monitoring methods conventional in the art, and is generally the end point of the reaction when the desired grafting rate is reached, and the time of the grafting reaction is preferably 3 hours to 7 hours, such as 5 hours or 6 hours.
In step 2, the inert gas in the inert gas protection may be an inert gas conventional in the art, preferably nitrogen and/or argon, and the inert gas is introduced for a period of time of preferably 20 minutes to 30 minutes, for example 25 minutes. The speed of introducing the inert gas is preferably 0.1L/min to 5L/min, more preferably 0.1L/min to 0.8L/min, for example, 0.3L/min, 0.5L/min or 0.7L/min.
In step 2, the grafting reaction preferably comprises the following post-treatment steps: and after the reaction is finished, cleaning and drying to obtain the grafted modified PET film.
The cleaning and drying can adopt the conventional method adopted in the field, and the cleaning is preferably ultrasonic cleaning; the solvent adopted for cleaning is preferably water and/or an alcohol solvent, and the alcohol solvent is preferably methanol; the number of times of cleaning is preferably 3-5, and the time of each cleaning is preferably 0.5-1 hour. The drying temperature is preferably 50-60 ℃; the drying time is preferably 8 to 10 hours.
The above preferred conditions can be arbitrarily combined to obtain preferred embodiments of the present invention without departing from the common general knowledge in the art.
The reagents and starting materials used in the present invention are commercially available.
In the invention, the room temperature refers to the ambient temperature and is 15-35 ℃.
In the present invention, the normal pressure refers to 1 atmosphere and is 101325 Pa.
The positive progress effects of the invention are as follows:
1) an electron accelerator with lower energy of 0.5-1.5MeV is adopted to radiate the PET film under lower absorbed dose, so that the influence of radiation on the mechanical property of the PET film is reduced to the maximum extent;
2) the surface modification of the PET film by the pre-irradiation grafting method can better control the reaction degree and adjust the thickness of the grafting layer on the surface of the film.
3) The invention adopts the electron beam radiation grafting modified PET film, the preparation process is simple, the efficiency is high, the operation is easy, the applicability is wide, the prepared PET film has good surface hydrophilicity, good biocompatibility and printability and huge industrialization potential. Reactive functional groups such as carboxyl, acylamino and the like are introduced to the surface of the film by grafting, and the PET film with special functions such as an antibacterial film, an ion separation film and the like can be obtained by further processing. The modified PET film prepared by the invention has important application in the fields of medicine, electronics, optics, packaging and the like.
Detailed Description
The invention is further illustrated by the following examples, which are not intended to limit the scope of the invention. The experimental methods without specifying specific conditions in the following examples were selected according to the conventional methods and conditions, or according to the commercial instructions.
Example 1
100 parts by weight of a PET film (thickness 50 μm) was irradiated under an electron beam (1.5MeV, 0.9mA) at a radiation dose rate of 9kGy/h and an absorbed dose of 36kGy in an air atmosphere at room temperature to obtain a irradiated PET film.
100 parts of irradiated PET film were added to a solution consisting of 2500 parts of deionized water and 2500 parts of acrylic monomer, and 4.5 parts Mohr's salt was added. After the above system was purged with nitrogen at room temperature for 20 minutes (the purging rate was about 0.1L/min), it was placed in a water bath and heated to 65 ℃ for 6 hours. And after the reaction is finished, taking out the PET film, ultrasonically cleaning the PET film for 3-5 times by using deionized water and methanol respectively, wherein each time lasts for 0.5 hour, then placing the PET film in an oven, and drying the PET film for 8 hours at the temperature of 50-60 ℃ to obtain the grafted modified PET film. The weight calculation graft yield was 8.5%, and the contact drop after grafting was found to be about 6 ° by the water contact angle test.
Example 2
100 parts by weight of a PET film (thickness: 35 μm) was irradiated under an electron beam (1.46MeV, 4.0mA) at a radiation dose rate of 50kGy/h and an absorbed dose of 200kGy in an air atmosphere at room temperature to obtain a irradiated PET film.
100 parts of irradiated PET film was added to a solution consisting of 3200 parts of deionized water and 1800 parts of an acrylic monomer, and 4 parts of Mohr's salt was added. After the above system was purged with nitrogen at room temperature for 30 minutes (the purging rate was about 0.3L/min), it was placed in a water bath and heated to 70 ℃ for 6 hours. After the reaction is finished, taking out the PET film, ultrasonically cleaning the PET film for 3-5 times by using deionized water and methanol respectively, wherein each time is 0.5 hour, then placing the PET film in an oven, and drying the PET film for 8 hours at the temperature of 60 ℃ to obtain the grafted modified PET film. The weight calculation graft yield was 25.5%, and the contact drop after grafting was found to be about 16 ° by the water contact angle test.
Example 3
100 parts by weight of a PET film (thickness: 80 μm) was irradiated under an electron beam (1.5MeV, 6.0mA) at a radiation dose rate of 70kGy/h and an absorbed dose of 200kGy in an air atmosphere at room temperature to obtain a irradiated PET film.
100 parts of irradiated PET film were added to a solution consisting of 3000 parts of deionized water and 2000 parts of acrylic monomer, and 4 parts of Mohr's salt was added. After nitrogen was introduced into the system at room temperature for 25 minutes (the introduction rate of nitrogen was about 0.5L/min), the system was placed in a water bath and heated to 50 ℃ for 6 hours. After the reaction is finished, taking out the PET film, ultrasonically cleaning the PET film for 3-5 times by using deionized water and methanol respectively, wherein each time is 0.5 hour, then placing the PET film in an oven, and drying the PET film for 8 hours at the temperature of 60 ℃ to obtain the grafted modified PET film. The weight calculation graft yield was 11.1%, and the contact drop after grafting was found to be about 9 ° by the water contact angle test.
Example 4
100 parts by weight of a PET film (thickness: 15 μm) was irradiated under an electron beam (1.48MeV, 2.7mA) at a radiation dose rate of 30kGy/h and an absorbed dose of 36kGy in an air atmosphere at room temperature to obtain a irradiated PET film.
100 parts of irradiated PET film were added to a solution consisting of 3200 parts of methanol and 1800 parts of acrylamide monomer, and 5 parts of Mohr's salt was added. After the above system was purged with nitrogen at room temperature for 20 minutes (the purging rate was about 0.7L/min), it was placed in a water bath and heated to 70 ℃ for 6 hours. After the reaction is finished, taking out the PET film, ultrasonically cleaning the PET film for 3-5 times by using deionized water and methanol respectively, wherein each time is 0.5 hour, then placing the PET film in an oven, and drying the PET film for 8 hours at the temperature of 60 ℃ to obtain the grafted modified PET film. The weight calculation graft yield was 11.5%, and the contact after grafting was found to be reduced by about 10 ° by the water contact angle test.
Example 5
100 parts by weight of a PET film (thickness 70 μm) was irradiated under an electron beam (1.48MeV, 2.7mA) at a radiation dose rate of 70kGy/h and an absorbed dose of 210kGy in an air atmosphere at room temperature to obtain a irradiated PET film.
100 parts of irradiated PET film are added to a solution of 3000 parts of methanol and 2000 parts of N-isopropylacrylamide monomer, 2 parts of Mohr's salt being added. After the above system was purged with nitrogen at room temperature for 30 minutes (the purging rate was about 0.5L/min), it was placed in a water bath and heated to 70 ℃ for 5 hours. After the reaction is finished, taking out the PET film, ultrasonically cleaning the PET film for 3-5 times by using deionized water and methanol respectively, wherein each time is 0.5 hour, then placing the PET film in an oven, and drying the PET film for 8 hours at the temperature of 60 ℃ to obtain the grafted modified PET film. The grafting yield was calculated by weighing as 12% and the contact after grafting was found to be reduced by about 11 ° by water contact angle measurement.
Claims (10)
1. A method for grafting and modifying a PET film by electron beam pre-irradiation is characterized by comprising the following steps:
step 1: at room temperature, the PET film is radiated under 0.5 MeV-1.5 MeV electron beams, the radiation dose rate is 8-70 kGy/h, and the absorbed dose is 30-230 kGy, so as to obtain the radiated PET film;
step 2: and (2) under the protection of inert gas, in a solvent and in the presence of a monomer polymerization inhibitor, carrying out a grafting reaction on the irradiated PET film obtained in the step (1) and a monomer to obtain an electron beam pre-irradiation grafting modified PET film.
2. The method of claim 1, wherein the grafting of the modified PET film by electron beam pre-irradiation comprises: in the step 1, the radiation is carried out in air or inert atmosphere under normal pressure;
and/or the presence of a gas in the gas,
in the step 1, the electron beam is obtained by an electron accelerator;
and/or the presence of a gas in the gas,
in the step 1, 100 parts of PET film is used, and the thickness of 100 parts of PET film is 3-120 μm;
and/or the presence of a gas in the gas,
in the step 1, the current of the electron beam is 0.9 mA-6.0 mA;
and/or the presence of a gas in the gas,
in step 1, the kinetic energy of the electron beam is 1.40 MeV-1.50 MeV.
3. The method of electron beam pre-irradiation graft modification of PET film as claimed in claim 2, wherein: in the step 1, nitrogen and/or argon is/are adopted as the inert atmosphere;
and/or the presence of a gas in the gas,
in the step 1, the thickness of 100 parts of PET film is 15-80 μm;
and/or the presence of a gas in the gas,
in the step 1, the current of the electron beam is 2.7mA or 4.0 mA;
and/or the presence of a gas in the gas,
in step 1, the kinetic energy of the electron beam is 1.46MeV or 1.48 MeV.
4. The method of claim 1, wherein the grafting of the modified PET film by electron beam pre-irradiation comprises: in the step 1, the radiation dose rate is 9 kGy/h-70 kGy/h;
and/or the presence of a gas in the gas,
in the step 1, the absorbed dose is 36 kGy-210 kGy;
and/or the presence of a gas in the gas,
in the step 1, the irradiated PET film is stored in the air at room temperature for no more than 1 hour.
5. The method of claim 4, wherein the grafting of the modified PET film by electron beam pre-irradiation comprises: in the step 1, the radiation dose rate is 30kGy/h or 50 kGy/h;
and/or the presence of a gas in the gas,
in step 1, the absorbed dose is 200 kGy.
6. The method of claim 1, wherein the grafting of the modified PET film by electron beam pre-irradiation comprises: in the step 2, the solvent water and/or the alcohol solvent;
and/or the presence of a gas in the gas,
in the step 2, the mass fraction ratio of the solvent to the irradiated PET film obtained in the step 1 is 20-35;
and/or the presence of a gas in the gas,
in the step 2, the monomer is one or more of acrylic acid monomer, acrylamide monomer and N-isopropyl acrylamide monomer;
and/or the presence of a gas in the gas,
in the step 2, the mass fraction ratio of the monomer to the irradiated PET film obtained in the step 1 is 15-30;
and/or the presence of a gas in the gas,
in the step 2, the monomer polymerization inhibitor is molal salt;
and/or the presence of a gas in the gas,
in the step 2, the mass fraction ratio of the monomer polymerization inhibitor to the irradiated PET film obtained in the step 1 is 0.01-0.06;
and/or the presence of a gas in the gas,
in the step 2, the temperature of the grafting reaction is 50-70 ℃;
and/or the presence of a gas in the gas,
in the step 2, the grafting reaction time is 3 to 7 hours;
and/or the presence of a gas in the gas,
in the step 2, the inert gas in the inert gas protection is nitrogen and/or argon.
7. The method of claim 6, wherein the grafting of the modified PET film by electron beam pre-irradiation comprises: in the step 2, the water is deionized water;
and/or the presence of a gas in the gas,
in the step 2, the alcohol solvent is methanol;
and/or the presence of a gas in the gas,
in the step 2, the mass fraction ratio of the solvent to the irradiated PET film obtained in the step 1 is 20-32;
and/or the presence of a gas in the gas,
in the step 2, the mass fraction ratio of the monomer to the irradiated PET film obtained in the step 1 is 18-25;
and/or the presence of a gas in the gas,
in the step 2, the mass fraction ratio of the monomer polymerization inhibitor to the irradiated PET film obtained in the step 1 is 0.02-0.05;
and/or the presence of a gas in the gas,
in the step 2, the temperature of the grafting reaction is 65 ℃;
and/or the presence of a gas in the gas,
in the step 2, the grafting reaction time is 5 hours or 6 hours;
and/or the presence of a gas in the gas,
in the step 2, the inert gas is introduced for 20 to 30 minutes;
and/or the presence of a gas in the gas,
in the step 2, the speed of introducing the inert gas is 0.1L/min-5L/min.
8. The method of electron beam pre-irradiation graft modification of PET film as claimed in claim 7, wherein: in the step 2, the mass fraction ratio of the solvent to the irradiated PET film obtained in the step 1 is 25 or 30;
and/or the presence of a gas in the gas,
in the step 2, the mass fraction ratio of the monomer to the irradiated PET film obtained in the step 1 is 20;
and/or the presence of a gas in the gas,
in the step 2, the mass fraction ratio of the monomer polymerization inhibitor to the irradiated PET film obtained in the step 1 is 0.04 or 0.045;
and/or the presence of a gas in the gas,
in the step 2, the inert gas is introduced for 25 minutes;
and/or the presence of a gas in the gas,
in the step 2, the speed of introducing the inert gas is 0.1L/min-0.8L/min.
9. The method of claim 1, wherein the grafting of the modified PET film by electron beam pre-irradiation comprises: in step 2, the grafting reaction comprises the following post-treatment steps: and after the reaction is finished, cleaning and drying to obtain the grafted modified PET film.
10. The method of electron beam pre-irradiation graft modification of PET film as claimed in claim 9, wherein: in the post-treatment step of the grafting reaction in the step 2, the cleaning is ultrasonic cleaning;
and/or the presence of a gas in the gas,
the solvent adopted for cleaning is water and/or an alcohol solvent;
and/or the presence of a gas in the gas,
the cleaning times are 3-5 times, and the cleaning time is 0.5-1 hour each time;
and/or the presence of a gas in the gas,
the drying temperature is 50-60 ℃;
and/or the presence of a gas in the gas,
the drying time is 8-10 hours.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1370795A (en) * | 2001-02-26 | 2002-09-25 | 四川大学 | Pre-irradiation grafting technoogical process of preparing antifogging polyethylene film |
| CN102644196A (en) * | 2012-04-29 | 2012-08-22 | 中国人民解放军总后勤部军需装备研究所 | Processing method for improving hydrophilicity of polyester fiber and fabric of polyester fiber |
| CN104744720A (en) * | 2013-12-31 | 2015-07-01 | 吉林师范大学 | Preparation method of polyvinylpyrrolidone grafting modified polyethylene terephthalate film |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1370795A (en) * | 2001-02-26 | 2002-09-25 | 四川大学 | Pre-irradiation grafting technoogical process of preparing antifogging polyethylene film |
| CN102644196A (en) * | 2012-04-29 | 2012-08-22 | 中国人民解放军总后勤部军需装备研究所 | Processing method for improving hydrophilicity of polyester fiber and fabric of polyester fiber |
| CN104744720A (en) * | 2013-12-31 | 2015-07-01 | 吉林师范大学 | Preparation method of polyvinylpyrrolidone grafting modified polyethylene terephthalate film |
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