Preparation method of antistatic polyester film

By introducing modified nanopowders and surface conductive layers into the polyester material, the problem of easy loss of the anti-static polyester film electrostatic layer is solved, and a long-term stable anti-static effect is achieved.

CN118955984BActive Publication Date: 2025-07-18SHENZHEN XINGLIDONG TECH
View PDF 3 Cites 0 Cited by

Patent Information

Application Number
CN202411046028.9
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2024-08-01
Publication Date
2025-07-18
Estimated Expiration
2044-08-01

AI Technical Summary

Technical Problem

The existing anti-static polyester film is prone to damage and loss during long-term use, resulting in the gradual weakening of the anti-static effect and being unable to maintain it for a long time.

Method used

By introducing modified nanopowders into the polyester material, a nickel layer is plated on the surface of the carbon nanotubes by electroless plating, and combined with aluminum units doping zinc oxide nanopowders to form a conductive network, a three-dimensional current network chain is constructed, and a conductive layer is formed on the surface of the polyester film, and anti-static properties are enhanced by swelling agents.

Benefits of technology

Polyester film maintains excellent antistatic properties during long-term use, is not affected by surface damage, has low resistance, and significantly improves the antistatic effect.

✦ Generated by Eureka AI based on patent content.
Patent Text Reader

Abstract

The present invention relates to the technical field of polyester film processing, and particularly relates to a preparation method of an antistatic polyester film. S1: Blend a polyester matrix with modified nano-powders and granulate to obtain a polyester masterbatch; S2: Melt-blend the polyester masterbatch, cast film through a die head, longitudinally draw, transversely draw, and wind and form to obtain a semi-finished polyester film; S3: Immerse the semi-finished polyester film in a swelling liquid, soak it and then take it out, evenly spray a treatment liquid on the surface, place it in an oven, and dry it. In the present invention, by introducing conductive modified nano-powders into the polyester material and simultaneously forming a conductive layer on its surface layer, the formed polyester film has good conductivity and low-resistance performance, thus having an antistatic effect. And during long-term use, even if the conductive layer on the surface layer is damaged or lost, it will not have a substantial impact on the antistatic property, and the polyester film can still be used normally.
Need to check novelty before this filing date? Find Prior Art

Description

Technical Field

[0001] The present invention relates to the technical field of polyester film processing, and specifically provides a method for preparing an antistatic polyester film. Background Art

[0002] Polyester films have good comprehensive properties and are widely used in fields such as electronics, electrical appliances, and optics. However, as a polymer insulating material, polyester films have a relatively high resistivity themselves and are prone to generating static electricity due to friction during production and use, which brings many inconveniences to the application of polyester films. Especially when applied in the field of electronics and electrical appliances, static electricity discharge phenomena can cause semiconductor failure and affect product performance. Therefore, antistatic modification of polyester films has very important practical significance. The antistatic property represents the property of discharging the charges accumulated on the surface of an insulating material by an appropriate method. In order to improve the antistatic property of polyester films, generally, an antistatic layer or a conductive layer can be formed on the surface of the polyester film, or conductive or antistatic substances (such as metals, carbon powders, antistatic agents, etc.) can be added to the polyester material matrix to effectively discharge the charges accumulated on the surface.

[0003] For example, the invention patent with the publication number CN116041770A discloses a method for preparing an antistatic polyester film. This film uses the suspension interface assembly method to achieve the single-sided enrichment of conductive TiO2, improving the utilization rate of conductive TiO2. The suspension interface assembly method realizes the single-sided enrichment of conductive TiO2 particles, greatly improving the utilization efficiency of conductive TiO2, and its surface resistance can be reduced to 10 6 Ω / sq. Under the same addition amount of conductive TiO2, compared with the melt blending method and the surface coating method, it has decreased by 5 orders of magnitude. In addition, the suspension interface modification also greatly improves the surface hydrophilicity of the antistatic PET film, and the surface contact angle decreases to 25°. The polyester film prepared by this method has excellent antistatic performance; since this technical solution realizes the antistatic effect by forming an electrostatic layer on the surface of the polyester film, however, this polyester film is not resistant to water washing, and during long-term use, affected by various factors, the electrostatic layer on the surface is prone to breakage and loss, resulting in the antistatic effect of the polyester film becoming worse and worse over time and not having long-term use performance. Summary of the Invention

[0004] Aiming at the problems existing in the prior art, the purpose of the present invention is to provide a method for preparing an antistatic polyester film.

[0005] To achieve the above purpose, the present invention provides the following technical solutions:

[0006] A method for preparing an antistatic polyester film specifically includes the following steps:

[0007] S1. Blend the polyester matrix with the modified nano-powders and granulate to obtain a polyester masterbatch;

[0008] S2. Melt-blend the polyester masterbatch, cast films through a die, longitudinally stretch, transversely stretch, and wind up to form a semi-finished polyester film;

[0009] S3. Immerse the semi-finished polyester film in a swelling solution, soak it at 80 - 90 °C for 20 - 50 min. After taking it out, evenly spray the treatment liquid on the surface, place it in an oven, dry it at 95 - 98 °C, control the total air volume in the oven to be 25000 - 30000 m 3 / h, and dry for 90 - 120 s.

[0010] As a further preferred embodiment of the present invention, the mass ratio of the polyester matrix to the modified nano-powders is (75 - 85):(15 - 25).

[0011] As a further preferred embodiment of the present invention, the preparation method of the modified nano-powders is as follows:

[0012] 1) Add carbon nanotubes to a mixed solution composed of stannous chloride and hydrochloric acid solution at 93 - 98 °C for sensitization treatment for 45 - 60 min, adjust the pH value to 2.0 - 2.5 with urea, filter and wash, and dry to constant weight at 85 - 90 °C. Then place it in a nickel sulfate solution, soak it at room temperature for 10 - 30 min, wash with water, reduce it with potassium borohydride for 15 - 30 min, and then immerse it in an electroless plating solution, and perform plating solution treatment at 85 - 89 °C and pH of 6.0 - 6.5 for 3 - 7 h. After drying, obtain modified carbon nanotubes;

[0013] 2) Dissolve zinc chloride and aluminum nitrate in deionized water, then add polyethylene glycol, stir at 300 - 500 r / min for 30 - 50 min to obtain a mixed solution. Prepare a mixed alkali solution according to sodium hydroxide and sodium carbonate, and then dropwise add the mixed alkali solution to the mixed solution under magnetic stirring, ensuring that the pH value during the reaction is 7.5 - 8.5, react at 60 - 65 °C for 2 - 5 h. After the reaction is completed, let the product stand for aging for 2 - 5 h, wash it repeatedly with deionized water and then dry it to obtain a precursor powder;

[0014] 3) Place the precursor powder in a tubular furnace, keep it at 300 - 350 °C for 2 - 4 h, then raise the temperature to 800 - 860 °C and continue to keep it for 2 - 4 h. After naturally cooling to room temperature, mix the product with the modified carbon nanotubes in a mass ratio of 1:(2 - 6) and perform ball milling for 2 - 5 h to obtain the modified nano-powders.

[0015] As a further preferred embodiment of the present invention, in step 1), the mass ratio of the stannous chloride to the hydrochloric acid solution is 1:(3 - 5);

[0016] The concentration of the hydrochloric acid solution is 1-3 mol / L;

[0017] The concentration of the nickel sulfate solution is 0.2-0.5 mol / L;

[0018] The electroless plating solution is composed of 25-30 g / L of nickel sulfate, 20-26 g / L of sodium dihydrogen phosphate, 15-18 g / L of sodium citrate, and 5-8 g / L of sodium acetate.

[0019] As a further preferred embodiment of the present invention, in step 2), in the mixed solution, the dosage ratios of zinc chloride, aluminum nitrate, deionized water, and polyethylene glycol are (10-16) g:(0.1-0.2) g:(80-130) mL:(0.2-0.5) g;

[0020] In the mixed alkali solution, the molar ratio of sodium hydroxide to sodium carbonate is (2.0-2.6):1.

[0021] As a further preferred embodiment of the present invention, in step 3), the rotation speed of the ball milling is 120-180 r / min.

[0022] As a further preferred embodiment of the present invention, the swelling solution is composed of toluene, p-xylene, m-xylene, and 1,1,2,2-tetrachloroethane in a mass ratio of 1:(0.5-1.2):(0.2-0.7):(0.5-1.8).

[0023] As a further preferred embodiment of the present invention, the preparation method of the treatment solution is as follows:

[0024] 1) Add multi-walled carbon nanotubes, a dispersant, and ethyl acetate into a ball mill and ball mill for 45-50 h, then in a centrifuge, centrifuge at a rotation speed of 8000-10000 r / min for 5-10 min, take the supernatant to obtain a multi-walled carbon nanotube dispersion;

[0025] 2) Add the organosilicon resin into toluene, stir and disperse evenly, then add a platinum catalyst and the multi-walled carbon nanotube dispersion, and stir and disperse evenly.

[0026] As a further preferred embodiment of the present invention, in step 1), the dosage ratios of the multi-walled carbon nanotubes, the dispersant, and ethyl acetate are (4-9) g:(4.5-9.8) g:(400-600) mL;

[0027] The dispersant is composed of dispersant BYK-2155 and dispersant BYK-9076 in a mass ratio of (4-9):(0.5-0.8);

[0028] The rotation speed of the centrifugation is 8000-10000 r / min.

[0029] As a further preferred embodiment of the present invention, in step 2), the dosage ratio of the silicone resin, toluene, platinum catalyst, and multi-walled carbon nanotube dispersion is (5-10) g:(5-10) mL:(0.1-0.3) g:(2-5) mL.

[0030] Compared with the prior art, the beneficial effects of the present invention are as follows:

[0031] In the present invention, carbon nanotubes are used as the matrix material, and a nickel layer is plated on its surface by electroless plating to obtain modified carbon nanotubes. The plated metal nickel layer endows the matrix material with stable conductivity. When introduced into the polyester material, the polyester material has good conductivity. At the same time, due to the large aspect ratio of the filled modified carbon nanotubes, the percolation threshold of the polyester material is reduced, so it has good antistatic properties. Moreover, the modified carbon nanotubes form three-dimensional contacts in the polyester material, constructing a conductive network and forming a parallel structure with the polyester material. The current will preferentially flow along the low-resistance modified carbon nanotubes and bypass the high-resistance polyester material matrix. The three-dimensional current network chain composed of modified carbon nanotubes plays a controlling role in the conductivity of the overall system, thus greatly improving the conductivity of the polyester material and making it have good antistatic effects. At the same time, in the present invention, nano-powders of aluminum-doped zinc oxide are obtained by chemical co-precipitation method, and they are physically combined with modified carbon nanotubes by ball milling. By doping aluminum units in zinc oxide, the nano-powders exhibit a well-crystallized hexagonal wurtzite structure, and with the appropriate increase in the doping amount of aluminum units, the electrical properties of the nano-powders are improved. After being combined with modified carbon nanotubes, they can exhibit more excellent electrical properties and, when introduced into the polyester material, significantly improve its antistatic performance.

[0032] At the same time, in order to further enhance the antistatic performance of the polyester material, in the present invention, a treatment liquid is prepared with a multi-walled carbon nanotube dispersion with a small tube diameter as the conductive functional body and a silicone resin as the matrix material. After swelling the surface of the polyester film with a swelling agent, the substances in the treatment liquid can penetrate into the surface layer of the polyester film to construct a conductive layer, thereby reducing the surface resistance of the polyester film and achieving the antistatic effect, so that the polyester film has a more excellent antistatic effect.

[0033] In the present invention, by introducing conductive modified nano-powders into the polyester material and forming a conductive layer on its surface layer, the formed polyester film has good conductivity and low-resistance performance, thus having an antistatic effect. And during long-term use, even if the conductive layer on the surface layer is damaged or lost, it will not have a substantial impact on the antistatic property, and the polyester film can still be used normally. Detailed implementation manners

[0034] The technical solutions in the embodiments of the present invention will be clearly and completely described below. Obviously, the described embodiments are only a part of the embodiments of the present invention, rather than all the embodiments. All other embodiments obtained by those of ordinary skill in the art based on the embodiments of the present invention without creative efforts belong to the scope of protection of the present invention.

[0035] Embodiment 1

[0036] A preparation method of an antistatic polyester film specifically includes the following steps:

[0037] S1. Blend the polyester matrix and the modified nano powder in a mass ratio of 75:25, and granulate to obtain a polyester masterbatch;

[0038] S2. Melt-blend the polyester masterbatch, cast film through a die head, longitudinally draw, transversely draw, and wind up to form a semi-finished polyester film;

[0039] S3. Immerse the semi-finished polyester film in a swelling solution, soak it at 80 °C for 20 min, take it out, evenly spray the treatment solution on the surface, place it in an oven, dry it at 95 °C, and control the total air volume in the oven to be 25000 m 3 / h, and dry for 90 s;

[0040] Among them, the swelling solution is composed of toluene, p-xylene, m-xylene, and 1,1,2,2-tetrachloroethane in a mass ratio of 1:0.5:0.2:0.5.

[0041] Among them, the preparation method of the modified nano powder is as follows:

[0042] 1) Add carbon nanotubes to a mixed solution composed of stannous chloride and a hydrochloric acid solution with a concentration of 1 mol / L at 93 °C for sensitization treatment for 45 min. The mass ratio of stannous chloride to the hydrochloric acid solution is 1:3. Adjust the pH value to 2.0 with urea, filter, wash, and dry at 85 °C to constant weight. Then place it in a nickel sulfate solution with a concentration of 0.2 mol / L, soak it at room temperature for 10 min, wash it with water, reduce it with potassium borohydride for 15 min, and then immerse it in a chemical plating solution. Perform plating solution treatment at 85 °C and pH 6.0 for 3 h, and dry it to obtain modified carbon nanotubes;

[0043] Among them, the chemical plating solution is composed of 25 g / L nickel sulfate, 20 g / L sodium dihydrogen phosphate, 15 g / L sodium citrate, and 5 g / L sodium acetate;

[0044] 2) Dissolve 10 g of zinc chloride and 0.1 g of aluminum nitrate in 80 mL of deionized water, then add 0.2 g of polyethylene glycol, stir at 300 r / min for 30 min to obtain a mixed solution. Prepare a mixed alkali solution according to a molar ratio of sodium hydroxide to sodium carbonate of 2:1, and then dropwise add the mixed alkali solution to the mixed solution under magnetic stirring, ensuring that the pH value during the reaction is 7.5. React at 60 °C for 2 h. After the reaction is completed, let the product stand for aging for 2 h, wash it repeatedly with deionized water and then dry it to obtain the precursor powder;

[0045] 3) Place the precursor powder in a tube furnace, keep it at 300 °C for 2 h, then raise the temperature to 800 °C and continue to keep it for 2 h. After naturally cooling to room temperature, mix the product with modified carbon nanotubes in a mass ratio of 1:2 and then carry out ball milling. Ball mill at a rotation speed of 120 r / min for 2 h to obtain the modified nano powder.

[0046] Among them, the preparation method of the treatment liquid is as follows:

[0047] 1) Add 4 g of multi-walled carbon nanotubes, 4 g of dispersant BYK-2155, 0.5 g of dispersant BYK-9076, and 400 mL of ethyl acetate to the ball mill and ball mill for 45 h. Then, in a centrifuge, centrifuge at a rotation speed of 8000 r / min for 5 min, take the supernatant to obtain the multi-walled carbon nanotube dispersion;

[0048] 2) Add 5 g of silicone resin to 5 mL of toluene, stir well to disperse evenly, then add 0.1 g of platinum catalyst and 2 mL of multi-walled carbon nanotube dispersion, and stir well to disperse evenly.

[0049] Example 2

[0050] A preparation method of an antistatic polyester film specifically includes the following steps:

[0051] S1. Blend the polyester matrix and the modified nano powder in a mass ratio of 80:20, and granulate to obtain a polyester masterbatch;

[0052] S2. Melt-blend the polyester masterbatch, cast film through a die head, longitudinally stretch, horizontally stretch, and wind up to form a semi-finished polyester film;

[0053] S3. Immerse the semi-finished polyester film in a swelling solution, soak it at 85 °C for 35 min, take it out, evenly spray the treatment liquid on the surface, place it in an oven, dry it at 96 °C, and control the total air volume in the oven to be 28000 m 3 / h, and dry for 110 s;

[0054] Among them, the swelling liquid is composed of toluene, p-xylene, m-xylene, and 1,1,2,2-tetrachloroethane in a mass ratio of 1:0.7:0.5:1.3.

[0055] Among them, the preparation method of the modified nano powder is as follows:

[0056] 1) At 95 °C, add carbon nanotubes to a mixed solution composed of stannous chloride and a hydrochloric acid solution with a concentration of 2 mol / L for sensitization treatment for 55 min. The mass ratio of stannous chloride to the hydrochloric acid solution is 1:4. Use urea to adjust the pH value to 2.5. After filtration and washing, dry at 87 °C to constant weight, then place it in a nickel sulfate solution with a concentration of 0.3 mol / L, soak at room temperature for 20 min, wash with water, and then reduce it with potassium borohydride for 25 min. Then immerse it in the electroless plating solution and perform plating solution treatment at 86 °C and pH 6.5 for 5 h. After drying, obtain modified carbon nanotubes;

[0057] Among them, the electroless plating solution is composed of 27 g / L nickel sulfate, 23 g / L sodium dihydrogen phosphate, 17 g / L sodium citrate, and 7 g / L sodium acetate;

[0058] 2) Dissolve 15 g of zinc chloride and 0.2 g of aluminum nitrate in 120 mL of deionized water, then add 0.3 g of polyethylene glycol, stir at 400 r / min for 40 min to obtain a mixed solution. Prepare a mixed alkali solution according to the molar ratio of sodium hydroxide to sodium carbonate of 2.3:1. Then, dropwise add the mixed alkali solution to the mixed solution under magnetic stirring, ensuring that the pH value during the reaction is 8. React at 63 °C for 3 h. After the reaction ends, let the product stand for aging for 3 h, wash repeatedly with deionized water, and then dry to obtain the precursor powder;

[0059] 3) Place the precursor powder in a tubular furnace, keep it at 320 °C for 3 h, then raise the temperature to 850 °C and continue to keep it for 3 h. After natural cooling to room temperature, mix the product with the modified carbon nanotubes in a mass ratio of 1:5, and then perform ball milling at a rotation speed of 150 r / min for 3 h to obtain the modified nano powder.

[0060] Among them, the preparation method of the treatment liquid is as follows:

[0061] 1) Add 7 g of multi-walled carbon nanotubes, 7 g of dispersant BYK-2155, 0.7 g of dispersant BYK-9076, and 500 mL of ethyl acetate to the ball mill and ball mill for 46 h. Then, in a centrifuge, centrifuge at a speed of 9000 r / min for 7 min, take the supernatant to obtain the multi-walled carbon nanotube dispersion;

[0062] 2) Add 8 g of silicone resin to 8 mL of toluene, stir well to disperse evenly, then add 0.2 g of platinum catalyst and 3 mL of multi-walled carbon nanotube dispersion, and stir well to disperse evenly.

[0063] Example 3

[0064] A method for preparing an antistatic polyester film specifically includes the following steps:

[0065] S1. Blend the polyester matrix and the modified nano powder in a mass ratio of 85:15, and granulate to obtain a polyester masterbatch;

[0066] S2. Melt-blend the polyester masterbatch, cast a film through a die, longitudinally draw, transversely draw, and wind up to form a semi-finished polyester film;

[0067] S3. Immerse the semi-finished polyester film in a swelling solution, soak it at 90 °C for 50 min, take it out, evenly spray the treatment solution on the surface, place it in an oven, dry it at 98 °C, and control the total air volume in the oven to be 30000 m 3 / h, and dry for 120 s;

[0068] Among them, the swelling solution is composed of toluene, p-xylene, m-xylene, and 1,1,2,2-tetrachloroethane in a mass ratio of 1:1.2:0.7:1.8.

[0069] Among them, the preparation method of the modified nano powder is as follows:

[0070] 1) Add carbon nanotubes to a mixed solution composed of stannous chloride and a hydrochloric acid solution with a concentration of 3 mol / L at 98 °C for sensitization treatment for 60 min. The mass ratio of stannous chloride to the hydrochloric acid solution is 1:5. Adjust the pH value to 2.5 with urea, filter and wash, dry to constant weight at 90 °C, then place it in a nickel sulfate solution with a concentration of 0.5 mol / L, soak it at room temperature for 30 min, wash it with water, reduce it with potassium borohydride for 30 min, and then immerse it in an electroless plating solution. Perform plating solution treatment at 89 °C and pH 6.5 for 7 h, and dry it to obtain modified carbon nanotubes;

[0071] Among them, the electroless plating solution is composed of 30 g / L of nickel sulfate, 26 g / L of sodium dihydrogen phosphate, 18 g / L of sodium citrate, and 8 g / L of sodium acetate;

[0072] 2) Dissolve 16 g of zinc chloride and 0.2 g of aluminum nitrate in 130 mL of deionized water, then add 0.5 g of polyethylene glycol, stir at 500 r / min for 50 min to obtain a mixed solution. Prepare a mixed alkali solution according to the molar ratio of sodium hydroxide to sodium carbonate of 2.6:1, and then dropwise add the mixed alkali solution to the mixed solution under magnetic stirring, ensuring that the pH value during the reaction is 8.5. React at 65 °C for 5 h. After the reaction is completed, let the product stand for aging for 5 h, wash it repeatedly with deionized water, and then dry it to obtain the precursor powder;

[0073] 3) Place the precursor powder in a tube furnace, keep it at 350 °C for 4 h, then heat it to 860 °C and continue to keep it for 4 h. After natural cooling to room temperature, mix the product with modified carbon nanotubes in a mass ratio of 1:6 and then perform ball milling. Ball mill at a rotation speed of 180 r / min for 5 h to obtain the modified nano powder.

[0074] Among them, the preparation method of the treatment liquid is as follows:

[0075] 1) Add 9 g of multi-walled carbon nanotubes, 9 g of dispersant BYK-2155, 0.8 g of dispersant BYK-9076, and 600 mL of ethyl acetate to the ball mill and ball mill for 50 h. Then, in a centrifuge, centrifuge at a speed of 10000 r / min for 10 min, take the supernatant to obtain the multi-walled carbon nanotube dispersion;

[0076] 2) Add 10 g of silicone resin to 10 mL of toluene, stir well to disperse evenly, then add 0.3 g of platinum catalyst and 5 mL of multi-walled carbon nanotube dispersion, and stir well to disperse evenly.

[0077] Comparative Example 1: This comparative example is basically the same as Example 1, except that it does not contain the modified nano powder.

[0078] Comparative Example 2: This comparative example is basically the same as Example 1, except that in the preparation of the modified nano powder, step 1) is omitted.

[0079] Comparative Example 3: This comparative example is basically the same as Example 1, except that in the preparation of the modified nano powder, step 2) is omitted.

[0080] Comparative Example 4: This comparative example is basically the same as Example 1, except that it does not contain the treatment liquid.

[0081] Comparative Example 5: This comparative example is basically the same as Example 1, except that in the preparation of the treatment liquid, step 1) is omitted.

[0082] Testing experiment:

[0083] Using the methods provided in Examples 1-3 and Comparative Examples 1-5, antistatic polyester film samples were processed respectively, and then their antistatic properties were tested. The specific results are shown in Table 1;

[0084] For the antistatic property test, in an environment with a temperature of 23 °C and a humidity of 50% RH, the antistatic polyester film sample was placed in an antistatic property tester (Mitsubishi Corporation, MCP-T600), and then its surface resistance was measured based on JIS K7194.

[0085] Table 1

[0086] Example 1 Example 2 Example 3 Comparative Example 1 Surface resistance Ω / sq <![CDATA[4.15×10 4 > <![CDATA[4.06×10 4 > <![CDATA[4.11×10 4 > <![CDATA[3.68×10 8 > Comparative Example 2 Comparative Example 3 Comparative Example 4 Comparative Example 5 Surface resistance Ω / sq <![CDATA[5.23×10 6 > <![CDATA[6.89×10 6 > <![CDATA[8.57×10 5 > <![CDATA[7.02×10 5 >

[0087] As can be seen from Table 1, the antistatic polyester film prepared in the present invention has the characteristic of low surface resistance and can exhibit excellent antistatic performance.

[0088] The preferred embodiments of the present invention disclosed above are only used to help illustrate the present invention. The preferred embodiments do not describe all the details in detail, nor do they limit the invention to the specific embodiments described. Obviously, many modifications and changes can be made according to the content of this specification. These embodiments are selected and specifically described in this specification to better explain the principle and practical application of the present invention, so that those skilled in the art can understand and utilize the present invention well. The present invention is only limited by the claims and their full scope and equivalents.

Claims

1. A method for preparing an antistatic polyester film, characterized in that, Specifically, it includes the following steps: S1. Blend the polyester matrix with the modified nano powder and granulate to obtain a polyester masterbatch; S2. Melt-blend the polyester masterbatch, cast film through a die head, longitudinally draw, transversely draw, and wind up to form a semi-finished polyester film; S3. Immerse the semi-finished polyester film in the swelling solution, soak it at 80 - 90 °C for 20 - 50 min. After taking it out, evenly spray the treatment liquid on the surface, place it in an oven, and dry it at 95 - 98 °C, controlling the total air volume in the oven to be 25000 - 30000 m 3 / h, and dry it for 90 - 120 s; The preparation method of the modified nano powder is as follows: 1) Add carbon nanotubes to a mixed solution composed of stannous chloride and hydrochloric acid solution at 93 - 98 °C for sensitization treatment for 45 - 60 min. Adjust the pH value to 2.0 - 2.5 using urea, filter and wash, dry to constant weight at 85 - 90 °C, then place it in a nickel sulfate solution, soak at room temperature for 10 - 30 min, wash with water, reduce with potassium borohydride for 15 - 30 min, and then immerse it in a chemical plating solution. Perform plating solution treatment at 85 - 89 °C and pH of 6.0 - 6.5 for 3 - 7 h, and dry to obtain modified carbon nanotubes; 2) Dissolve zinc chloride and aluminum nitrate in deionized water, then add polyethylene glycol, stir at 300 - 500 r / min for 30 - 50 min to obtain a mixed solution. Prepare a mixed alkali solution according to sodium hydroxide and sodium carbonate, and then dropwise add the mixed alkali solution to the mixed solution under magnetic stirring, ensuring that the pH value during the reaction is 7.5 - 8.5, react at 60 - 65 °C for 2 - 5 h. After the reaction ends, let the product stand for aging for 2 - 5 h, wash repeatedly with deionized water and then dry to obtain a precursor powder; 3) Place the precursor powder in a tubular furnace, keep it at 300 - 350 °C for 2 - 4 h, then raise the temperature to 800 - 860 °C and continue to keep it for 2 - 4 h. After naturally cooling to room temperature, mix the product with the modified carbon nanotubes in a mass ratio of 1:(2 - 6) and perform ball milling for 2 - 5 h to obtain the modified nano powder; The preparation method of the treatment solution is as follows: 1) Add multi-walled carbon nanotubes, a dispersant, and ethyl acetate to a ball mill and ball mill for 45 - 50 h, then centrifuge in a centrifuge at a speed of 8000 - 10000 r / min for 5 - 10 min, take the supernatant to obtain a multi-walled carbon nanotube dispersion; 2) Add silicone resin to toluene, stir well to disperse evenly, then add a platinum catalyst and the multi-walled carbon nanotube dispersion, and stir well to disperse evenly.

2. The preparation method of an antistatic polyester film according to claim 1, characterized in that, The mass ratio of the polyester matrix to the modified nano powder is (75 - 85):(15 - 25).

3. The preparation method of an antistatic polyester film according to claim 1, wherein In step 1), the mass ratio of the stannous chloride to the hydrochloric acid solution is 1:(3 - 5); The concentration of the hydrochloric acid solution is 1 - 3 mol / L; The concentration of the nickel sulfate solution is 0.2 - 0.5 mol / L; The chemical plating solution is composed of 25 - 30 g / L of nickel sulfate, 20 - 26 g / L of sodium dihydrogen phosphate, 15 - 18 g / L of sodium citrate, and 5 - 8 g / L of sodium acetate.

4. The preparation method of an antistatic polyester film according to claim 1, characterized in that, In step 2), in the mixed solution, the dosage ratio of zinc chloride, aluminum nitrate, deionized water, and polyethylene glycol is (10 - 16) g:(0.1 - 0.2) g:(80 - 130) mL:(0.2 - 0.5) g; In the mixed alkali solution, the molar ratio of sodium hydroxide to sodium carbonate is (2.0 - 2.6):

1.

5. The preparation method of an antistatic polyester film according to claim 1, wherein, In step 3), the rotation speed of the ball milling is 120 - 180 r / min.

6. The preparation method of an antistatic polyester film according to claim 1, wherein, The swelling solution is composed of toluene, p-xylene, m-xylene, and 1,1,2,2-tetrachloroethane in a mass ratio of 1:(0.5 - 1.2):(0.2 - 0.7):(0.5 - 1.8).

7. The preparation method of an antistatic polyester film according to claim 1, characterized in that, In step 1), the dosage ratio of the multi-walled carbon nanotubes, dispersant, and ethyl acetate is (4 - 9) g:(4.5 - 9.8) g:(400 - 600) mL; The dispersant is composed of dispersant BYK-2155 and dispersant BYK-9076 in a mass ratio of (4 - 9):(0.5 - 0.8); The rotation speed of the centrifugation is 8000 - 10000 r / min.

8. The preparation method of an antistatic polyester film according to claim 7, characterized in that, In step 2), the dosage ratio of the silicone resin, toluene, platinum catalyst, and multi-walled carbon nanotube dispersion is (5 - 10) g:(5 - 10) mL:(0.1 - 0.3) g:(2 - 5) mL.

Citation Information

Patent Citations

  • Preparation method of antistatic polyester film

    CN116041770A

  • Wide band electromagnetic wave-shielded polyethylene compound film containing nickel-plating carbon nanotube and preparation method thereof

    CN101362389A

  • Antistatic polyester film and preparation method thereof

    CN116426020A