An antistatic epoxy resin composite coating and its preparation method

Abstract

This invention relates to the field of coating technology and discloses an antistatic epoxy resin composite coating. Compared with pure-phase epoxy resin coatings, epoxy resin coatings with added quaternized polyacrylate grafted graphene have better antistatic properties and mechanical strength. Graphene and epoxy resin matrix materials form a highly conductive network structure, which not only increases the conductivity of the coating but also increases the mechanical strength of the epoxy resin coating. Adding quaternary ammonium salt to the coating can further reduce the resistivity of the epoxy resin coating and increase its antistatic properties. Grafting quaternary ammonium salt onto the graphene surface can not only promote the synergistic effect between the two and increase the antistatic properties of the coating, but also avoid the precipitation behavior of quaternary ammonium salt in the matrix. When polyacrylate is added to the coating, it increases the mechanical strength of the epoxy resin coating.

Description

Technical Field

[0001] This invention relates to the field of coating technology, specifically to an antistatic epoxy resin composite coating and its preparation method. Background Technology

[0002] With the miniaturization of electronic devices and the high integration of circuits, the power density of electronic devices is gradually increasing, and the electrostatic sensitivity of their electronic components is also increasing. The application of various epoxy resin materials in the manufacturing process and application of electronic components makes the generation of electrostatic charges easier and more widespread. With the increase of electrostatic charges accumulating on the material surface, it may cause many hazards to electronic components, such as dust trapping, which can cause electric field interference, leading to electrostatic discharge with sparks and a large amount of heat, thereby reducing material performance and even damaging sealed circuits. Therefore, improving the antistatic performance of components is of great significance to ensuring the safe and reliable operation of electronic components.

[0003] Epoxy resins are frequently used for encapsulation in electronic devices due to their excellent processability. However, their inherent insulating properties make them unsuitable for meeting the ever-increasing antistatic requirements of modern electronic devices. As a conventional technique to prevent the accumulation of static charge in epoxy resin matrix materials, methods typically involve mixing antistatic agents into the epoxy resin or applying antistatic agents to the epoxy resin surface. Chinese Patent Publication No. CN106010118A discloses an epoxy resin coating with antistatic properties and its preparation method, and Chinese Patent Publication No. CN106010141B discloses a method for preparing a uniform antistatic coating. Although both methods involve adding a pure-phase antistatic agent... While improving the antistatic properties of epoxy resin coatings, issues such as low antistatic performance and high addition amounts still exist. Therefore, using more efficient antistatic agents has become a key direction for improving epoxy resin coatings. Various nanoparticles with high electrical conductivity have been used as fillers to improve the antistatic properties of epoxy resin-based composites, such as carbon nanotubes and graphene. Graphene has attracted much attention in the field of antistatic materials due to its exceptional electrical properties. In addition, quaternary ammonium salts are also commonly used antistatic agents, but they have poor compatibility with the coating matrix and are prone to precipitating onto the coating surface during use, thus losing and reducing the antistatic effect of the coating. Grafting them onto the graphene surface can avoid such problems.

[0004] (a) Technical problems to be solved

[0005] To address the shortcomings of existing technologies, this invention provides an antistatic epoxy resin composite coating and its preparation method, solving the problems of poor antistatic ability and low mechanical strength of epoxy resin coatings.

[0006] (II) Technical Solution

[0007] To achieve the above objectives, the present invention provides the following technical solution: an antistatic epoxy resin composite coating, wherein the preparation method of the antistatic epoxy resin composite coating includes the following steps:

[0008] (1) Graphene oxide was ultrasonically dispersed in N,N-dimethylformamide at a mass ratio of 10:4500-8000:18-40:80-200. Then γ-methacryloyloxypropyltrimethoxysilane and ethanol solvent were added. After adjusting the pH to 3-6 h, the reaction was carried out at 50-80 °C for 8-20 h. After the reaction was completed, vinyl graphene was obtained.

[0009] (2) Dissolve vinyl graphene and emulsifier OP-10 in deionized water and stir. Then add butyl acrylate, ethyl acrylate, glycidyl acrylate, acrylic acid and initiator ammonium persulfate (APS). After stirring evenly, carry out the reaction. After the reaction is completed, polyacrylate grafted graphene is obtained.

[0010] (3) Place polyacrylate-grafted graphene, epichlorohydrin, and triphenylphosphine (PPh3) catalyst in a reaction flask, stir evenly, and then carry out the reaction. After the reaction is completed, chlorinated polyacrylate-grafted graphene is obtained.

[0011] (4) Chlorinated polyacrylate-grafted graphene and N,N-dimethylethylenediamine were stirred evenly and then reacted to obtain quaternized polyacrylate-grafted graphene.

[0012] (5) Epoxy resin and quaternized polyacrylate grafted graphene are ultrasonically dispersed in deionized water and dispersed until uniform under high-speed shear force. Then, the mixture is ground by sand milling. Next, defoamer polyether modified organosilicon and leveling agent hydroxypropyl methylcellulose are added and stirred evenly. Then, epoxy curing agent is added and stirred evenly. After standing, an antistatic epoxy resin composite coating is obtained.

[0013] Preferably, in step (2), the mass ratio between vinyl graphene, emulsifier OP-10, deionized water, butyl acrylate, ethyl acrylate, glycidyl acrylate, acrylic acid and ammonium persulfate is 100:350-800:1600-3000:30-60:30-60:15-30:35-80:7-15.

[0014] Preferably, the reaction temperature in step (2) is 60-90℃ and the reaction time is 4-10h.

[0015] Preferably, in step (3), the mass ratio between polyacrylate-grafted graphene, epichlorohydrin and triphenylphosphine is 100:45-80:0.3-0.8.

[0016] Preferably, the reaction temperature in step (3) is 80-120℃ and the reaction time is 8-20h.

[0017] Preferably, in step (4), the mass ratio between chlorinated polyacrylate-grafted graphene and N,N-dimethylethylenediamine is 100:35-90.

[0018] Preferably, the reaction temperature in step (4) is 50-90℃ and the reaction time is 5-12h.

[0019] Preferably, the type of curing agent in step (5) includes tetrahydromethylphthalic anhydride or hexahydrophthalic anhydride.

[0020] Preferably, in step (5), the mass ratio of epoxy resin, quaternized polyacrylate grafted graphene, deionized water, polyether modified organosilicon, hydroxypropyl methylcellulose and epoxy curing agent is 100:2-6:20-40:0.5-1:0.35-0.8:25-60.

[0021] (iii) Beneficial technical effects

[0022] Compared with the prior art, the present invention has the following experimental principles and beneficial technical effects:

[0023] This antistatic epoxy resin composite coating is prepared by first modifying the surface of graphene oxide with γ-methacryloxypropyltrimethoxysilane to obtain vinyl graphene. Then, the solution is emulsified with emulsifier OP-10. Using ammonium persulfate as an initiator, the alkenyl groups of vinyl graphene undergo an in-situ polymerization reaction with butyl acrylate, ethyl acrylate, glycidyl acrylate, and acrylic acid to obtain polyacrylate-grafted graphene. Next, using triphenylphosphine as a catalyst, the carboxyl groups in the polyacrylate-grafted graphene undergo a ring-opening reaction with the epoxy groups of epichlorohydrin to obtain chlorinated polyacrylate-grafted graphene. Then, the chlorinated polyacrylate-grafted graphene undergoes a quaternization reaction with N,N-dimethylethylenediamine to obtain quaternized polyacrylate-grafted graphene. Finally, the antistatic epoxy resin composite coating is prepared by physical blending.

[0024] This antistatic epoxy resin composite coating, compared to pure-phase epoxy resin coatings, exhibits better antistatic properties and mechanical strength when combined with quaternized polyacrylate-grafted graphene. Graphene, as an excellent conductive material, is added to the epoxy resin matrix coating to form a highly conductive network structure, increasing the coating's conductivity. 2The hybrid structure reduces the resistance to electron transport in the coating, allowing them to move freely within the crystal lattice. Furthermore, when the coating is subjected to external forces, the graphene-epoxy resin network structure helps to disperse stress throughout the entire coating structure, preventing stress concentration and damage. This increases the mechanical strength of the epoxy resin coating. Adding quaternary ammonium salts further reduces the resistivity of the epoxy resin coating, increasing its antistatic properties. Quaternary ammonium salts contain numerous carbon chains and polar ionic functional groups. The carbon chains can intertwine with the epoxy resin structure, achieving compatibilization, while the polar functional groups have good hydrophilicity, absorbing water molecules from the substrate surface to form a conductive film structure, further enhancing the coating's structural integrity. The increased conductivity and reduced resistance of graphene by grafting quaternary ammonium salts onto the graphene surface not only promote the synergistic effect between the two and increase the antistatic properties of the coating, but also prevent the precipitation of quaternary ammonium salts in the matrix, thus increasing the stability of the antistatic coating. The amino groups of quaternary ammonium salts can also act as amine promoters, while simultaneously affecting epoxy resins and acid anhydride curing agents, reducing the reactivity of the curing agents, improving the performance of the cured product, reducing the harm of acid curing agents, and promoting the curing behavior of epoxy resins. Adding polyacrylate to epoxy resin coatings can improve the mechanical strength of the coating. When polyacrylate is added to the coating, under the action of external force, the coating will develop crazes. The crazes absorb a large amount of destructive energy during their appearance, development, and fracture, thus increasing the mechanical strength of the epoxy resin coating. Attached Figure Description

[0025] Figure 1 This is a schematic diagram of the structure of polyacrylate-grafted graphene;

[0026] Figure 2 It is a reaction formula of polyacrylate grafted graphene and epichlorohydrin.

[0027] Figure 3 It is a reaction formula of chlorinated polyacrylate grafted graphene and N,N-dimethylethylenediamine. Detailed Implementation

[0028] To achieve the above objectives, the present invention provides the following specific embodiments and examples: an antistatic epoxy resin composite coating, the preparation method of which includes the following steps:

[0029] (1) Graphene oxide was ultrasonically dispersed in N,N-dimethylformamide at a mass ratio of 10:4500-8000:18-40:80-200. Then γ-methacryloyloxypropyltrimethoxysilane and ethanol solvent were added. After adjusting the pH to 3-6h, the reaction was carried out at 50-80℃ for 8-20h. After the reaction was completed, the mixture was filtered and washed with ethanol 2-4 times. Vinyl graphene was obtained completely at 40-60℃.

[0030] (2) According to the mass ratio of 100:350-800:1600-3000:30-60:30-60:15-30:35-80:7-15, vinyl graphene and emulsifier OP-10 are dissolved in deionized water and stirred. Then, butyl acrylate, ethyl acrylate, glycidyl acrylate, acrylic acid and initiator ammonium persulfate (APS) are added. After stirring evenly, the reaction is carried out at 60-90℃ for 4-10h. After the reaction is completed, the graphene is centrifuged at 4000-6000r / min and washed to obtain polyacrylate-grafted graphene.

[0031] (3) According to the mass ratio of 100:45-80:0.3-0.8, polyacrylate-grafted graphene, epichlorohydrin, and catalyst triphenylphosphine (PPh3) are placed in a reaction flask, stirred evenly, and reacted at 80-120℃ for 8-20h. After the reaction is completed, the mixture is filtered and washed with ethanol to obtain chlorinated polyacrylate-grafted graphene.

[0032] (4) Chlorinated polyacrylate-grafted graphene and N,N-dimethylethylenediamine were mixed at a mass ratio of 100:35-90 and reacted at 50-90℃ for 5-12h. After filtration, the mixture was washed with ethanol to obtain quaternized polyacrylate-grafted graphene.

[0033] (5) Epoxy resin and quaternized polyacrylate grafted graphene are ultrasonically dispersed in deionized water according to a mass ratio of 100:2-6:20-40:0.5-1:0.35-0.8:25-60, and dispersed until uniform under high-speed shear force. Then, the mixture is ground by sand milling. Next, defoamer polyether modified organosilicon and leveling agent hydroxypropyl methylcellulose are added and stirred evenly. Then, epoxy curing agent is added, including tetrahydromethylphthalic anhydride or hexahydrophthalic anhydride. After stirring evenly, the mixture is allowed to stand to obtain an antistatic epoxy resin composite coating.

[0034] Example 1

[0035] (1) 5g of graphene oxide was ultrasonically dispersed in 2500g of N,N-dimethylformamide, and then 9g of γ-methacryloyloxypropyltrimethoxysilane and 40g of ethanol solvent were added. After adjusting the pH to 3h, the reaction was carried out at 50℃ for 8h. After the reaction was completed, the mixture was filtered and washed twice with ethanol. The reaction was carried out at 40℃ until vinyl graphene was completely obtained.

[0036] (2) Dissolve 5g vinyl graphene and 17.5g emulsifier OP-10 in 80g deionized water and stir. Then add 1.5g butyl acrylate, 1.5g ethyl acrylate, 0.75g glycidyl acrylate, 1.75g ​​acrylic acid and 0.35g initiator ammonium persulfate (APS). After stirring evenly, react at 60℃ for 4h. After the reaction is completed, centrifuge at 4000r / min and wash to obtain polyacrylate-grafted graphene.

[0037] (3) Place 4g of polyacrylate-grafted graphene, 1.8g of epichlorohydrin, and 0.012g of catalyst triphenylphosphine (PPh3) in a reaction flask, stir evenly, and react at 80°C for 8h. After the reaction is complete, filter and wash with ethanol to obtain chlorinated polyacrylate-grafted graphene.

[0038] (4) 4g of chlorinated polyacrylate-grafted graphene and 1.4g of N,N-dimethylethylenediamine were stirred evenly and reacted at 50°C for 5h. After filtration, the mixture was washed with ethanol to obtain quaternized polyacrylate-grafted graphene.

[0039] (5) 10g of epoxy resin and 0.2g of quaternized polyacrylate grafted graphene were ultrasonically dispersed in 2g of deionized water and dispersed until uniform under high-speed shear force. Then, the mixture was ground by sand milling. Next, 0.05g of defoamer polyether modified organosilicon and 0.035g of leveling agent hydroxypropyl methylcellulose were added and stirred evenly. Then, 2.5g of epoxy curing agent was added. The type of curing agent included tetrahydromethylphthalic anhydride or hexahydrophthalic anhydride. After stirring evenly, the mixture was allowed to stand to obtain an antistatic epoxy resin composite coating.

[0040] Example 2

[0041] (1) 5g of graphene oxide was ultrasonically dispersed in 3000g of N,N-dimethylformamide, and then 10g of γ-methacryloyloxypropyltrimethoxysilane and 60g of ethanol solvent were added. After adjusting the pH to 4h, the reaction was carried out at 60℃ for 10h. After the reaction was completed, the mixture was filtered and washed twice with ethanol. The reaction was carried out at 45℃ until vinyl graphene was completely obtained.

[0042] (2) Dissolve 5g vinyl graphene and 20g emulsifier OP-10 in 100g deionized water and stir. Then add 2g butyl acrylate, 2g ethyl acrylate, 1g glycidyl acrylate, 2g acrylic acid and 0.4g initiator ammonium persulfate (APS). After stirring evenly, react at 70℃ for 5h. After the reaction is completed, centrifuge at 4500r / min and wash to obtain polyacrylate-grafted graphene.

[0043] (3) Place 4g of polyacrylate-grafted graphene, 2.4g of epichlorohydrin, and 0.016g of triphenylphosphine (PPh3) catalyst in a reaction flask, stir evenly, and react at 90°C for 10h. After the reaction is completed, filter and wash with ethanol to obtain chlorinated polyacrylate-grafted graphene.

[0044] (4) 4g of chlorinated polyacrylate-grafted graphene and 2g of N,N-dimethylethylenediamine were stirred evenly and reacted at 60°C for 6h. After filtration, the mixture was washed with ethanol to obtain quaternized polyacrylate-grafted graphene.

[0045] (5) 10g of epoxy resin and 0.3g of quaternized polyacrylate grafted graphene were ultrasonically dispersed in 2.5g of deionized water and dispersed until uniform under high-speed shear force. Then, the mixture was ground by sand milling. Next, 0.06g of defoamer polyether modified organosilicon and 0.04g of leveling agent hydroxypropyl methylcellulose were added and stirred evenly. Then, 3g of epoxy curing agent was added. The type of curing agent included tetrahydromethyl phthalic anhydride or hexahydrophthalic anhydride. After stirring evenly, the mixture was allowed to stand to obtain an antistatic epoxy resin composite coating. Example 3

[0046] (1) 5g of graphene oxide was ultrasonically dispersed in 3500g of N,N-dimethylformamide, and then 16g of γ-methacryloyloxypropyltrimethoxysilane and 80g of ethanol solvent were added. After adjusting the pH to 5h, the reaction was carried out at 70℃ for 16h. After the reaction was completed, the mixture was filtered and washed three times with ethanol. The reaction was carried out at 50℃ until vinyl graphene was completely obtained.

[0047] (2) Dissolve 5g vinyl graphene and 30g emulsifier OP-10 in 120g deionized water and stir. Then add 2.5g butyl acrylate, 2.5g ethyl acrylate, 1.2g glycidyl acrylate, 3g acrylic acid and 0.6g initiator ammonium persulfate (APS). After stirring evenly, react at 80℃ for 8h. After the reaction is completed, centrifuge at 5000r / min and wash to obtain polyacrylate-grafted graphene.

[0048] (3) Place 4g of polyacrylate-grafted graphene, 2.8g of epichlorohydrin, and 0.028g of triphenylphosphine (PPh3) catalyst in a reaction flask, stir evenly, and react at 100℃ for 16h. After the reaction is completed, filter and wash with ethanol to obtain chlorinated polyacrylate-grafted graphene.

[0049] (4) 4g of chlorinated polyacrylate-grafted graphene and 3.2g of N,N-dimethylethylenediamine were stirred evenly and reacted at 80°C for 10h. After filtration, the mixture was washed with ethanol to obtain quaternized polyacrylate-grafted graphene.

[0050] (5) 10g of epoxy resin and 0.5g of quaternized polyacrylate grafted graphene were ultrasonically dispersed in 3.5g of deionized water and dispersed until uniform under high-speed shear force. Then, the mixture was ground by sand milling. Next, 0.08g of defoamer polyether modified organosilicon and 0.06g of leveling agent hydroxypropyl methylcellulose were added and stirred evenly. Then, 5g of epoxy curing agent was added. The type of curing agent included tetrahydromethyl phthalic anhydride or hexahydrophthalic anhydride. After stirring evenly, the mixture was allowed to stand to obtain an antistatic epoxy resin composite coating. Example 4

[0051] (1) 5g of graphene oxide was ultrasonically dispersed in 4000g of N,N-dimethylformamide, and then 20g of γ-methacryloyloxypropyltrimethoxysilane and 100g of ethanol solvent were added. After adjusting the pH to 6h, the reaction was carried out at 80℃ for 20h. After the reaction was completed, the mixture was filtered and washed 4 times with ethanol. The reaction was carried out at 60℃ until vinyl graphene was completely obtained.

[0052] (2) Dissolve 5g vinyl graphene and 40g emulsifier OP-10 in 150g deionized water and stir. Then add 3g butyl acrylate, 3g ethyl acrylate, 1.5g glycidyl acrylate, 4g acrylic acid and 0.75g initiator ammonium persulfate (APS). After stirring evenly, react at 90℃ for 10h. After the reaction is completed, centrifuge at 6000r / min and wash to obtain polyacrylate-grafted graphene.

[0053] (3) Place 4g of polyacrylate-grafted graphene, 3.2g of epichlorohydrin, and 0.032g of triphenylphosphine (PPh3) catalyst in a reaction flask, stir evenly, and react at 120℃ for 20h. After the reaction is completed, filter and wash with ethanol to obtain chlorinated polyacrylate-grafted graphene.

[0054] (4) 4g of chlorinated polyacrylate-grafted graphene and 3.6g of N,N-dimethylethylenediamine were stirred evenly and reacted at 90°C for 12h. After filtration, the mixture was washed with ethanol to obtain quaternized polyacrylate-grafted graphene.

[0055] (5) 10g of epoxy resin and 0.6g of quaternized polyacrylate grafted graphene were ultrasonically dispersed in 4g of deionized water and dispersed until uniform under high-speed shear force. Then, the mixture was ground by sand milling. Next, 0.1g of defoaming agent polyether modified organosilicon and 0.08g of leveling agent hydroxypropyl methylcellulose were added and stirred evenly. Then, 6g of epoxy curing agent was added. The type of curing agent included tetrahydromethyl phthalic anhydride or hexahydrophthalic anhydride. After stirring evenly, the mixture was allowed to stand to obtain an antistatic epoxy resin composite coating.

[0056] Comparative Example 1

[0057] (1) 5g of graphene oxide was ultrasonically dispersed in 3000g of N,N-dimethylformamide, and then 10g of γ-methacryloyloxypropyltrimethoxysilane and 60g of ethanol solvent were added. After adjusting the pH to 4h, the reaction was carried out at 60℃ for 10h. After the reaction was completed, the mixture was filtered and washed 3 times with ethanol. The reaction was carried out at 40℃ until vinyl graphene was completely obtained.

[0058] (2) Dissolve 5g vinyl graphene and 20g emulsifier OP-10 in 120g deionized water and stir. Then add 2.4g butyl acrylate, 2.4g ethyl acrylate, 1.2g glycidyl acrylate, 2g acrylic acid and 0.4g ammonium persulfate (APS) initiator. After stirring evenly, react at 80℃ for 8h. After the reaction is completed, centrifuge at 4500r / min and wash to obtain polyacrylate-grafted graphene.

[0059] (3) 10g of epoxy resin and 0.3g of polyacrylate-grafted graphene were ultrasonically dispersed in 3g of deionized water and dispersed until uniform under high-speed shear force. Then, the mixture was ground by sand milling. Next, 0.08g of defoamer polyether modified organosilicon and 0.06g of leveling agent hydroxypropyl methylcellulose were added and stirred evenly. Then, 4g of epoxy curing agent was added. The type of curing agent included tetrahydromethylphthalic anhydride or hexahydrophthalic anhydride. After stirring evenly, the mixture was allowed to stand to obtain an antistatic epoxy resin composite coating.

[0060] Comparative Example 2

[0061] (1) 10g of epoxy resin and 0.3g of graphene were ultrasonically dispersed in 2g of deionized water and dispersed until uniform under high-speed shear force. Then, the mixture was ground by sand milling. Next, 0.08g of defoamer polyether modified organosilicon and 0.07g of leveling agent hydroxypropyl methylcellulose were added and stirred evenly. Then, 4g of epoxy curing agent was added. The type of curing agent included tetrahydromethyl phthalic anhydride or hexahydrophthalic anhydride. After stirring evenly, the mixture was allowed to stand to obtain an antistatic epoxy resin composite coating.

[0062] Resistivity tests were conducted on antistatic epoxy resin composite coatings according to the national standard GB / T 11210-2014.

[0063] test Example 1 Example 2 Example 3 Example 4 Comparative Example 1 Comparative Example 2 Resistivity (Ω) <![CDATA[1.70×10 9 ]]> <![CDATA[2.71×10 6 ]]> <![CDATA[6.28×10 5 ]]> <![CDATA[7.67×10 8 ]]> <![CDATA[3.15×10 12 ]]> <![CDATA[8.08×10 12 ]]>

[0064] Mechanical strength tests were conducted on antistatic epoxy resin composite coatings in accordance with the national standard GB / T 1732—1979(88).

[0065]

Claims

1. A method for preparing an antistatic epoxy resin composite coating, characterized in that: The antistatic epoxy resin composite coating is prepared by the following steps: (1) Graphene oxide was ultrasonically dispersed in N,N-dimethylformamide at a mass ratio of 10:4500-8000:18-40:80-200. Then γ-methacryloyloxypropyltrimethoxysilane and ethanol solvent were added. After adjusting the pH to 3-6 h, the reaction was carried out at 50-80 °C for 8-20 h. After the reaction was completed, vinyl graphene was obtained. (2) Dissolve vinyl graphene and emulsifier OP-10 in deionized water and stir. Then add butyl acrylate, ethyl acrylate, glycidyl acrylate, acrylic acid and initiator ammonium persulfate (APS). After stirring evenly, carry out the reaction. After the reaction is completed, polyacrylate grafted graphene is obtained. (3) Place polyacrylate-grafted graphene, epichlorohydrin, and triphenylphosphine (PPh3) catalyst in a reaction flask, stir evenly, and then carry out the reaction. After the reaction is completed, chlorinated polyacrylate-grafted graphene is obtained. (4) Chlorinated polyacrylate-grafted graphene and N,N-dimethylethylenediamine were stirred evenly and then reacted to obtain quaternized polyacrylate-grafted graphene. (5) Epoxy resin and quaternized polyacrylate grafted graphene are ultrasonically dispersed in deionized water and dispersed until uniform under high-speed shear force. Then, the mixture is ground by sand milling. Next, defoamer polyether modified organosilicon and leveling agent hydroxypropyl methylcellulose are added and stirred evenly. Then, epoxy curing agent is added and stirred evenly. After standing, an antistatic epoxy resin composite coating is obtained.

2. The method for preparing an antistatic epoxy resin composite coating according to claim 1, characterized in that: In step (2), the mass ratio of vinyl graphene, emulsifier OP-10, deionized water, butyl acrylate, ethyl acrylate, glycidyl acrylate, acrylic acid and ammonium persulfate is 100:350-800:1600-3000:30-60:30-60:15-30:35-80:7-15.

3. The method for preparing an antistatic epoxy resin composite coating according to claim 1, characterized in that: The reaction temperature in step (2) is 60-90℃ and the reaction time is 4-10h.

4. The method for preparing an antistatic epoxy resin composite coating according to claim 1, characterized in that: In step (3), the mass ratio of polyacrylate-grafted graphene, epichlorohydrin and triphenylphosphine is 100:45-80:0.3-0.

8.

5. The method for preparing an antistatic epoxy resin composite coating according to claim 1, characterized in that: The reaction temperature in step (3) is 80-120℃ and the reaction time is 8-20h.

6. The method for preparing an antistatic epoxy resin composite coating according to claim 1, characterized in that: In step (4), the mass ratio between chlorinated polyacrylate-grafted graphene and N,N-dimethylethylenediamine is 100:35-90.

7. The method for preparing an antistatic epoxy resin composite coating according to claim 1, characterized in that: The reaction temperature in step (4) is 50-90℃ and the reaction time is 5-12h.

8. The method for preparing an antistatic epoxy resin composite coating according to claim 1, characterized in that: The curing agent in step (5) includes tetrahydromethylphthalic anhydride or hexahydrophthalic anhydride.

9. The method for preparing an antistatic epoxy resin composite coating according to claim 1, characterized in that: In step (5), the mass ratio of epoxy resin, quaternized polyacrylate grafted graphene, deionized water, polyether modified organosilicon, hydroxypropyl methylcellulose and epoxy curing agent is 100:2-6:20-40:0.5-1:0.35-0.8:25-60.

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