Flame-retardant antistatic coating and method for producing the same

Abstract

The present application relates to the technical field of paint, and discloses a kind of fire-retardant antistatic paint, the fire-retardant antistatic paint includes the following weight parts raw materials: 25-30 parts epoxy resin, 20-25 parts solvent, double effect agent 10-15 parts doped with whisker, coordination reinforcing agent 4-8 parts, hydroxymethyl cellulose 3-6 parts, flame retardant 4-8 parts, isocyanate curing agent 3-5 parts.The fire-retardant antistatic paint of the present application is made of epoxy resin, hydroxymethyl cellulose, flame retardant, isocyanate curing agent and solvent, double effect agent doped with whisker and coordination reinforcing agent.The paint has excellent antistatic and fire-retardant properties, and the performance of the two can be improved coordinately.The stability of the product's washability is significantly improved.

Description

Technical Field

[0001] This invention relates to the field of coating technology, specifically to a flame-retardant and antistatic coating and its preparation method. Background Technology

[0002] Static electricity buildup on equipment materials can render the equipment unusable, causing malfunctions in precision instruments and damage to electronic components. Antistatic coatings not only conduct current quickly and eliminate static charge, but also ensure the safe operation of equipment.

[0003] Existing antistatic coatings do not possess antistatic properties. To improve antistatic properties, antistatic agents are added to give them antistatic functions, but the antistatic performance of the products is generally poor. At the same time, in order to improve the antistatic effect, the flame retardancy of the products will be reduced accordingly. It is difficult to coordinate the improvement of the flame retardancy and antistatic performance of the products, which limits the efficiency of the products and results in poor stability of the washability, further reducing the efficiency of the products. Summary of the Invention

[0004] In view of the deficiencies of the prior art, the purpose of this invention is to provide a flame-retardant and antistatic coating and its preparation method, so as to solve the problems mentioned in the background art.

[0005] The present invention solves the technical problem by adopting the following technical solution:

[0006] This invention provides a flame-retardant and antistatic coating, which comprises the following raw materials in parts by weight:

[0007] 25-30 parts epoxy resin, 20-25 parts solvent, 10-15 parts dual-effect agent with doped whiskers, 4-8 parts coordinating reinforcing agent, 3-6 parts hydroxymethyl cellulose, 4-8 parts flame retardant, and 3-5 parts isocyanate curing agent.

[0008] Preferably, the flame-retardant and antistatic coating comprises the following raw materials in parts by weight:

[0009] 27.5 parts epoxy resin, 22.5 parts solvent, 12.5 parts dual-effect agent with doped whiskers, 6 parts coordinating reinforcing agent, 4.5 parts hydroxymethyl cellulose, 6 parts flame retardant, and 4 parts isocyanate curing agent.

[0010] Preferably, the isocyanate curing agent is one of Bayhydur and XP2655; the solvent is xylene; and the flame retardant is a mixture of ammonium polyphosphate, melamine, and pentaerythritol in a weight ratio of 2:2:1.

[0011] Preferably, the method for preparing the doped whisker dual-effect agent is as follows:

[0012] S01: First, place the zinc oxide whiskers in a mixed acid solution with a volume of 4-6 times the total volume of the zinc oxide whiskers and stir evenly. Then wash with water, dry, preheat at 110-120℃ for 5-10 minutes, and then air cool to room temperature to obtain pretreated zinc oxide whiskers.

[0013] SO2: Add 2-5 parts of lanthanum chloride solution to 10-15 parts of sodium dodecyl sulfate solution, then add 1-3 parts of phosphate buffer solution and 2-5 parts of nano-silica sol, stir thoroughly to obtain the conditioning base solution;

[0014] S03: Mix modified sheet graphene and pretreated zinc oxide whiskers at a weight ratio of 2:7, heat treat at 310-320℃ for 5-10 min, then cool to 50-55℃ at a rate of 2-5℃ / min and hold to obtain sheet graphene-modified zinc oxide whisker agent.

[0015] S04: Add 5-10 parts of sheet graphene and zinc oxide whisker agent to 15-20 parts of conditioning base solution, then add 1-2 parts of silane coupling agent KH560, and ultrasonically disperse at 350-400W for 1-2 hours. After ultrasonic treatment, wash with water and dry to obtain the dual-effect agent with doped whiskers.

[0016] Preferably, the mixed acid solution is prepared by citric acid, oxalic acid and deionized water in a weight ratio of 2:2:5.

[0017] Preferably, the lanthanum chloride solution has a mass fraction of 4-7%; the sodium dodecyl sulfate solution has a mass fraction of 10-15%; and the phosphate buffer solution has a pH value of 5.0.

[0018] Preferably, the modification method of the modified sheet graphene is as follows:

[0019] The sheet-like graphene was placed in a proton irradiation chamber and irradiated for 20-25 minutes at an irradiation power of 300-350W. After irradiation, the irradiant was obtained.

[0020] Add 5-8 parts of irradiant to 15-20 parts of ethanol, then add 2-5 parts of glycolic acid, 1-3 parts of diethanolamine, and 0.25-0.35 parts of sodium lignosulfonate. Stir the reaction mixture. After stirring, wash with water and dry to obtain modified sheet graphene.

[0021] Preferably, the conditions for the stirring reaction treatment are: stirring at 55-60℃ for 1-2 hours and stirring speed of 350-450 r / min.

[0022] Preferably, the method for preparing the coordinating reinforcing agent is as follows:

[0023] S11: Place 5-10 parts of nano-silica in 10-15 parts of 5% potassium permanganate solution and stir thoroughly. Wash with water and dry to obtain nano-silica modifier.

[0024] S12: Mix 4-7 parts of 10% sodium alginate solution, 1-3 parts of 2% hydrochloric acid solution and 1-2 parts of 5% yttrium nitrate solution to obtain the impregnating agent.

[0025] The nano-silica modifier is preheated at 50-55℃ for 10-15 minutes. The preheated nano-silica modifier and impregnation agent are then impregnated at a weight ratio of 1:5. After impregnation, the mixture is filtered and dried to obtain the coordinating reinforcing agent.

[0026] Preferably, the immersion treatment conditions are: immersion treatment under high pressure of 10-15 Ma, and immersion time of 1-2 hours.

[0027] This invention also provides a method for preparing a flame-retardant and antistatic coating, comprising the following steps:

[0028] The flame retardant, epoxy resin, solvent, dual-effect agent of doped whiskers, synergistic reinforcing agent, and hydroxymethyl cellulose are first mixed and stirred evenly, and finally an isocyanate curing agent is added. The mixture is then placed at 40-45°C for 1-2 hours to obtain the flame retardant and antistatic coating of the present invention.

[0029] Compared with the prior art, the present invention has the following beneficial effects:

[0030] This invention relates to a flame-retardant and antistatic coating made from epoxy resin, hydroxymethyl cellulose, flame retardant, isocyanate curing agent and solvent, a dual-effect agent with doped whiskers, and a synergistic reinforcing agent. The coating exhibits excellent antistatic and flame-retardant properties, with synergistic improvements in both properties. Simultaneously, the product demonstrates significant improvement in washability and stability. The synergistic effect of the dual-effect agent with doped whiskers further enhances the product's performance. The dual-effect agent with doped whiskers uses zinc oxide whiskers as a matrix, distributing within the matrix to provide a foundation for interfacial connectivity between raw materials. The whiskers are preheated in a mixed acid solution at 110-120°C for 5-10 minutes to optimize their activity and dispersibility. Synergistic effects are achieved through the modification of sheet-like graphene. The sheet-like structure of the graphene, supported by the whisker structure, is interwoven within the system, improving the flame-retardant and conductive properties, as well as the overall stability of the system. Lanthanum chloride solution and dodecyl sulfide are used in the coating. A matrix agent composed of sodium alginate solution, phosphate buffer solution, and nano-silica sol enhances the synergistic effect between modified sheet graphene and zinc oxide whiskers. Simultaneously, the addition of silane coupling agent KH560 enhances the interfacial compatibility between the doped whiskers and epoxy resin raw materials, improving the system's performance. Modified sheet graphene, obtained by proton irradiation and synergistic formulation with glycolic acid, diethanolamine, and sodium lignosulfonate, exhibits enhanced synergistic effects with zinc oxide whiskers, thus improving the product's antistatic and flame-retardant properties. The reinforcing agent, nano-silica treated with potassium permanganate solution, optimizes its activity. Further enhancement is achieved through impregnation with a solution composed of sodium alginate, hydrochloric acid, and yttrium nitrate, resulting in a further enhanced synergistic effect between the reinforcing agent and the doped whiskers. The product system's antistatic, flame-retardant, and washability properties are significantly improved. Detailed Implementation

[0031] The technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to specific examples. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.

[0032] This embodiment provides a flame-retardant and antistatic coating, which comprises the following raw materials in parts by weight:

[0033] 25-30 parts epoxy resin, 20-25 parts solvent, 10-15 parts dual-effect agent with doped whiskers, 4-8 parts coordinating reinforcing agent, 3-6 parts hydroxymethyl cellulose, 4-8 parts flame retardant, and 3-5 parts isocyanate curing agent.

[0034] The flame-retardant and antistatic coating of this embodiment comprises the following raw materials in parts by weight:

[0035] 27.5 parts epoxy resin, 22.5 parts solvent, 12.5 parts dual-effect agent with doped whiskers, 6 parts coordinating reinforcing agent, 4.5 parts hydroxymethyl cellulose, 6 parts flame retardant, and 4 parts isocyanate curing agent.

[0036] In this embodiment, the isocyanate curing agent is one of Bayhydur and XP2655; the solvent is xylene; and the flame retardant is a mixture of ammonium polyphosphate, melamine, and pentaerythritol in a weight ratio of 2:2:1.

[0037] The preparation method of the doped whisker dual-effect agent in this embodiment is as follows:

[0038] S01: First, place the zinc oxide whiskers in a mixed acid solution with a volume of 4-6 times the total volume of the zinc oxide whiskers and stir evenly. Then wash with water, dry, preheat at 110-120℃ for 5-10 minutes, and then air cool to room temperature to obtain pretreated zinc oxide whiskers.

[0039] SO2: Add 2-5 parts of lanthanum chloride solution to 10-15 parts of sodium dodecyl sulfate solution, then add 1-3 parts of phosphate buffer solution and 2-5 parts of nano-silica sol, stir thoroughly to obtain the conditioning base solution;

[0040] S03: Mix modified sheet graphene and pretreated zinc oxide whiskers at a weight ratio of 2:7, heat treat at 310-320℃ for 5-10 min, then cool to 50-55℃ at a rate of 2-5℃ / min and hold to obtain sheet graphene-modified zinc oxide whisker agent.

[0041] S04: Add 5-10 parts of sheet graphene and zinc oxide whisker agent to 15-20 parts of conditioning base solution, then add 1-2 parts of silane coupling agent KH560, and ultrasonically disperse at 350-400W for 1-2 hours. After ultrasonic treatment, wash with water and dry to obtain the dual-effect agent with doped whiskers.

[0042] The mixed acid solution in this embodiment is prepared by mixing citric acid, oxalic acid and deionized water in a weight ratio of 2:2:5.

[0043] In this embodiment, the lanthanum chloride solution has a mass fraction of 4-7%; the sodium dodecyl sulfate solution has a mass fraction of 10-15%; and the phosphate buffer solution has a pH value of 5.0.

[0044] The modification method of the modified sheet graphene in this embodiment is as follows:

[0045] The sheet-like graphene was placed in a proton irradiation chamber and irradiated for 20-25 minutes at an irradiation power of 300-350W. After irradiation, the irradiant was obtained.

[0046] Add 5-8 parts of irradiant to 15-20 parts of ethanol, then add 2-5 parts of glycolic acid, 1-3 parts of diethanolamine, and 0.25-0.35 parts of sodium lignosulfonate. Stir the reaction mixture. After stirring, wash with water and dry to obtain modified sheet graphene.

[0047] The conditions for the stirring reaction in this embodiment are: stirring at 55-60℃ for 1-2 hours and stirring speed of 350-450 r / min.

[0048] The preparation method of the coordinating reinforcing agent in this embodiment:

[0049] S11: Place 5-10 parts of nano-silica in 10-15 parts of 5% potassium permanganate solution and stir thoroughly. Wash with water and dry to obtain nano-silica modifier.

[0050] S12: Mix 4-7 parts of 10% sodium alginate solution, 1-3 parts of 2% hydrochloric acid solution and 1-2 parts of 5% yttrium nitrate solution to obtain the impregnating agent.

[0051] The nano-silica modifier is preheated at 50-55℃ for 10-15 minutes. The preheated nano-silica modifier and impregnation agent are then impregnated at a weight ratio of 1:5. After impregnation, the mixture is filtered and dried to obtain the coordinating reinforcing agent.

[0052] The immersion treatment conditions in this embodiment are: immersion treatment under high pressure of 10-15 Ma, and immersion time of 1-2 hours.

[0053] The preparation method of the flame-retardant and antistatic coating in this embodiment includes the following steps:

[0054] The flame retardant, epoxy resin, solvent, dual-effect agent of doped whiskers, synergistic reinforcing agent, and hydroxymethyl cellulose are first mixed and stirred evenly, and finally an isocyanate curing agent is added. The mixture is then placed at 40-45°C for 1-2 hours to obtain the flame retardant and antistatic coating of the present invention.

[0055] Example 1.

[0056] This embodiment provides a flame-retardant and antistatic coating, which comprises the following raw materials in parts by weight:

[0057] 25 parts epoxy resin, 20 parts solvent, 10 parts dual-effect agent with doped whiskers, 4 parts coordinating reinforcing agent, 3 parts hydroxymethyl cellulose, 4 parts flame retardant, and 3 parts isocyanate curing agent.

[0058] In this embodiment, the isocyanate curing agent is Bayhydur; the solvent is xylene; and the flame retardant is a mixture of ammonium polyphosphate, melamine, and pentaerythritol in a weight ratio of 2:2:1.

[0059] The preparation method of the doped whisker dual-effect agent in this embodiment is as follows:

[0060] S01: First, place the zinc oxide whiskers in a mixed acid solution with a volume of 4 times the total volume of the zinc oxide whiskers and stir evenly. Then wash with water, dry, preheat at 110℃ for 5 minutes, and then air cool to room temperature to obtain pretreated zinc oxide whiskers.

[0061] SO2: Add 2 parts of lanthanum chloride solution to 10 parts of sodium dodecyl sulfate solution, then add 1 part of phosphate buffer solution and 2 parts of nano silica sol, stir thoroughly to obtain the conditioning base solution;

[0062] S03: Modified sheet graphene and pretreated zinc oxide whiskers are mixed at a weight ratio of 2:7, heat-treated at 310℃ for 5 min, and then cooled to 50℃ at a rate of 2℃ / min and kept at the temperature to obtain sheet graphene-modified zinc oxide whisker agent.

[0063] S04: Add 5 parts of sheet graphene and zinc oxide whisker agent to 15 parts of conditioning base liquid, then add 1 part of silane coupling agent KH560, and ultrasonically disperse at 350W for 1 hour. After ultrasonic treatment, wash with water and dry to obtain a dual-effect agent with doped whiskers.

[0064] The mixed acid solution in this embodiment is prepared by mixing citric acid, oxalic acid and deionized water in a weight ratio of 2:2:5.

[0065] In this embodiment, the lanthanum chloride solution has a mass fraction of 4%; the sodium dodecyl sulfate solution has a mass fraction of 10%; and the phosphate buffer solution has a pH value of 5.0.

[0066] The modification method of the modified sheet graphene in this embodiment is as follows:

[0067] The sheet-like graphene was placed in a proton irradiation chamber and irradiated for 20 minutes at a power of 300W. After irradiation, the irradiant was obtained.

[0068] Five parts of irradiant were added to 15 parts of ethanol, followed by two parts of glycolic acid, one part of diethanolamine, and 0.25 parts of sodium lignosulfonate. The mixture was stirred and reacted. After stirring, the mixture was washed with water and dried to obtain modified sheet graphene.

[0069] The conditions for the stirring reaction in this embodiment are: stirring at 55°C for 1 hour and stirring speed of 350 r / min.

[0070] The preparation method of the coordinating reinforcing agent in this embodiment:

[0071] S11: Place 5 parts of nano-silica in 10 parts of 5% potassium permanganate solution and stir thoroughly. Wash with water and dry to obtain nano-silica modifier.

[0072] S12: Mix 4 parts of 10% sodium alginate solution, 1 part of 2% hydrochloric acid solution and 1 part of 5% yttrium nitrate solution to obtain the impregnating agent;

[0073] The nano-silica modifier was preheated at 50°C for 10 minutes. The preheated nano-silica modifier and the impregnation agent were then impregnated at a weight ratio of 1:5. After impregnation, the mixture was filtered and dried to obtain the coordinating reinforcing agent.

[0074] The immersion treatment conditions in this embodiment are: immersion treatment under a high pressure of 1 MPa for 1 hour.

[0075] The preparation method of the flame-retardant and antistatic coating in this embodiment includes the following steps:

[0076] The flame retardant, epoxy resin, solvent, dual-effect agent of doped whiskers, synergistic reinforcing agent, and hydroxymethyl cellulose are first mixed and stirred evenly, and finally an isocyanate curing agent is added. The mixture is then placed at 40°C for 1 hour to obtain the flame retardant and antistatic coating of the present invention.

[0077] Example 2.

[0078] This embodiment provides a flame-retardant and antistatic coating, which comprises the following raw materials in parts by weight:

[0079] 30 parts epoxy resin, 25 parts solvent, 15 parts dual-effect agent with doped whiskers, 8 parts coordinating reinforcing agent, 6 parts hydroxymethyl cellulose, 8 parts flame retardant, and 5 parts isocyanate curing agent.

[0080] In this embodiment, the isocyanate curing agent is XP2655; the solvent is xylene; and the flame retardant is a mixture of ammonium polyphosphate, melamine, and pentaerythritol in a weight ratio of 2:2:1.

[0081] The preparation method of the doped whisker dual-effect agent in this embodiment is as follows:

[0082] S01: First, place the zinc oxide whiskers in a mixed acid solution with a volume of 6 times the total volume of the zinc oxide whiskers and stir evenly. Then wash with water, dry, preheat at 120°C for 10 minutes, and then air cool to room temperature to obtain pretreated zinc oxide whiskers.

[0083] S02: Add 5 parts of lanthanum chloride solution to 15 parts of sodium dodecyl sulfate solution, then add 3 parts of phosphate buffer solution and 5 parts of nano silica sol, stir thoroughly to obtain the conditioning base solution;

[0084] S03: Modified sheet graphene and pretreated zinc oxide whiskers are mixed at a weight ratio of 2:7, heat-treated at 320℃ for 10 min, and then cooled to 55℃ at a rate of 5℃ / min and kept at the temperature to obtain sheet graphene-modified zinc oxide whisker agent.

[0085] S04: Add 10 parts of sheet graphene and zinc oxide whisker agent to 20 parts of conditioning base liquid, then add 2 parts of silane coupling agent KH560, and ultrasonically disperse at 400W ultrasonic power for 1-2 hours. After ultrasonic treatment, wash with water and dry to obtain a dual-effect agent with doped whiskers.

[0086] The mixed acid solution in this embodiment is prepared by mixing citric acid, oxalic acid and deionized water in a weight ratio of 2:2:5.

[0087] In this embodiment, the lanthanum chloride solution has a mass fraction of 7%; the sodium dodecyl sulfate solution has a mass fraction of 15%; and the phosphate buffer solution has a pH value of 5.0.

[0088] The modification method of the modified sheet graphene in this embodiment is as follows:

[0089] The sheet-like graphene was placed in a proton irradiation chamber and irradiated for 25 minutes at a power of 350W. After irradiation, the irradiant was obtained.

[0090] Eight parts of irradiant were added to 20 parts of ethanol, followed by five parts of glycolic acid, three parts of diethanolamine, and 0.35 parts of sodium lignosulfonate. The mixture was stirred and reacted. After stirring, the mixture was washed with water and dried to obtain modified sheet graphene.

[0091] The conditions for the stirring reaction in this embodiment are: stirring at 60°C for 2 hours and stirring speed of 450 r / min.

[0092] The preparation method of the coordinating reinforcing agent in this embodiment:

[0093] S11: Place 10 parts of nano-silica in 15 parts of 5% potassium permanganate solution and stir thoroughly. Wash with water and dry to obtain nano-silica modifier.

[0094] S12: Mix 7 parts of 10% sodium alginate solution, 3 parts of 2% hydrochloric acid solution and 2 parts of 5% yttrium nitrate solution to obtain the impregnating agent;

[0095] The nano-silica modifier was preheated at 55℃ for 15 minutes. The preheated nano-silica modifier and the impregnation agent were then impregnated at a weight ratio of 1:5. After impregnation, the mixture was filtered and dried to obtain the coordinating reinforcing agent.

[0096] The immersion treatment conditions in this embodiment are: immersion treatment under a high pressure of 15 Ma for 2 hours.

[0097] The preparation method of the flame-retardant and antistatic coating in this embodiment includes the following steps:

[0098] The flame retardant, epoxy resin, solvent, dual-effect agent for doped whiskers, synergistic reinforcing agent, and hydroxymethyl cellulose are first mixed and stirred evenly, and finally an isocyanate curing agent is added. The mixture is then placed at 45°C for 2 hours to obtain the flame retardant and antistatic coating of the present invention.

[0099] Example 3.

[0100] This embodiment provides a flame-retardant and antistatic coating, which comprises the following raw materials in parts by weight:

[0101] 27.5 parts epoxy resin, 22.5 parts solvent, 12.5 parts dual-effect agent with doped whiskers, 6 parts coordinating reinforcing agent, 4.5 parts hydroxymethyl cellulose, 6 parts flame retardant, and 4 parts isocyanate curing agent.

[0102] In this embodiment, the isocyanate curing agent is XP2655; the solvent is xylene; and the flame retardant is a mixture of ammonium polyphosphate, melamine, and pentaerythritol in a weight ratio of 2:2:1.

[0103] The preparation method of the doped whisker dual-effect agent in this embodiment is as follows:

[0104] S01: First, place the zinc oxide whiskers in a mixed acid solution with a volume of 5 times the total volume of the zinc oxide whiskers and stir evenly. Then wash with water, dry, preheat at 115℃ for 7.5 min, and then air cool to room temperature to obtain pretreated zinc oxide whiskers.

[0105] SO2: Add 3.5 parts of lanthanum chloride solution to 12.5 parts of sodium dodecyl sulfate solution, then add 2 parts of phosphate buffer solution and 3.5 parts of nano-silica sol, stir thoroughly to obtain the conditioning base solution;

[0106] S03: Modified sheet graphene and pretreated zinc oxide whiskers are mixed at a weight ratio of 2:7, heat-treated at 315℃ for 7.5 min, and then cooled to 52.5℃ at a rate of 3.5℃ / min and held at the temperature to obtain sheet graphene-modified zinc oxide whisker agent.

[0107] S04: 7.5 parts of sheet graphene and zinc oxide whisker agent were added to 17.5 parts of conditioning base solution, followed by 1.5 parts of silane coupling agent KH560. The mixture was ultrasonically dispersed at 370W for 1.5 hours. After ultrasonic treatment, the mixture was washed with water and dried to obtain a dual-effect agent with doped whiskers.

[0108] The mixed acid solution in this embodiment is prepared by mixing citric acid, oxalic acid and deionized water in a weight ratio of 2:2:5.

[0109] In this embodiment, the lanthanum chloride solution has a mass fraction of 5.5%; the sodium dodecyl sulfate solution has a mass fraction of 12.5%; and the phosphate buffer solution has a pH value of 5.0.

[0110] The modification method of the modified sheet graphene in this embodiment is as follows:

[0111] The sheet-like graphene was placed in a proton irradiation chamber and irradiated for 22.5 minutes at an irradiation power of 320W. After irradiation, the irradiant was obtained.

[0112] 6.5 parts of irradiant were added to 17.5 parts of ethanol, followed by 3.5 parts of glycolic acid, 2 parts of diethanolamine, and 0.30 parts of sodium lignosulfonate. The mixture was stirred and reacted. After stirring, the mixture was washed with water and dried to obtain modified sheet graphene.

[0113] The conditions for the stirring reaction in this embodiment are: stirring at 57.5℃ for 1.5 hours and stirring speed of 400 r / min.

[0114] The preparation method of the coordinating reinforcing agent in this embodiment:

[0115] S11: Place 7.5 parts of nano-silica in 12.5 parts of a 5% potassium permanganate solution and stir thoroughly. Wash with water and dry to obtain nano-silica modifier.

[0116] S12: Mix 5.5 parts of 10% sodium alginate solution, 2 parts of 2% hydrochloric acid solution, and 1.5 parts of 5% yttrium nitrate solution to obtain the impregnating agent;

[0117] The nano-silica modifier was preheated at 52℃ for 12.5 min. The preheated nano-silica modifier and the impregnation agent were then impregnated at a weight ratio of 1:5. After impregnation, the mixture was filtered and dried to obtain the coordinating reinforcing agent.

[0118] The immersion treatment conditions in this embodiment are: immersion treatment under a high pressure of 12.5 Ma and an immersion time of 1.5 h.

[0119] The preparation method of the flame-retardant and antistatic coating in this embodiment includes the following steps:

[0120] The flame retardant, epoxy resin, solvent, dual-effect agent of doped whiskers, synergistic reinforcing agent, and hydroxymethyl cellulose are first mixed and stirred evenly, and finally an isocyanate curing agent is added. The mixture is then placed at 42.5°C for 1.5 hours to obtain the flame retardant and antistatic coating of the present invention.

[0121] Comparative Example 1.

[0122] Unlike Example 3, this is a dual-effect agent without the addition of doped whiskers.

[0123] Comparative Example 2.

[0124] Unlike Example 3, the SO1 step was not used in the preparation of the doped whisker dual-effect agent.

[0125] Comparative Example 3.

[0126] Unlike Example 3, the preparation of the doped whisker dual-effect agent did not involve heat treatment at 315°C for 7.5 min followed by cooling to 52.5°C at a rate of 3.5°C / min and holding at that temperature.

[0127] Comparative Example 4.

[0128] Unlike Example 3, the preparation of the doped whisker dual-effect agent did not use modified sheet graphene treatment.

[0129] Comparative Example 5.

[0130] Unlike Example 3, lanthanum chloride solution was not added in the preparation of the conditioning base solution.

[0131] Comparative Example 6.

[0132] Unlike Example 3, no nano-silica sol was added in the preparation of the conditioning base solution.

[0133] Comparative Example 7.

[0134] Unlike Example 3, no coordinating reinforcing agent was added.

[0135] Comparative Example 8.

[0136] Unlike Example 3, no impregnation agent was used in the preparation of the coordinating reinforcing agent.

[0137] Comparative Example 9.

[0138] Unlike Example 3, yttrium nitrate solution was not added during the preparation of the impregnating agent.

[0139] The performance test and measurement results of the products in Examples 1-3 and Comparative Examples 1-9 under normal conditions and after 2000 washes are as follows:

[0140]

[0141]

[0142] From Examples 1-3 and Comparative Examples 1-9, it was found that...

[0143] The product of Embodiment 3 of the present invention has excellent surface resistance and flame retardancy time. The flame retardant and antistatic properties of the product can be improved in a coordinated manner. At the same time, the performance stability of the product remains stable under the condition of 2000 washes.

[0144] As can be seen from Comparative Examples 1-6 and Example 3, the surface resistivity and flame retardancy of the dual-effect agent without added whiskers deteriorated significantly under normal conditions and after 2000 washes. Furthermore, the absence of the SO1 step in the preparation of the dual-effect agent with added whiskers, the absence of heat treatment at 315°C for 7.5 min followed by cooling to 52.5°C at a rate of 3.5°C / min and holding treatment, the absence of modified sheet graphene treatment in the preparation of the dual-effect agent with added whiskers, the absence of lanthanum chloride solution in the preparation of the base liquid, and the absence of nano-silica sol all contributed to the deterioration of the product's performance.

[0145] The product exhibits the most significant performance when the base liquid prepared by the method of this invention is combined with the modified sheet graphene treatment of this invention and the doped whisker dual-effect agent prepared by the specific process of this invention. Meanwhile, the preparation of the doped whisker dual-effect agent does not employ the modified sheet graphene treatment, which has the greatest impact on the preparation of the doped whisker dual-effect agent. The modified sheet graphene plays an important role in the performance of the product.

[0146] As can be seen from Comparative Examples 7-9, Comparative Example 1 and Example 3, the performance of the products tends to deteriorate when no coordinating reinforcing agent is added, no impregnation agent is used in the preparation of the coordinating reinforcing agent, and no yttrium nitrate solution is added in the preparation of the impregnation agent. The coordinating reinforcing agent prepared by the method of the present invention, combined with the doped whisker dual-effect agent of the present invention, has the most significant synergistic effect and the most obvious performance effect of the product.

[0147] In this invention, the performance of the product tends to deteriorate significantly when neither of the two-effect agents (either the coordinating reinforcing agent or the doped whiskers) is added. Only by using a combination of both agents to achieve a synergistic effect can the product performance be most significantly improved.

[0148] Based on the above tests, this invention found that modified sheet graphene has a significant impact on the performance of the product. Based on this, this invention further explores its effects.

[0149] The modification method for modified sheet graphene is as follows:

[0150] The sheet-like graphene was placed in a proton irradiation chamber and irradiated for 22.5 minutes at an irradiation power of 320W. After irradiation, the irradiant was obtained.

[0151] 6.5 parts of irradiant were added to 17.5 parts of ethanol, followed by 3.5 parts of glycolic acid, 2 parts of diethanolamine, and 0.30 parts of sodium lignosulfonate. The mixture was stirred and reacted. After stirring, the mixture was washed with water and dried to obtain modified sheet graphene.

[0152] The conditions for the stirring reaction in this embodiment are: stirring at 57.5℃ for 1.5 hours and stirring speed of 400 r / min.

[0153] Experimental Example 1.

[0154] Same as Example 3, except that no irradiation treatment was used in the preparation of the modified sheet graphene.

[0155] Experimental Example 2.

[0156] Same as Example 3, except that glycolic acid was not added in the preparation of the modified sheet graphene.

[0157] Experimental Example 3.

[0158] Same as Example 3, except that sodium lignosulfonate was not added in the preparation of the modified sheet graphene.

[0159] Experimental Example 4.

[0160] Same as Example 3, except that diethanolamine was not added in the preparation of the modified sheet graphene.

[0161]

[0162] As can be seen from Experiments 1-4, the performance of the modified sheet graphene showed the greatest trend when diethanolamine was not added during preparation. Diethanolamine plays a dominant role in the preparation of modified sheet graphene. The performance of the modified sheet graphene deteriorated when glycolic acid, sodium lignosulfonate, or irradiation treatment were not used during preparation. Only the modified sheet graphene prepared by the specific method of this invention showed the most significant performance effect. When other methods were used, the performance effect of the product was not as obvious as that of this invention.

[0163] It will be apparent to those skilled in the art that the present invention is not limited to the details of the exemplary embodiments described above, and that the invention can be implemented in other specific forms without departing from the spirit or essential characteristics of the invention. Therefore, the embodiments should be considered in all respects as exemplary and non-limiting, and the scope of the invention is defined by the appended claims rather than the foregoing description. Thus, it is intended that all variations falling within the meaning and scope of equivalents of the claims be included within the present invention.

[0164] Furthermore, it should be understood that although this specification describes embodiments, not every embodiment contains only one independent technical solution. This narrative style is merely for clarity. Those skilled in the art should consider the specification as a whole, and the technical solutions in each embodiment can also be appropriately combined to form other embodiments that can be understood by those skilled in the art.

Claims

1. A flame-retardant and antistatic coating, characterized in that, The flame-retardant and antistatic coating comprises the following raw materials in parts by weight: 25-30 parts epoxy resin, 20-25 parts solvent, 10-15 parts dual-effect agent with doped whiskers, 4-8 parts coordinating reinforcing agent, 3-6 parts hydroxymethyl cellulose, 4-8 parts flame retardant, and 3-5 parts isocyanate curing agent. The preparation method of the doped whisker dual-effect agent is as follows: S01: First, place the zinc oxide whiskers in a mixed acid solution with a volume of 4-6 times the total volume of the zinc oxide whiskers and stir evenly. Then wash with water, dry, preheat at 110-120℃ for 5-10 minutes, and then air cool to room temperature to obtain pretreated zinc oxide whiskers. SO2: Add 2-5 parts of lanthanum chloride solution to 10-15 parts of sodium dodecyl sulfate solution, then add 1-3 parts of phosphate buffer solution and 2-5 parts of nano silica sol, stir thoroughly to obtain the conditioning base solution; S03: Mix modified sheet graphene and pretreated zinc oxide whiskers at a weight ratio of 2:7, heat treat at 310-320℃ for 5-10 min, then cool to 50-55℃ at a rate of 2-5℃ / min and hold to obtain sheet graphene-modified zinc oxide whisker agent. S04: Add 5-10 parts of sheet graphene and zinc oxide whisker agent to 15-20 parts of conditioning base liquid, then add 1-2 parts of silane coupling agent KH560, and ultrasonically disperse at 350-400W ultrasonic power for 1-2 hours. After ultrasonic treatment, wash with water and dry to obtain the dual-effect agent with doped whiskers. The modification method for the modified sheet graphene is as follows: The sheet-like graphene was placed in a proton irradiation chamber and irradiated for 20-25 minutes at an irradiation power of 300-350W. After irradiation, the irradiant was obtained. Add 5-8 parts of irradiant to 15-20 parts of ethanol, then add 2-5 parts of glycolic acid, 1-3 parts of diethanolamine, and 0.25-0.35 parts of sodium lignosulfonate. Stir the reaction mixture. After stirring, wash with water and dry to obtain modified sheet graphene. The preparation method of the synergistic reinforcing agent: S11: Place 5-10 parts of nano-silica in 10-15 parts of a 5% potassium permanganate solution and stir thoroughly. Wash with water and dry to obtain nano-silica modifier. S12: Mix 4-7 parts of 10% sodium alginate solution, 1-3 parts of 2% hydrochloric acid solution and 1-2 parts of 5% yttrium nitrate solution to obtain an impregnating agent; The nano-silica modifier is preheated at 50-55℃ for 10-15 minutes. The preheated nano-silica modifier and impregnation agent are then impregnated at a weight ratio of 1:

5. After impregnation, the mixture is filtered and dried to obtain the coordinating reinforcing agent.

2. The flame-retardant and antistatic coating according to claim 1, characterized in that, The flame-retardant and antistatic coating comprises the following raw materials in parts by weight: 27.5 parts epoxy resin, 22.5 parts solvent, 12.5 parts dual-effect agent with doped whiskers, 6 parts coordinating reinforcing agent, 4.5 parts hydroxymethyl cellulose, 6 parts flame retardant, and 4 parts isocyanate curing agent.

3. The flame-retardant and antistatic coating according to claim 1, characterized in that, The isocyanate curing agent is one of Bayhydur and XP2655; the solvent is xylene; and the flame retardant is a mixture of ammonium polyphosphate, melamine, and pentaerythritol in a weight ratio of 2:2:

1.

4. The flame-retardant and antistatic coating according to claim 1, characterized in that, The mixed acid solution is prepared by citric acid, oxalic acid and deionized water in a weight ratio of 2:2:

5. The lanthanum chloride solution has a mass fraction of 4-7%; the sodium dodecyl sulfate solution has a mass fraction of 10-15%; and the phosphate buffer solution has a pH of 5.

0.

5. The flame-retardant and antistatic coating according to claim 1, characterized in that, The conditions for the stirring reaction treatment are: stirring at 55-60℃ for 1-2 hours, with a stirring speed of 350-450 r / min.

6. The flame-retardant and antistatic coating according to claim 5, characterized in that, The immersion treatment conditions are: immersion treatment under high pressure of 10-15 Ma, and immersion time of 1-2 hours.

7. A method for preparing a flame-retardant and antistatic coating as described in any one of claims 1-6, characterized in that, Includes the following steps: The flame retardant, epoxy resin, solvent, dual-effect agent of doped whiskers, synergistic reinforcing agent, and hydroxymethyl cellulose are first mixed and stirred evenly, and finally an isocyanate curing agent is added. The mixture is then placed at 40-45°C for 1-2 hours to obtain the flame retardant and antistatic coating of the present invention.

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