CN117844340A - Flame-retardant antistatic coating and preparation method thereof - Google Patents
Flame-retardant antistatic coating and preparation method thereof Download PDFInfo
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- CN117844340A CN117844340A CN202311805059.3A CN202311805059A CN117844340A CN 117844340 A CN117844340 A CN 117844340A CN 202311805059 A CN202311805059 A CN 202311805059A CN 117844340 A CN117844340 A CN 117844340A
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- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 title claims abstract description 69
- 239000003063 flame retardant Substances 0.000 title claims abstract description 69
- 238000000576 coating method Methods 0.000 title claims abstract description 41
- 239000011248 coating agent Substances 0.000 title claims abstract description 39
- 238000002360 preparation method Methods 0.000 title claims description 42
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 101
- 239000012744 reinforcing agent Substances 0.000 claims abstract description 39
- 238000005406 washing Methods 0.000 claims abstract description 31
- 239000012948 isocyanate Substances 0.000 claims abstract description 26
- 150000002513 isocyanates Chemical class 0.000 claims abstract description 26
- 239000002904 solvent Substances 0.000 claims abstract description 26
- 239000003822 epoxy resin Substances 0.000 claims abstract description 21
- 229920000647 polyepoxide Polymers 0.000 claims abstract description 21
- 229920003063 hydroxymethyl cellulose Polymers 0.000 claims abstract description 18
- 229940031574 hydroxymethyl cellulose Drugs 0.000 claims abstract description 18
- 239000002994 raw material Substances 0.000 claims abstract description 12
- 239000000243 solution Substances 0.000 claims description 85
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 78
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 62
- 229910021389 graphene Inorganic materials 0.000 claims description 59
- 238000003756 stirring Methods 0.000 claims description 59
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 50
- 239000011787 zinc oxide Substances 0.000 claims description 39
- 238000011282 treatment Methods 0.000 claims description 38
- 238000001035 drying Methods 0.000 claims description 31
- 239000005543 nano-size silicon particle Substances 0.000 claims description 26
- 235000012239 silicon dioxide Nutrition 0.000 claims description 25
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 23
- AEMRFAOFKBGASW-UHFFFAOYSA-N Glycolic acid Chemical compound OCC(O)=O AEMRFAOFKBGASW-UHFFFAOYSA-N 0.000 claims description 20
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 18
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 18
- 238000007654 immersion Methods 0.000 claims description 18
- 238000002156 mixing Methods 0.000 claims description 18
- 239000003607 modifier Substances 0.000 claims description 18
- ICAKDTKJOYSXGC-UHFFFAOYSA-K lanthanum(iii) chloride Chemical compound Cl[La](Cl)Cl ICAKDTKJOYSXGC-UHFFFAOYSA-K 0.000 claims description 15
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 14
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 14
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 14
- 238000006243 chemical reaction Methods 0.000 claims description 14
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 claims description 13
- 239000002253 acid Substances 0.000 claims description 13
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical group CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims description 12
- 238000001816 cooling Methods 0.000 claims description 12
- ZBCBWPMODOFKDW-UHFFFAOYSA-N diethanolamine Chemical compound OCCNCCO ZBCBWPMODOFKDW-UHFFFAOYSA-N 0.000 claims description 11
- YDEXUEFDPVHGHE-GGMCWBHBSA-L disodium;(2r)-3-(2-hydroxy-3-methoxyphenyl)-2-[2-methoxy-4-(3-sulfonatopropyl)phenoxy]propane-1-sulfonate Chemical compound [Na+].[Na+].COC1=CC=CC(C[C@H](CS([O-])(=O)=O)OC=2C(=CC(CCCS([O-])(=O)=O)=CC=2)OC)=C1O YDEXUEFDPVHGHE-GGMCWBHBSA-L 0.000 claims description 10
- NGDQQLAVJWUYSF-UHFFFAOYSA-N 4-methyl-2-phenyl-1,3-thiazole-5-sulfonyl chloride Chemical compound S1C(S(Cl)(=O)=O)=C(C)N=C1C1=CC=CC=C1 NGDQQLAVJWUYSF-UHFFFAOYSA-N 0.000 claims description 9
- 238000010438 heat treatment Methods 0.000 claims description 8
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 claims description 8
- IXPNQXFRVYWDDI-UHFFFAOYSA-N 1-methyl-2,4-dioxo-1,3-diazinane-5-carboximidamide Chemical compound CN1CC(C(N)=N)C(=O)NC1=O IXPNQXFRVYWDDI-UHFFFAOYSA-N 0.000 claims description 7
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 7
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 7
- 239000007853 buffer solution Substances 0.000 claims description 7
- 238000001802 infusion Methods 0.000 claims description 7
- 238000002715 modification method Methods 0.000 claims description 7
- 239000012286 potassium permanganate Substances 0.000 claims description 7
- 239000000661 sodium alginate Substances 0.000 claims description 7
- 235000010413 sodium alginate Nutrition 0.000 claims description 7
- 229940005550 sodium alginate Drugs 0.000 claims description 7
- 239000004114 Ammonium polyphosphate Substances 0.000 claims description 6
- 229920000877 Melamine resin Polymers 0.000 claims description 6
- 235000019826 ammonium polyphosphate Nutrition 0.000 claims description 6
- 229920001276 ammonium polyphosphate Polymers 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 claims description 6
- 238000000034 method Methods 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 6
- 235000006408 oxalic acid Nutrition 0.000 claims description 6
- WXZMFSXDPGVJKK-UHFFFAOYSA-N pentaerythritol Chemical compound OCC(CO)(CO)CO WXZMFSXDPGVJKK-UHFFFAOYSA-N 0.000 claims description 6
- 239000008055 phosphate buffer solution Substances 0.000 claims description 6
- 230000001105 regulatory effect Effects 0.000 claims description 6
- 238000000967 suction filtration Methods 0.000 claims description 6
- 238000001132 ultrasonic dispersion Methods 0.000 claims description 6
- 230000000694 effects Effects 0.000 abstract description 17
- 230000001976 improved effect Effects 0.000 abstract description 7
- 230000000052 comparative effect Effects 0.000 description 14
- 230000002195 synergetic effect Effects 0.000 description 5
- 239000011159 matrix material Substances 0.000 description 3
- 230000003068 static effect Effects 0.000 description 3
- 238000009210 therapy by ultrasound Methods 0.000 description 3
- 230000003750 conditioning effect Effects 0.000 description 2
- 230000006866 deterioration Effects 0.000 description 2
- 238000007598 dipping method Methods 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 239000002216 antistatic agent Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
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Abstract
The invention relates to the technical field of coatings, and particularly discloses a flame-retardant antistatic coating which comprises the following raw materials in parts by weight: 25-30 parts of epoxy resin, 20-25 parts of solvent, 10-15 parts of whisker-doped double-effect agent, 4-8 parts of coordination reinforcing agent, 3-6 parts of hydroxymethyl cellulose, 4-8 parts of flame retardant and 3-5 parts of isocyanate curing agent. The flame-retardant antistatic coating prepared by adopting epoxy resin, hydroxymethyl cellulose, flame retardant, isocyanate curing agent, solvent, whisker-doped double-effect agent and coordination reinforcing agent has excellent antistatic and flame-retardant properties, the properties of the epoxy resin, the flame retardant and the isocyanate curing agent and the solvent can be coordinately improved, and meanwhile, the washing resistance stability effect of the product is obvious.
Description
Technical Field
The invention relates to the technical field of coatings, in particular to a flame-retardant antistatic coating and a preparation method thereof.
Background
If static electricity is accumulated on equipment materials in a large amount, the equipment cannot be used, such as distortion of precise instruments, scrapping of electronic components and the like. The antistatic coating can not only conduct current rapidly and eliminate static charge, but also provide guarantee for the operation of equipment.
The existing antistatic coating does not have antistatic property, in order to improve the antistatic property, an antistatic agent is added to enable the antistatic coating to have an antistatic function, but the antistatic performance effect of a product is general, and in order to improve the antistatic effect, the flame retardance of the product is correspondingly reduced, so that the flame retardance and the antistatic performance of the product are difficult to coordinate and improve, the service efficiency of the product is limited, the stability of the washing resistance performance of the product is poor, and the product efficiency is further reduced.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a flame-retardant antistatic coating and a preparation method thereof, so as to solve the problems in the prior art.
The invention solves the technical problems by adopting the following technical scheme:
the invention provides a flame-retardant antistatic coating which comprises the following raw materials in parts by weight:
25-30 parts of epoxy resin, 20-25 parts of solvent, 10-15 parts of whisker-doped double-effect agent, 4-8 parts of coordination reinforcing agent, 3-6 parts of hydroxymethyl cellulose, 4-8 parts of flame retardant and 3-5 parts of isocyanate curing agent.
Preferably, the flame-retardant antistatic coating comprises the following raw materials in parts by weight:
27.5 parts of epoxy resin, 22.5 parts of solvent, 12.5 parts of whisker-doped double-effect agent, 6 parts of coordination reinforcing agent, 4.5 parts of hydroxymethyl cellulose, 6 parts of flame retardant and 4 parts of isocyanate curing agent.
Preferably, the isocyanate curing agent is one of bayhydur and XP2655; the solvent is dimethylbenzene; the flame retardant is formed by mixing ammonium polyphosphate, melamine and pentaerythritol according to a weight ratio of 2:2:1.
Preferably, the preparation method of the whisker-doped double-effect agent comprises the following steps:
s01: placing zinc oxide whisker into mixed acid solution with the total amount of 4-6 times of the zinc oxide whisker, uniformly stirring, washing with water, drying, preheating for 5-10min at 110-120 ℃, and then air-cooling to room temperature to obtain pretreated zinc oxide whisker;
s02: adding 2-5 parts of lanthanum chloride solution into 10-15 parts of sodium dodecyl sulfate solution, then adding 1-3 parts of phosphoric acid buffer solution and 2-5 parts of nano silica sol, and stirring fully to obtain a regulating base solution;
s03: uniformly mixing the modified flaky graphene and the pretreated zinc oxide whisker according to the weight ratio of 2:7, performing heat treatment at 310-320 ℃ for 5-10min, then cooling to 50-55 ℃ at the speed of 2-5 ℃/min, and preserving heat to obtain a flaky graphene blended zinc oxide whisker agent;
s04: adding 5-10 parts of flaky graphene and zinc oxide whisker agent into 15-20 parts of adjusting base solution, then adding 1-2 parts of silane coupling agent KH560, performing ultrasonic power ultrasonic dispersion treatment for 1-2 hours at 350-400W, performing ultrasonic finishing, washing with water, and drying to obtain the whisker-doped double-effect agent.
Preferably, the mixed acid solution is prepared from citric acid, oxalic acid and deionized water according to a weight ratio of 2:2:5.
Preferably, the lanthanum chloride solution has a mass fraction of 4-7%; the mass fraction of the sodium dodecyl sulfate solution is 10-15%; the pH value of the phosphate buffer solution is 5.0.
Preferably, the modification method of the modified flaky graphene comprises the following steps:
placing the flaky graphene in a proton irradiation box for irradiation for 20-25min, wherein the irradiation power is 300-350W, and obtaining an irradiation agent after the irradiation is finished;
adding 5-8 parts of an irradiator into 15-20 parts of ethanol, then adding 2-5 parts of glycolic acid, 1-3 parts of diethanolamine and 0.25-0.35 part of sodium lignin sulfonate, stirring for reaction treatment, and washing and drying after stirring is finished to obtain the modified flaky graphene.
Preferably, the conditions of the stirring reaction treatment are as follows: stirring at 55-60deg.C for 1-2 hr at a stirring speed of 350-450r/min.
Preferably, the preparation method of the coordination reinforcing agent comprises the following steps:
s11: placing 5-10 parts of nano silicon dioxide into 10-15 parts of potassium permanganate solution with mass fraction of 5%, stirring thoroughly, washing with water, and drying to obtain nano silicon dioxide modifier;
s12: uniformly stirring and mixing 4-7 parts of sodium alginate solution with the mass fraction of 10%, 1-3 parts of hydrochloric acid solution with the mass fraction of 2% and 1-2 parts of yttrium nitrate solution with the mass fraction of 5%, so as to obtain an infusion;
preheating the nano silicon dioxide modifier for 10-15min at 50-55 ℃, immersing the preheated nano silicon dioxide modifier and the immersing agent according to the weight ratio of 1:5, and carrying out suction filtration and drying after the immersing is finished to obtain the coordination reinforcing agent.
Preferably, the conditions of the immersion treatment are: the immersion treatment is carried out under high pressure of 10-15Ma, and the immersion time is 1-2h.
The invention also provides a preparation method of the flame-retardant antistatic coating, which comprises the following steps:
the flame retardant, the epoxy resin, the solvent, the whisker-doped double-effect agent, the coordination reinforcing agent and the hydroxymethyl cellulose are firstly mixed and stirred uniformly, and finally the isocyanate curing agent is added, and the mixture is placed at 40-45 ℃ for 1-2 hours, so that the flame retardant antistatic coating is obtained.
Compared with the prior art, the invention has the following beneficial effects:
the flame-retardant antistatic coating prepared by adopting epoxy resin, hydroxymethyl cellulose, flame retardant, isocyanate curing agent, solvent, whisker-doped double-effect agent and coordination reinforcing agent has excellent antistatic and flame-retardant properties, the performance of the epoxy resin, the flame retardant and the isocyanate curing agent and the solvent can be coordinately improved, and meanwhile, the washing resistance stability effect of the product is obvious; the double-effect agent doped with whisker and the coordination reinforcing agent are used for cooperation, so that the performance of the product is further enhanced; the whisker-doped double-effect agent takes zinc oxide whiskers as a matrix, the whiskers are distributed in the matrix to provide a basis for the interfacial connectivity between raw materials of a product, meanwhile, the whiskers are preheated for 5-10min at 110-120 ℃ by adopting a mixed acid solution, the activity and the dispersity of the whiskers are optimized, the flaky graphene is mutually cooperated and cooperated with the whisker-doped double-effect agent, the flaky graphene is supported by the whisker structure and is mutually cooperated, the flaky graphene is inserted into a system to provide an improved effect for the flame retardance and the electric conduction coordination of the system, the stability of the system is improved, and the synergistic effect between the modified flaky graphene and the zinc oxide whiskers is enhanced by adopting a matrix agent which is mutually harmonized by lanthanum chloride solution, sodium dodecyl sulfate solution, phosphoric acid buffer solution and nano silica sol, and meanwhile, the interfacial compatibility between the whisker-doped double-effect agent and the epoxy resin raw materials can be enhanced by adding a silane coupling agent KH560, and the performance effect of the system is improved; the modified flaky graphene is subjected to proton irradiation by graphene, and the synergistic effect of the obtained modified flaky graphene and zinc oxide whisker is enhanced by mutual harmonization and coordination improvement among glycolic acid, diethanolamine and sodium lignin sulfonate, so that the synergistic efficiency of the antistatic and flame-retardant properties of the product is enhanced, the coordination reinforcing agent adopts nano silicon dioxide to be treated by potassium permanganate solution, the activity efficiency of the product is optimized, the dipping agent formed by sodium alginate solution, hydrochloric acid solution and yttrium nitrate solution is subjected to dipping improvement treatment, and the synergistic effect of the obtained coordination reinforcing agent and the double-effect agent doped with whisker is further enhanced, and the static, flame-retardant properties and washing stability of the product system are obviously improved.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and fully with reference to the accompanying drawings, in which it is evident that the embodiments described are only some, but not all embodiments of the invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
The flame-retardant antistatic coating comprises the following raw materials in parts by weight:
25-30 parts of epoxy resin, 20-25 parts of solvent, 10-15 parts of whisker-doped double-effect agent, 4-8 parts of coordination reinforcing agent, 3-6 parts of hydroxymethyl cellulose, 4-8 parts of flame retardant and 3-5 parts of isocyanate curing agent.
The flame-retardant antistatic coating comprises the following raw materials in parts by weight:
27.5 parts of epoxy resin, 22.5 parts of solvent, 12.5 parts of whisker-doped double-effect agent, 6 parts of coordination reinforcing agent, 4.5 parts of hydroxymethyl cellulose, 6 parts of flame retardant and 4 parts of isocyanate curing agent.
The isocyanate curing agent of the embodiment is one of bayhydur and XP2655; the solvent is dimethylbenzene; the flame retardant is formed by mixing ammonium polyphosphate, melamine and pentaerythritol according to a weight ratio of 2:2:1.
The preparation method of the whisker-doped double-effect agent comprises the following steps:
s01: placing zinc oxide whisker into mixed acid solution with the total amount of 4-6 times of the zinc oxide whisker, uniformly stirring, washing with water, drying, preheating for 5-10min at 110-120 ℃, and then air-cooling to room temperature to obtain pretreated zinc oxide whisker;
s02: adding 2-5 parts of lanthanum chloride solution into 10-15 parts of sodium dodecyl sulfate solution, then adding 1-3 parts of phosphoric acid buffer solution and 2-5 parts of nano silica sol, and stirring fully to obtain a regulating base solution;
s03: uniformly mixing the modified flaky graphene and the pretreated zinc oxide whisker according to the weight ratio of 2:7, performing heat treatment at 310-320 ℃ for 5-10min, then cooling to 50-55 ℃ at the speed of 2-5 ℃/min, and preserving heat to obtain a flaky graphene blended zinc oxide whisker agent;
s04: adding 5-10 parts of flaky graphene and zinc oxide whisker agent into 15-20 parts of adjusting base solution, then adding 1-2 parts of silane coupling agent KH560, performing ultrasonic power ultrasonic dispersion treatment for 1-2 hours at 350-400W, performing ultrasonic finishing, washing with water, and drying to obtain the whisker-doped double-effect agent.
The mixed acid solution of the embodiment is prepared from citric acid, oxalic acid and deionized water according to a weight ratio of 2:2:5.
The mass fraction of the lanthanum chloride solution in the embodiment is 4-7%; the mass fraction of the sodium dodecyl sulfate solution is 10-15%; the pH value of the phosphate buffer solution is 5.0.
The modification method of the modified flaky graphene in the embodiment comprises the following steps:
placing the flaky graphene in a proton irradiation box for irradiation for 20-25min, wherein the irradiation power is 300-350W, and obtaining an irradiation agent after the irradiation is finished;
adding 5-8 parts of an irradiator into 15-20 parts of ethanol, then adding 2-5 parts of glycolic acid, 1-3 parts of diethanolamine and 0.25-0.35 part of sodium lignin sulfonate, stirring for reaction treatment, and washing and drying after stirring is finished to obtain the modified flaky graphene.
The conditions for the stirring reaction treatment of this example were: stirring at 55-60deg.C for 1-2 hr at a stirring speed of 350-450r/min.
The preparation method of the coordination reinforcing agent comprises the following steps:
s11: placing 5-10 parts of nano silicon dioxide into 10-15 parts of potassium permanganate solution with mass fraction of 5%, stirring thoroughly, washing with water, and drying to obtain nano silicon dioxide modifier;
s12: uniformly stirring and mixing 4-7 parts of sodium alginate solution with the mass fraction of 10%, 1-3 parts of hydrochloric acid solution with the mass fraction of 2% and 1-2 parts of yttrium nitrate solution with the mass fraction of 5%, so as to obtain an infusion;
preheating the nano silicon dioxide modifier for 10-15min at 50-55 ℃, immersing the preheated nano silicon dioxide modifier and the immersing agent according to the weight ratio of 1:5, and carrying out suction filtration and drying after the immersing is finished to obtain the coordination reinforcing agent.
The conditions of the immersion treatment of this embodiment are: the immersion treatment is carried out under high pressure of 10-15Ma, and the immersion time is 1-2h.
The preparation method of the flame-retardant antistatic coating comprises the following steps:
the flame retardant, the epoxy resin, the solvent, the whisker-doped double-effect agent, the coordination reinforcing agent and the hydroxymethyl cellulose are firstly mixed and stirred uniformly, and finally the isocyanate curing agent is added, and the mixture is placed at 40-45 ℃ for 1-2 hours, so that the flame retardant antistatic coating is obtained.
Example 1.
The flame-retardant antistatic coating comprises the following raw materials in parts by weight:
25 parts of epoxy resin, 20 parts of solvent, 10 parts of whisker-doped double-effect agent, 4 parts of coordination reinforcing agent, 3 parts of hydroxymethyl cellulose, 4 parts of flame retardant and 3 parts of isocyanate curing agent.
The isocyanate curing agent of the embodiment is bayhydur; the solvent is dimethylbenzene; the flame retardant is formed by mixing ammonium polyphosphate, melamine and pentaerythritol according to a weight ratio of 2:2:1.
The preparation method of the whisker-doped double-effect agent comprises the following steps:
s01: placing zinc oxide whisker into a mixed acid solution with the total amount of 4 times of the zinc oxide whisker, uniformly stirring, washing with water, drying, preheating for 5min at 110 ℃, and then air-cooling to room temperature to obtain pretreated zinc oxide whisker;
s02: adding 2 parts of lanthanum chloride solution into 10 parts of sodium dodecyl sulfate solution, then adding 1 part of phosphoric acid buffer solution and 2 parts of nano silica sol, and stirring fully to obtain a regulating base solution;
s03: uniformly mixing the modified flaky graphene and the pretreated zinc oxide whisker according to the weight ratio of 2:7, performing heat treatment at 310 ℃ for 5min, then cooling to 50 ℃ at the speed of 2 ℃/min, and preserving heat to obtain a flaky graphene blended zinc oxide whisker agent;
s04: adding 5 parts of flaky graphene and zinc oxide whisker agent into 15 parts of adjusting base solution, then adding 1 part of silane coupling agent KH560 and 350W ultrasonic power, performing ultrasonic dispersion treatment for 1h, ending ultrasonic treatment, washing with water, and drying to obtain the whisker-doped double-effect agent.
The mixed acid solution of the embodiment is prepared from citric acid, oxalic acid and deionized water according to a weight ratio of 2:2:5.
The mass fraction of the lanthanum chloride solution in this example was 4%; the mass fraction of the sodium dodecyl sulfate solution is 10%; the pH value of the phosphate buffer solution is 5.0.
The modification method of the modified flaky graphene in the embodiment comprises the following steps:
placing the flaky graphene in a proton irradiation box for irradiation for 20min, wherein the irradiation power is 300W, and obtaining an irradiation agent after the irradiation is finished;
adding 5 parts of an irradiator into 15 parts of ethanol, then adding 2 parts of glycolic acid, 1 part of diethanolamine and 0.25 part of sodium lignin sulfonate, stirring for reaction treatment, and washing and drying after stirring is finished to obtain the modified flaky graphene.
The conditions for the stirring reaction treatment of this example were: stirring is carried out for 1h at 55 ℃ with the stirring speed of 350r/min.
The preparation method of the coordination reinforcing agent comprises the following steps:
s11: placing 5 parts of nano silicon dioxide into 10 parts of potassium permanganate solution with the mass fraction of 5%, stirring thoroughly, washing with water, and drying to obtain a nano silicon dioxide modifier;
s12: uniformly stirring and mixing 4 parts of sodium alginate solution with the mass fraction of 10%, 1 part of hydrochloric acid solution with the mass fraction of 2% and 1 part of yttrium nitrate solution with the mass fraction of 5%, so as to obtain an infusion;
preheating the nano silicon dioxide modifier for 10min at 50 ℃, immersing the preheated nano silicon dioxide modifier and the immersing agent according to the weight ratio of 1:5, and carrying out suction filtration and drying after the immersing is finished to obtain the coordination reinforcing agent.
The conditions of the immersion treatment of this embodiment are: 1Ma, and the immersion time is 1h.
The preparation method of the flame-retardant antistatic coating comprises the following steps:
the flame retardant, the epoxy resin, the solvent, the whisker-doped double-effect agent, the coordination reinforcing agent and the hydroxymethyl cellulose are firstly mixed and stirred uniformly, and finally the isocyanate curing agent is added, and the mixture is placed for 1h at the temperature of 40 ℃ to obtain the flame retardant antistatic coating.
Example 2.
The flame-retardant antistatic coating comprises the following raw materials in parts by weight:
30 parts of epoxy resin, 25 parts of solvent, 15 parts of whisker-doped double-effect agent, 8 parts of coordination reinforcing agent, 6 parts of hydroxymethyl cellulose, 8 parts of flame retardant and 5 parts of isocyanate curing agent.
The isocyanate curing agent of the embodiment is XP2655; the solvent is dimethylbenzene; the flame retardant is formed by mixing ammonium polyphosphate, melamine and pentaerythritol according to a weight ratio of 2:2:1.
The preparation method of the whisker-doped double-effect agent comprises the following steps:
s01: placing zinc oxide whisker into a mixed acid solution with the total amount of the zinc oxide whisker being 6 times, uniformly stirring, washing with water, drying, preheating for 10min at 120 ℃, and then air-cooling to room temperature to obtain pretreated zinc oxide whisker;
s02: adding 5 parts of lanthanum chloride solution into 15 parts of sodium dodecyl sulfate solution, then adding 3 parts of phosphoric acid buffer solution and 5 parts of nano silica sol, and stirring fully to obtain a regulating base solution;
s03: uniformly mixing the modified flaky graphene and the pretreated zinc oxide whisker according to the weight ratio of 2:7, performing heat treatment at 320 ℃ for 10min, then cooling to 55 ℃ at the speed of 5 ℃/min, and preserving heat to obtain a flaky graphene blended zinc oxide whisker agent;
s04: adding 10 parts of flaky graphene and zinc oxide whisker agent into 20 parts of adjusting base solution, then adding 2 parts of silane coupling agent KH560, performing ultrasonic power ultrasonic dispersion treatment for 1-2h at 400W, and washing and drying after ultrasonic treatment to obtain the whisker-doped double-effect agent.
The mixed acid solution of the embodiment is prepared from citric acid, oxalic acid and deionized water according to a weight ratio of 2:2:5.
The mass fraction of the lanthanum chloride solution in this example was 7%; the mass fraction of the sodium dodecyl sulfate solution is 15%; the pH value of the phosphate buffer solution is 5.0.
The modification method of the modified flaky graphene in the embodiment comprises the following steps:
placing the flaky graphene in a proton irradiation box for irradiation for 25min, wherein the irradiation power is 350W, and the irradiation is finished to obtain an irradiation agent;
and adding 8 parts of an irradiator into 20 parts of ethanol, then adding 5 parts of glycolic acid, 3 parts of diethanolamine and 0.35 part of sodium lignin sulfonate, stirring for reaction treatment, and washing and drying after stirring is finished to obtain the modified flaky graphene.
The conditions for the stirring reaction treatment of this example were: stirring is carried out for 2h at 60 ℃ with the stirring speed of 450r/min.
The preparation method of the coordination reinforcing agent comprises the following steps:
s11: placing 10 parts of nano silicon dioxide into 15 parts of potassium permanganate solution with mass fraction of 5%, stirring thoroughly, washing with water, and drying to obtain a nano silicon dioxide modifier;
s12: uniformly stirring and mixing 7 parts of sodium alginate solution with the mass fraction of 10%, 3 parts of hydrochloric acid solution with the mass fraction of 2% and 2 parts of yttrium nitrate solution with the mass fraction of 5%, so as to obtain an infusion;
preheating the nano silicon dioxide modifier for 15min at 55 ℃, immersing the preheated nano silicon dioxide modifier and the immersing agent according to the weight ratio of 1:5, and carrying out suction filtration and drying after the immersing is finished to obtain the coordination reinforcing agent.
The conditions of the immersion treatment of this embodiment are: the immersion treatment was carried out under high pressure of 15Ma for 2 hours.
The preparation method of the flame-retardant antistatic coating comprises the following steps:
the flame retardant, the epoxy resin, the solvent, the whisker-doped double-effect agent, the coordination reinforcing agent and the hydroxymethyl cellulose are firstly mixed and stirred uniformly, and finally the isocyanate curing agent is added, and the mixture is placed for 2 hours at 45 ℃ to obtain the flame retardant antistatic coating.
Example 3.
The flame-retardant antistatic coating comprises the following raw materials in parts by weight:
27.5 parts of epoxy resin, 22.5 parts of solvent, 12.5 parts of whisker-doped double-effect agent, 6 parts of coordination reinforcing agent, 4.5 parts of hydroxymethyl cellulose, 6 parts of flame retardant and 4 parts of isocyanate curing agent.
The isocyanate curing agent of the embodiment is XP2655; the solvent is dimethylbenzene; the flame retardant is formed by mixing ammonium polyphosphate, melamine and pentaerythritol according to a weight ratio of 2:2:1.
The preparation method of the whisker-doped double-effect agent comprises the following steps:
s01: placing zinc oxide whisker into a mixed acid solution which is 5 times of the total amount of the zinc oxide whisker, uniformly stirring, washing with water, drying, preheating for 7.5min at 115 ℃, and then air-cooling to room temperature to obtain pretreated zinc oxide whisker;
s02: adding 3.5 parts of lanthanum chloride solution into 12.5 parts of sodium dodecyl sulfate solution, then adding 2 parts of phosphoric acid buffer solution and 3.5 parts of nano silica sol, and stirring fully to obtain a regulating base solution;
s03: uniformly mixing the modified flaky graphene and the pretreated zinc oxide whisker according to the weight ratio of 2:7, performing heat treatment at 315 ℃ for 7.5min, then cooling to 52.5 ℃ at the speed of 3.5 ℃/min, and preserving heat to obtain a flaky graphene and zinc oxide whisker agent;
s04: adding 7.5 parts of flaky graphene and zinc oxide whisker agent into 17.5 parts of adjusting base solution, then adding 1.5 parts of silane coupling agent KH560 and 370W, performing ultrasonic power ultrasonic dispersion treatment for 1.5 hours, finishing ultrasonic treatment, washing with water, and drying to obtain the whisker-doped double-effect agent.
The mixed acid solution of the embodiment is prepared from citric acid, oxalic acid and deionized water according to a weight ratio of 2:2:5.
The mass fraction of the lanthanum chloride solution of the embodiment is 5.5%; the mass fraction of the sodium dodecyl sulfate solution is 12.5%; the pH value of the phosphate buffer solution is 5.0.
The modification method of the modified flaky graphene in the embodiment comprises the following steps:
placing the flaky graphene in a proton irradiation box for irradiation for 22.5min, wherein the irradiation power is 320W, and obtaining an irradiation agent after the irradiation is finished;
adding 6.5 parts of an irradiator into 17.5 parts of ethanol, then adding 3.5 parts of glycolic acid, 2 parts of diethanolamine and 0.30 part of sodium lignin sulfonate, stirring for reaction treatment, and washing and drying after stirring is finished to obtain the modified flaky graphene.
The conditions for the stirring reaction treatment of this example were: stirring at 57.5℃for 1.5h at a stirring speed of 400r/min.
The preparation method of the coordination reinforcing agent comprises the following steps:
s11: placing 7.5 parts of nano silicon dioxide into 12.5 parts of potassium permanganate solution with mass fraction of 5%, stirring thoroughly, washing with water, and drying to obtain a nano silicon dioxide modifier;
s12: uniformly stirring and mixing 5.5 parts of sodium alginate solution with the mass fraction of 10%, 2 parts of hydrochloric acid solution with the mass fraction of 2% and 1.5 parts of yttrium nitrate solution with the mass fraction of 5%, so as to obtain an infusion;
preheating the nano silicon dioxide modifier for 12.5min at 52 ℃, immersing the preheated nano silicon dioxide modifier and the immersing agent according to the weight ratio of 1:5, and carrying out suction filtration and drying after the immersing is finished to obtain the coordination reinforcing agent.
The conditions of the immersion treatment of this embodiment are: the immersion treatment was carried out under high pressure of 12.5Ma for 1.5h.
The preparation method of the flame-retardant antistatic coating comprises the following steps:
the flame retardant, the epoxy resin, the solvent, the whisker-doped double-effect agent, the coordination reinforcing agent and the hydroxymethyl cellulose are firstly mixed and stirred uniformly, and finally the isocyanate curing agent is added, and the mixture is placed at 42.5 ℃ for 1.5 hours, so that the flame retardant antistatic coating is obtained.
Comparative example 1.
The difference from example 3 is that no double effect of doping whiskers was added.
Comparative example 2.
The difference from example 3 is that the double-effect preparation of the doped whiskers did not take the S01 step treatment.
Comparative example 3.
The difference from example 3 is that the double-effect agent doped with whiskers is prepared without heat treatment at 315 ℃ for 7.5min, then cooled to 52.5 ℃ at a rate of 3.5 ℃/min and heat-insulated.
Comparative example 4.
The difference from example 3 is that the whisker doped double effect agent was prepared without modified graphene flakes.
Comparative example 5.
The difference from example 3 is that no lanthanum chloride solution was added in the preparation of the conditioning base solution.
Comparative example 6.
The difference from example 3 is that no nanosilicon sol was added in the preparation of the conditioning base liquid.
Comparative example 7.
Unlike example 3, no co-ordinating reinforcing agent was added.
Comparative example 8.
Unlike example 3, no immersion agent treatment was used in the preparation of the co-ordinated reinforcing agent.
Comparative example 9.
The difference from example 3 is that no yttrium nitrate solution was added in the preparation of the infusion.
The products of examples 1-3 and comparative examples 1-9 were tested and measured under conventional conditions for 2000 wash-and-rinse performance as follows
From examples 1 to 3 and comparative examples 1 to 9,
the product of the embodiment 3 of the invention has excellent surface resistance and flame-retardant time, the flame-retardant and antistatic performance effects of the product can be improved in a coordinated manner, and meanwhile, the performance stability of the product is still stable under the condition of 2000 times of washing;
as shown in comparative examples 1-6 and example 3, the surface resistance and flame-retardant time of the product are obviously poor under the conditions of normal and washing for 2000 times, meanwhile, the preparation of the whisker-doped double-effect agent is not treated by adopting the step S01, the preparation of the whisker-doped double-effect agent is not treated by adopting the heat treatment at 315 ℃ for 7.5min, then the temperature is cooled to 52.5 ℃ at the speed of 3.5 ℃/min, the heat preservation treatment is carried out, the preparation of the whisker-doped double-effect agent is not treated by adopting modified flaky graphene, the preparation of the base solution is not added with lanthanum chloride solution or nano silica sol, and the performance of the product is in a trend of poor;
only the adjusting base liquid prepared by the method is matched with the double-effect agent of the doped whisker prepared by the special process of the invention for treating the modified flaky graphene, and the performance effect of the product is most remarkable; meanwhile, the double-effect agent preparation of the doped whisker is not treated by modified flaky graphene, so that the influence factor is the largest in the double-effect agent preparation of the doped whisker, and the modified flaky graphene plays an important role in the performance effect of the product;
as shown in comparative examples 7-9, comparative example 1 and example 3, the invention does not add a coordination reinforcing agent, no immersion agent treatment is adopted in the preparation of the coordination reinforcing agent, no yttrium nitrate solution is added in the preparation of the immersion agent, the performance of the product is prone to be deteriorated, the coordination reinforcing agent prepared by the method of the invention is matched with the double-effect agent doped with whisker of the invention, the synergistic effect is most obvious, and the performance effect of the product is most obvious;
the invention has no one of the double-effect agents of coordination reinforcing agent and doping whisker, the performance of the product has obvious trend of deterioration, and the product has the most obvious performance effect only by adopting the two ingredients to cooperate together.
Based on the test, the invention discovers that the modified flaky graphene has a larger influence trend on the performance of the product, and based on the result, the invention further explores the product.
The modification method of the modified flaky graphene comprises the following steps:
placing the flaky graphene in a proton irradiation box for irradiation for 22.5min, wherein the irradiation power is 320W, and obtaining an irradiation agent after the irradiation is finished;
adding 6.5 parts of an irradiator into 17.5 parts of ethanol, then adding 3.5 parts of glycolic acid, 2 parts of diethanolamine and 0.30 part of sodium lignin sulfonate, stirring for reaction treatment, and washing and drying after stirring is finished to obtain the modified flaky graphene.
The conditions for the stirring reaction treatment of this example were: stirring at 57.5℃for 1.5h at a stirring speed of 400r/min.
Experimental example 1.
The same as in example 3, except that the irradiation treatment was not employed in the preparation of the modified flaky graphene.
Experimental example 2.
As in example 3, the modified graphene flakes were prepared without adding glycolic acid.
Experimental example 3.
The same as in example 3, except that sodium lignin sulfonate was not added in the preparation of the modified flaky graphene.
Experimental example 4.
As in example 3, except that diethanolamine was not added in the preparation of the modified graphene sheet.
From experimental examples 1-4, no diethanolamine is added in the preparation of the modified flaky graphene, the performance change trend of the product is the greatest, the diethanolamine plays a leading role in the preparation of the modified flaky graphene, no glycolic acid is added in the preparation of the modified flaky graphene, no sodium lignin sulfonate is added in the preparation of the modified flaky graphene, no irradiation treatment is adopted in the preparation of the modified flaky graphene, the performance of the product has a deterioration trend, the performance effect of the product is the most obvious only by adopting the modified flaky graphene prepared by the specific method of the invention, the performance effect of the product is replaced by other methods, and the performance effect of the product is not as obvious as that of the invention.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential characteristics thereof. The present embodiments are, therefore, to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein.
Furthermore, it should be understood that although the present disclosure describes embodiments, not every embodiment is provided with a separate embodiment, and that this description is provided for clarity only, and that the disclosure is not limited to the embodiments described in detail below, and that the embodiments described in the examples may be combined as appropriate to form other embodiments that will be apparent to those skilled in the art.
Claims (10)
1. The flame-retardant antistatic coating is characterized by comprising the following raw materials in parts by weight:
25-30 parts of epoxy resin, 20-25 parts of solvent, 10-15 parts of whisker-doped double-effect agent, 4-8 parts of coordination reinforcing agent, 3-6 parts of hydroxymethyl cellulose, 4-8 parts of flame retardant and 3-5 parts of isocyanate curing agent.
2. The flame-retardant antistatic coating according to claim 1, wherein the flame-retardant antistatic coating comprises the following raw materials in parts by weight:
27.5 parts of epoxy resin, 22.5 parts of solvent, 12.5 parts of whisker-doped double-effect agent, 6 parts of coordination reinforcing agent, 4.5 parts of hydroxymethyl cellulose, 6 parts of flame retardant and 4 parts of isocyanate curing agent.
3. The flame-retardant antistatic coating according to claim 1, wherein the isocyanate curing agent is one of bayhydur and XP2655; the solvent is dimethylbenzene; the flame retardant is formed by mixing ammonium polyphosphate, melamine and pentaerythritol according to a weight ratio of 2:2:1.
4. The flame-retardant antistatic coating according to claim 1, wherein the preparation method of the whisker-doped double-effect agent is as follows:
s01: placing zinc oxide whisker into mixed acid solution with the total amount of 4-6 times of the zinc oxide whisker, uniformly stirring, washing with water, drying, preheating for 5-10min at 110-120 ℃, and then air-cooling to room temperature to obtain pretreated zinc oxide whisker;
s02: adding 2-5 parts of lanthanum chloride solution into 10-15 parts of sodium dodecyl sulfate solution, then adding 1-3 parts of phosphoric acid buffer solution and 2-5 parts of nano silica sol, and stirring fully to obtain a regulating base solution;
s03: uniformly mixing the modified flaky graphene and the pretreated zinc oxide whisker according to the weight ratio of 2:7, performing heat treatment at 310-320 ℃ for 5-10min, then cooling to 50-55 ℃ at the speed of 2-5 ℃/min, and preserving heat to obtain a flaky graphene blended zinc oxide whisker agent;
s04: adding 5-10 parts of flaky graphene and zinc oxide whisker agent into 15-20 parts of adjusting base solution, then adding 1-2 parts of silane coupling agent KH560, performing ultrasonic power ultrasonic dispersion treatment for 1-2 hours at 350-400W, performing ultrasonic finishing, washing with water, and drying to obtain the whisker-doped double-effect agent.
5. The flame-retardant antistatic coating according to claim 4, wherein the mixed acid solution is prepared from citric acid, oxalic acid and deionized water according to a weight ratio of 2:2:5;
the mass fraction of the lanthanum chloride solution is 4-7%; the mass fraction of the sodium dodecyl sulfate solution is 10-15%; the pH value of the phosphate buffer solution is 5.0.
6. The flame-retardant antistatic coating according to claim 4, wherein the modification method of the modified flaky graphene comprises the following steps:
placing the flaky graphene in a proton irradiation box for irradiation for 20-25min, wherein the irradiation power is 300-350W, and obtaining an irradiation agent after the irradiation is finished;
adding 5-8 parts of an irradiator into 15-20 parts of ethanol, then adding 2-5 parts of glycolic acid, 1-3 parts of diethanolamine and 0.25-0.35 part of sodium lignin sulfonate, stirring for reaction treatment, and washing and drying after stirring is finished to obtain the modified flaky graphene.
7. The flame retardant antistatic coating according to claim 6, wherein the conditions of the stirring reaction treatment are: stirring at 55-60deg.C for 1-2 hr at a stirring speed of 350-450r/min.
8. The flame retardant antistatic coating according to claim 1, wherein the preparation method of the coordination reinforcing agent comprises the following steps:
s11: placing 5-10 parts of nano silicon dioxide into 10-15 parts of potassium permanganate solution with mass fraction of 5%, stirring thoroughly, washing with water, and drying to obtain nano silicon dioxide modifier;
s12: uniformly stirring and mixing 4-7 parts of sodium alginate solution with the mass fraction of 10%, 1-3 parts of hydrochloric acid solution with the mass fraction of 2% and 1-2 parts of yttrium nitrate solution with the mass fraction of 5%, so as to obtain an infusion;
preheating the nano silicon dioxide modifier for 10-15min at 50-55 ℃, immersing the preheated nano silicon dioxide modifier and the immersing agent according to the weight ratio of 1:5, and carrying out suction filtration and drying after the immersing is finished to obtain the coordination reinforcing agent.
9. A flame retardant antistatic coating according to claim 8, wherein the conditions of the immersion treatment are: the immersion treatment is carried out under high pressure of 10-15Ma, and the immersion time is 1-2h.
10. A method for preparing a flame retardant antistatic coating according to any one of claims 1 to 9, comprising the steps of:
the flame retardant, the epoxy resin, the solvent, the whisker-doped double-effect agent, the coordination reinforcing agent and the hydroxymethyl cellulose are firstly mixed and stirred uniformly, and finally the isocyanate curing agent is added, and the mixture is placed at 40-45 ℃ for 1-2 hours, so that the flame retardant antistatic coating is obtained.
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