CN107523182B - Hard anti-stripping graphene water-based paint and preparation method thereof - Google Patents
Hard anti-stripping graphene water-based paint and preparation method thereof Download PDFInfo
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 57
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 52
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 41
- 239000003973 paint Substances 0.000 title claims abstract description 26
- 238000002360 preparation method Methods 0.000 title claims description 20
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims abstract description 47
- 229910000077 silane Inorganic materials 0.000 claims abstract description 47
- 239000000839 emulsion Substances 0.000 claims abstract description 41
- SNAAJJQQZSMGQD-UHFFFAOYSA-N aluminum magnesium Chemical compound [Mg].[Al] SNAAJJQQZSMGQD-UHFFFAOYSA-N 0.000 claims abstract description 18
- SMZOGRDCAXLAAR-UHFFFAOYSA-N aluminium isopropoxide Chemical compound [Al+3].CC(C)[O-].CC(C)[O-].CC(C)[O-] SMZOGRDCAXLAAR-UHFFFAOYSA-N 0.000 claims abstract description 17
- ZYWUVGFIXPNBDL-UHFFFAOYSA-N n,n-diisopropylaminoethanol Chemical compound CC(C)N(C(C)C)CCO ZYWUVGFIXPNBDL-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000002994 raw material Substances 0.000 claims abstract description 16
- 239000003822 epoxy resin Substances 0.000 claims abstract description 14
- JPMIIZHYYWMHDT-UHFFFAOYSA-N octhilinone Chemical compound CCCCCCCCN1SC=CC1=O JPMIIZHYYWMHDT-UHFFFAOYSA-N 0.000 claims abstract description 14
- 229920000647 polyepoxide Polymers 0.000 claims abstract description 14
- 239000000344 soap Substances 0.000 claims abstract description 14
- 229940045845 sodium myristate Drugs 0.000 claims abstract description 14
- JUQGWKYSEXPRGL-UHFFFAOYSA-M sodium;tetradecanoate Chemical compound [Na+].CCCCCCCCCCCCCC([O-])=O JUQGWKYSEXPRGL-UHFFFAOYSA-M 0.000 claims abstract description 14
- QDCPNGVVOWVKJG-VAWYXSNFSA-N 2-[(e)-dodec-1-enyl]butanedioic acid Chemical compound CCCCCCCCCC\C=C\C(C(O)=O)CC(O)=O QDCPNGVVOWVKJG-VAWYXSNFSA-N 0.000 claims abstract description 12
- HLBLWEWZXPIGSM-UHFFFAOYSA-N 4-Aminophenyl ether Chemical compound C1=CC(N)=CC=C1OC1=CC=C(N)C=C1 HLBLWEWZXPIGSM-UHFFFAOYSA-N 0.000 claims abstract description 12
- FBPFZTCFMRRESA-KVTDHHQDSA-N D-Mannitol Chemical compound OC[C@@H](O)[C@@H](O)[C@H](O)[C@H](O)CO FBPFZTCFMRRESA-KVTDHHQDSA-N 0.000 claims abstract description 11
- 229930195725 Mannitol Natural products 0.000 claims abstract description 11
- 239000000594 mannitol Substances 0.000 claims abstract description 11
- 235000010355 mannitol Nutrition 0.000 claims abstract description 11
- 238000003756 stirring Methods 0.000 claims description 90
- 239000006185 dispersion Substances 0.000 claims description 57
- 239000007788 liquid Substances 0.000 claims description 42
- 150000001408 amides Chemical class 0.000 claims description 29
- 238000002156 mixing Methods 0.000 claims description 25
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 23
- 239000008367 deionised water Substances 0.000 claims description 20
- 229910021641 deionized water Inorganic materials 0.000 claims description 20
- 238000009210 therapy by ultrasound Methods 0.000 claims description 15
- 239000000203 mixture Substances 0.000 claims description 14
- 229920005989 resin Polymers 0.000 claims description 14
- 239000011347 resin Substances 0.000 claims description 14
- HMMGMWAXVFQUOA-UHFFFAOYSA-N octamethylcyclotetrasiloxane Chemical compound C[Si]1(C)O[Si](C)(C)O[Si](C)(C)O[Si](C)(C)O1 HMMGMWAXVFQUOA-UHFFFAOYSA-N 0.000 claims description 13
- BCZXFFBUYPCTSJ-UHFFFAOYSA-L Calcium propionate Chemical compound [Ca+2].CCC([O-])=O.CCC([O-])=O BCZXFFBUYPCTSJ-UHFFFAOYSA-L 0.000 claims description 11
- 235000010331 calcium propionate Nutrition 0.000 claims description 11
- 239000004330 calcium propionate Substances 0.000 claims description 11
- -1 carboxyl graphene Chemical compound 0.000 claims description 11
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 claims description 10
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims description 10
- 239000002131 composite material Substances 0.000 claims description 10
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims description 10
- 229920002554 vinyl polymer Polymers 0.000 claims description 10
- 239000011701 zinc Substances 0.000 claims description 10
- 229910052725 zinc Inorganic materials 0.000 claims description 10
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 5
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 5
- 239000000244 polyoxyethylene sorbitan monooleate Substances 0.000 claims description 5
- 235000010482 polyoxyethylene sorbitan monooleate Nutrition 0.000 claims description 5
- 229920000136 polysorbate Polymers 0.000 claims description 5
- 229950008882 polysorbate Drugs 0.000 claims description 5
- 229920000053 polysorbate 80 Polymers 0.000 claims description 5
- 229940068968 polysorbate 80 Drugs 0.000 claims description 5
- 238000004321 preservation Methods 0.000 claims description 3
- 238000000576 coating method Methods 0.000 abstract description 23
- 239000011248 coating agent Substances 0.000 abstract description 17
- 239000000853 adhesive Substances 0.000 abstract description 4
- 230000001070 adhesive effect Effects 0.000 abstract description 4
- 239000000463 material Substances 0.000 abstract description 2
- 235000019441 ethanol Nutrition 0.000 description 11
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 6
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 4
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 4
- 239000004593 Epoxy Substances 0.000 description 3
- 239000000654 additive Substances 0.000 description 3
- 238000005260 corrosion Methods 0.000 description 3
- 230000007797 corrosion Effects 0.000 description 3
- 239000002904 solvent Substances 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- 230000005587 bubbling Effects 0.000 description 2
- 239000012153 distilled water Substances 0.000 description 2
- 239000000945 filler Substances 0.000 description 2
- 239000011780 sodium chloride Substances 0.000 description 2
- 229910000831 Steel Inorganic materials 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 239000004568 cement Substances 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 239000004814 polyurethane Substances 0.000 description 1
- 229920002635 polyurethane Polymers 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D163/00—Coating compositions based on epoxy resins; Coating compositions based on derivatives of epoxy resins
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K13/00—Use of mixtures of ingredients not covered by one single of the preceding main groups, each of these compounds being essential
- C08K13/06—Pretreated ingredients and ingredients covered by the main groups C08K3/00 - C08K7/00
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/08—Metals
- C08K2003/0812—Aluminium
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/04—Carbon
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/34—Silicon-containing compounds
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
- C08K5/09—Carboxylic acids; Metal salts thereof; Anhydrides thereof
- C08K5/098—Metal salts of carboxylic acids
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/16—Nitrogen-containing compounds
- C08K5/20—Carboxylic acid amides
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
- C08K9/06—Ingredients treated with organic substances with silicon-containing compounds
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- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- Paints Or Removers (AREA)
Abstract
The invention discloses a hard anti-stripping graphene water-based paint which is prepared from the following raw materials in parts by weight: 25-30 parts of aluminum isopropoxide, 100-120 parts of epoxy resin E44100, 1-2 parts of dodecenylsuccinic acid, 0.7-1 part of sodium myristate soap, 0.1-0.2 part of octyl isothiazolinone, 0.8-1 part of diisopropylethanolamine, 0.06-0.1 part of diaminodiphenyl ether, 4-5 parts of mannitol, 10-14 parts of hard silane emulsion and 10-14 parts of graphene. The added sodium myristate soap and the added sol effectively improve the viscosity of the coating, improve the adhesive force between a finished coating and a base material, and enhance the peeling strength, and simultaneously, the added graphene, magnesium aluminum silicate and the like can effectively improve the surface hardness of the coating and enhance the impact strength.
Description
Technical Field
The invention belongs to the field of coatings, and particularly relates to a hard anti-stripping graphene water-based coating and a preparation method thereof.
Background
Compared with solvent-based coatings, water-based coatings have many advantages, such as low VOC content, low odor, nonflammability, safe use, water cleanability, and the like. Therefore, people can make epoxy resin into water paint by water-based treatment to meet higher requirements. Decades of research, development and application practices prove that the water-based epoxy paint coating has the advantages of epoxy resin, excellent adhesive force to steel and cement, low shrinkage rate, good corrosion resistance and permeability resistance to medium acid, alkali and other solvents, can be well mixed and dissolved with various resins, fillers and auxiliaries to prepare a series of common anticorrosive paints, and can form a system of the water-based epoxy anticorrosive paint.
However, compared with solvent-based coatings, the formulation of water-based coatings is complex, and in order to improve the mechanical properties of the surface of the finished coating, various inorganic additives such as graphene and silica are usually included, and the inorganic additives are poor in dispersibility with the resin, so that the stability of the coating is affected, and the properties of the coating are reduced.
Disclosure of Invention
The invention aims to provide a hard anti-stripping graphene water-based paint and a preparation method thereof, aiming at the problem that the performance of a coating film is reduced due to the influence of poor dispersibility of an inorganic additive and a resin on the stability of the coating film.
In order to achieve the purpose, the invention adopts the following technical scheme:
the hard anti-stripping graphene water-based paint is composed of the following raw materials in parts by weight:
25-30 parts of aluminum isopropoxide, 100-120 parts of epoxy resin E44100, 1-2 parts of dodecenylsuccinic acid, 0.7-1 part of sodium myristate soap, 0.1-0.2 part of octyl isothiazolinone, 0.8-1 part of diisopropylethanolamine, 0.06-0.1 part of diaminodiphenyl ether, 4-5 parts of mannitol, 10-14 parts of hard silane emulsion and 10-14 parts of graphene.
The hard silane emulsion is prepared from the following raw materials in parts by weight:
10-14 parts of magnesium aluminum silicate, 1-2 parts of octamethylcyclotetrasiloxane, 800.06-0.1 part of polysorbate, 3-5 parts of N-methylpyrrolidone, 1-2 parts of calcium propionate, 0.7-1 part of zinc dialkyl dithiophosphate and 50-60 parts of amide dispersion.
The preparation method of the amide dispersion liquid comprises the following steps: adding the vinyl distearamide into deionized water with the weight 30-40 times of that of the vinyl distearamide, and uniformly stirring to obtain the water-based emulsion.
The preparation method of the hard silane emulsion comprises the following steps:
(1) adding octamethylcyclotetrasiloxane into 10-16 times of anhydrous ethanol, stirring uniformly, adding magnesium aluminum silicate, stirring at 50-60 ℃ for 1-2 hours under heat preservation, adding polysorbate 80, and stirring to normal temperature to obtain a silane dispersion liquid;
(2) mixing zinc dialkyl dithiophosphate and calcium propionate, adding the mixture into the amide dispersion liquid, and performing ultrasonic treatment for 3-5 minutes to obtain a hard amide dispersion liquid;
(3) and (3) mixing the silane dispersion liquid and the hard amide dispersion liquid, uniformly stirring, adding N-methyl pyrrolidone, and carrying out ultrasonic treatment for 10-14 minutes to obtain the hard silane emulsion.
A preparation method of a hard anti-stripping graphene water-based paint comprises the following steps:
(1) adding octyl isothiazolinone into 5-7 times of anhydrous ethanol, stirring, adding mannitol, stirring at 60-70 deg.C for 4-10 min to obtain composite alcohol dispersion;
(2) mixing graphene and dodecenylsuccinic acid, adding the mixture into deionized water with the weight being 20-30 times of that of the mixture, uniformly stirring, adding diaminodiphenyl ether, and carrying out ultrasonic treatment for 4-5 minutes to obtain carboxyl graphene dispersion liquid;
(3) adding aluminum isopropoxide into deionized water 40-55 times of the weight of the aluminum isopropoxide, uniformly stirring, adding the composite alcohol dispersion, uniformly stirring, dropwise adding ammonia water, adjusting the pH to 10-13, stirring at normal temperature for 2-3 hours, adding sodium myristate soap, and uniformly stirring to obtain a sol-alcohol solution;
(4) adding diisopropylethanolamine into deionized water with the weight of 130-140 times that of the diisopropylethanolamine, uniformly stirring, adding epoxy resin E44 and hard silane emulsion, and stirring for 10-20 minutes at the temperature of 50-60 ℃ to obtain resin silane emulsion;
(5) and mixing the sol-alcohol solution and the carboxyl graphene dispersion solution, uniformly stirring, stirring for 2-3 hours at the temperature of 90-95 ℃, adding the resin silane emulsion, stirring to normal temperature, mixing with the rest raw materials, stirring for 30-40 minutes at 1600 revolutions per minute and 2000 minutes to obtain the hard anti-stripping graphene water-based paint.
The advantages and innovation points of the invention are mainly reflected in that:
the invention adopts octamethylcyclotetrasiloxane to treat the magnesium aluminum silicate, then disperses the magnesium aluminum silicate into an alcohol solution, and then blends the alcohol solution with an amide dispersion liquid, thereby effectively improving the dispersibility of the magnesium aluminum silicate and calcium propionate in the solution;
according to the preparation method, graphene is treated by dodecenylsuccinic acid and then is dispersed by using diaminodiphenyl ether to obtain carboxylated graphene, the surface of the graphene is organized, the dispersibility of the graphene in a finished coating is improved, and the stability of a finished product is improved;
according to the invention, aluminum isopropoxide is used as a precursor, hydrolyzed in an alcohol solution, and added with a sodium myristate soap, so that the viscosity of the sol is effectively improved, and then the sol is blended and esterified with a carboxyl graphene dispersion liquid, so that the aluminum sol is fully organized, and the dispersibility of the aluminum sol in the coating is improved;
according to the invention, the epoxy resin is dispersed into the amide solution and is blended with the hard silane emulsion, so that the dispersibility of the hard filler in the resin is effectively improved, the agglomeration is effectively reduced, and the stability of the finished product is improved;
the added sodium myristate soap and the added sol effectively improve the viscosity of the coating, improve the adhesive force between a finished coating and a base material, and enhance the peeling strength, and simultaneously, the added graphene, magnesium aluminum silicate and the like can effectively improve the surface hardness of the coating and enhance the impact strength.
Detailed Description
Example 1
The hard anti-stripping graphene water-based paint is composed of the following raw materials in parts by weight:
25 parts of aluminum isopropoxide, an epoxy resin E44100, 1 part of dodecenylsuccinic acid, 0.7 part of sodium myristate soap, 0.1 part of octyl isothiazolinone, 0.8 part of diisopropylethanolamine, 0.06 part of diaminodiphenyl ether, 4 parts of mannitol, 10 parts of hard silane emulsion and 10 parts of graphene.
The hard silane emulsion is prepared from the following raw materials in parts by weight:
10 parts of magnesium aluminum silicate, 1 part of octamethylcyclotetrasiloxane, 800.06 parts of polysorbate, 3 parts of N-methylpyrrolidone, 1 part of calcium propionate, 0.7 part of zinc dialkyl dithiophosphate and 50 parts of amide dispersion liquid.
The preparation method of the amide dispersion liquid comprises the following steps: adding the vinyl distearamide into deionized water with the weight 30 times of that of the vinyl distearamide, and uniformly stirring to obtain the water-based emulsion.
The preparation method of the hard silane emulsion comprises the following steps:
(1) adding octamethylcyclotetrasiloxane into 10 times of anhydrous ethanol, stirring uniformly, adding magnesium aluminum silicate, stirring at 50 ℃ for 1 hour under heat preservation, adding polysorbate 80, and stirring to normal temperature to obtain a silane dispersion liquid;
(2) mixing magnesium aluminum silicate and calcium propionate, adding into the amide dispersion liquid, and performing ultrasonic treatment for 3 minutes to obtain a hard amide dispersion liquid;
(3) and (3) mixing the silane dispersion liquid and the hard amide dispersion liquid, uniformly stirring, adding zinc dialkyl dithiophosphate and N-methyl pyrrolidone, and carrying out ultrasonic treatment for 10 minutes to obtain the hard silane emulsion.
A preparation method of a hard anti-stripping graphene water-based paint comprises the following steps:
(1) adding octyl isothiazolinone into absolute ethyl alcohol with the weight 5 times of that of the octyl isothiazolinone, uniformly stirring, adding mannitol, and stirring for 4 minutes at the temperature of 60 ℃ to obtain composite alcohol dispersion liquid;
(2) mixing graphene and dodecenylsuccinic acid, adding the mixture into deionized water with the weight being 20 times that of the mixture, uniformly stirring, adding diaminodiphenyl ether, and performing ultrasonic treatment for 4 minutes to obtain carboxyl graphene dispersion liquid;
(3) adding aluminum isopropoxide into deionized water 40 times of the weight of the aluminum isopropoxide, uniformly stirring, adding the composite alcohol dispersion, uniformly stirring, dropwise adding ammonia water, adjusting the pH to 10, stirring for 2 hours at normal temperature, adding sodium myristate soap, and uniformly stirring to obtain a sol-alcohol solution;
(4) adding diisopropylethanolamine into deionized water 130 times the weight of diisopropylethanolamine, uniformly stirring, adding epoxy resin E44 and hard silane emulsion, and stirring for 10 minutes at 50 ℃ to obtain resin silane emulsion;
(5) and (3) mixing the sol-alcohol solution and the carboxyl graphene dispersion solution, uniformly stirring, keeping the temperature at 90 ℃ and stirring for 2 hours, adding the resin silane emulsion, stirring to normal temperature, mixing with the rest raw materials, and stirring at 1600 rpm for 30 minutes to obtain the hard anti-stripping graphene water-based paint.
Example 2
The hard anti-stripping graphene water-based paint is composed of the following raw materials in parts by weight:
30 parts of aluminum isopropoxide, E44120 parts of epoxy resin, 2 parts of dodecenylsuccinic acid, 1 part of sodium myristate soap, 0.2 part of octyl isothiazolinone, 1 part of diisopropylethanolamine, 0.1 part of diaminodiphenyl ether, 5 parts of mannitol, 14 parts of hard silane emulsion and 14 parts of graphene.
The hard silane emulsion is prepared from the following raw materials in parts by weight:
14 parts of magnesium aluminum silicate, 2 parts of octamethylcyclotetrasiloxane, 800.1 parts of polysorbate, 5 parts of N-methylpyrrolidone, 2 parts of calcium propionate, 1 part of zinc dialkyl dithiophosphate and 60 parts of amide dispersion liquid.
The preparation method of the amide dispersion liquid comprises the following steps: adding the vinyl distearic acid amide into deionized water with the weight 40 times of that of the vinyl distearic acid amide, and uniformly stirring to obtain the water-based polyurethane adhesive.
The preparation method of the hard silane emulsion comprises the following steps:
(1) adding octamethylcyclotetrasiloxane into anhydrous ethanol with the weight 16 times of that of octamethylcyclotetrasiloxane, uniformly stirring, adding magnesium aluminum silicate, stirring for 2 hours at the temperature of 60 ℃, adding polysorbate 80, and stirring to normal temperature to obtain a silane dispersion liquid;
(2) mixing magnesium aluminum silicate and calcium propionate, adding into the amide dispersion liquid, and performing ultrasonic treatment for 5 minutes to obtain a hard amide dispersion liquid;
(3) and (3) mixing the silane dispersion liquid and the hard amide dispersion liquid, uniformly stirring, adding zinc dialkyl dithiophosphate and N-methyl pyrrolidone, and carrying out ultrasonic treatment for 14 minutes to obtain the hard silane emulsion.
A preparation method of a hard anti-stripping graphene water-based paint comprises the following steps:
(1) adding octyl isothiazolinone into absolute ethyl alcohol with the weight 7 times of that of the octyl isothiazolinone, uniformly stirring, adding mannitol, and stirring for 10 minutes at the temperature of 70 ℃ to obtain composite alcohol dispersion liquid;
(2) mixing graphene and dodecenylsuccinic acid, adding the mixture into deionized water with the weight being 20-30 times of that of the mixture, uniformly stirring, adding diaminodiphenyl ether, and performing ultrasonic treatment for 5 minutes to obtain carboxyl graphene dispersion liquid;
(3) adding aluminum isopropoxide into deionized water 55 times of the weight of the aluminum isopropoxide, uniformly stirring, adding the composite alcohol dispersion, uniformly stirring, dropwise adding ammonia water, adjusting the pH to 13, stirring for 3 hours at normal temperature, adding sodium myristate soap, and uniformly stirring to obtain a sol-alcohol solution;
(4) adding diisopropylethanolamine into deionized water 140 times the weight of diisopropylethanolamine, uniformly stirring, adding epoxy resin E44 and hard silane emulsion, and stirring for 20 minutes at 60 ℃ to obtain resin silane emulsion;
(5) and (3) mixing the sol-alcohol solution and the carboxyl graphene dispersion solution, uniformly stirring, keeping the temperature at 95 ℃ and stirring for 3 hours, adding the resin silane emulsion, stirring to normal temperature, mixing with the rest raw materials, and stirring at 2000 rpm for 40 minutes to obtain the hard anti-stripping graphene water-based paint.
Example 3
The hard anti-stripping graphene water-based paint is composed of the following raw materials in parts by weight:
aluminum isopropoxide 28, epoxy resin E44110, dodecenylsuccinic acid 1.5, sodium myristate soap 0.9, octyl isothiazolinone 0.15, diisopropyl ethanolamine 0.88, diaminodiphenyl ether 0.08, mannitol 4.5, hard silane emulsion 12 and graphene 13.
The hard silane emulsion is prepared from the following raw materials in parts by weight:
magnesium aluminum silicate 13, octamethylcyclotetrasiloxane 1.15, polysorbate 800.07, N-methylpyrrolidone 4, calcium propionate 1.5, zinc dialkyldithiophosphate 0.8, and amide dispersion 52.
The preparation method of the amide dispersion liquid comprises the following steps: adding the vinyl distearamide into deionized water with the weight 32 times of that of the vinyl distearamide, and uniformly stirring to obtain the water-based emulsion.
The preparation method of the hard silane emulsion comprises the following steps:
(1) adding octamethylcyclotetrasiloxane into anhydrous ethanol with the weight 14 times of that of octamethylcyclotetrasiloxane, stirring uniformly, adding magnesium aluminum silicate, stirring for 1.5 hours at the temperature of 52 ℃, adding polysorbate 80, and stirring to normal temperature to obtain a silane dispersion liquid;
(2) mixing zinc dialkyl dithiophosphate and calcium propionate, adding the mixture into the amide dispersion liquid, and performing ultrasonic treatment for 4 minutes to obtain a hard amide dispersion liquid;
(3) and (3) mixing the silane dispersion liquid and the hard amide dispersion liquid, uniformly stirring, adding N-methyl pyrrolidone, and carrying out ultrasonic treatment for 12 minutes to obtain the hard silane emulsion.
A preparation method of a hard anti-stripping graphene water-based paint comprises the following steps:
(1) adding octyl isothiazolinone into absolute ethyl alcohol with the weight 6 times of that of the octyl isothiazolinone, uniformly stirring, adding mannitol, and stirring for 7 minutes at the temperature of 65 ℃ to obtain composite alcohol dispersion liquid;
(2) mixing graphene and dodecenylsuccinic acid, adding the mixture into deionized water with the weight 24 times that of the mixture, uniformly stirring, adding diaminodiphenyl ether, and performing ultrasonic treatment for 4.5 minutes to obtain carboxyl graphene dispersion liquid;
(3) adding aluminum isopropoxide into deionized water with the weight being 48 times of that of the aluminum isopropoxide, uniformly stirring, adding the composite alcohol dispersion, uniformly stirring, dropwise adding ammonia water, adjusting the pH to 12, stirring for 2.5 hours at normal temperature, adding sodium myristate soap, and uniformly stirring to obtain a sol-alcohol solution;
(4) adding diisopropylethanolamine into deionized water with the weight being 136 times that of diisopropylethanolamine, uniformly stirring, adding epoxy resin E44 and hard silane emulsion, and stirring for 18 minutes at the temperature of 57 ℃ to obtain resin silane emulsion;
(5) and (3) mixing the sol-alcohol solution and the carboxyl graphene dispersion solution, uniformly stirring, stirring for 2.5 hours at the temperature of 92 ℃, adding the resin silane emulsion, stirring to normal temperature, mixing with the rest raw materials, and stirring for 38 minutes at 1800 rpm to obtain the hard anti-stripping graphene water-based paint.
Comparative Performance test
The hard anti-stripping graphene water-based paint comprises the following components in percentage by weight:
adhesion force: grade 1;
the corrosion resistance of the coating film is as follows:
distilled water/d soak edge blistering: 15-16;
3% sodium chloride solution/d soaked edge blistering: 19-20;
10% sodium hydroxide solution/d soaked edge blistering: 14-15;
10% hydrochloric acid solution/d soaked edge bubbling: 4-5;
gasoline/d soak edge blistering: 5-6;
pencil hardness: 4H;
tensile Strength/PMa: 100-104.
Commercial epoxy E44 waterborne coatings:
adhesion force: 2, level;
the corrosion resistance of the coating film is as follows:
distilled water/d soak edge blistering: 10-11;
3% sodium chloride solution/d soaked edge blistering: 13-14;
10% sodium hydroxide solution/d soaked edge blistering: 10-11;
10% hydrochloric acid solution/d soaked edge bubbling: 1-2;
gasoline/d soak edge blistering: 2-3;
pencil hardness: 3H;
tensile Strength/PMa: 90-93.
Claims (4)
1. The hard anti-stripping graphene water-based paint is characterized by comprising the following raw materials in parts by weight:
25-30 parts of aluminum isopropoxide, 100-120 parts of epoxy resin E44100, 1-2 parts of dodecenylsuccinic acid, 0.7-1 part of sodium myristate soap, 0.1-0.2 part of octyl isothiazolinone, 0.8-1 part of diisopropylethanolamine, 0.06-0.1 part of diaminodiphenyl ether, 4-5 parts of mannitol, 10-14 parts of hard silane emulsion and 10-14 parts of graphene;
the hard silane emulsion is prepared from the following raw materials in parts by weight: 10-14 parts of magnesium aluminum silicate, 1-2 parts of octamethylcyclotetrasiloxane, 800.06-0.1 part of polysorbate, 3-5 parts of N-methylpyrrolidone, 1-2 parts of calcium propionate, 0.7-1 part of zinc dialkyl dithiophosphate and 50-60 parts of amide dispersion.
2. The hard anti-stripping graphene water-based paint as claimed in claim 1, wherein the preparation method of the amide dispersion liquid comprises the following steps: adding the vinyl distearamide into deionized water with the weight 30-40 times of that of the vinyl distearamide, and uniformly stirring to obtain the water-based emulsion.
3. The hard anti-stripping graphene water-based paint as claimed in claim 1, wherein the preparation method of the hard silane emulsion comprises the following steps:
(1) adding octamethylcyclotetrasiloxane into 10-16 times of anhydrous ethanol, stirring uniformly, adding magnesium aluminum silicate, stirring at 50-60 ℃ for 1-2 hours under heat preservation, adding polysorbate 80, and stirring to normal temperature to obtain a silane dispersion liquid;
(2) mixing magnesium aluminum silicate and calcium propionate, adding into the amide dispersion liquid, and performing ultrasonic treatment for 3-5 minutes to obtain a hard amide dispersion liquid;
(3) and (3) mixing the silane dispersion liquid and the hard amide dispersion liquid, uniformly stirring, adding zinc dialkyl dithiophosphate and N-methyl pyrrolidone, and carrying out ultrasonic treatment for 10-14 minutes to obtain the hard silane emulsion.
4. The preparation method of the hard anti-stripping graphene water-based paint according to claim 1, characterized by comprising the following steps:
(1) adding octyl isothiazolinone into 5-7 times of anhydrous ethanol, stirring, adding mannitol, stirring at 60-70 deg.C for 4-10 min to obtain composite alcohol dispersion;
(2) mixing graphene and dodecenylsuccinic acid, adding the mixture into deionized water with the weight being 20-30 times of that of the mixture, uniformly stirring, adding diaminodiphenyl ether, and carrying out ultrasonic treatment for 4-5 minutes to obtain carboxyl graphene dispersion liquid;
(3) adding aluminum isopropoxide into deionized water 40-55 times of the weight of the aluminum isopropoxide, uniformly stirring, adding the composite alcohol dispersion, uniformly stirring, dropwise adding ammonia water, adjusting the pH to 10-13, stirring at normal temperature for 2-3 hours, adding sodium myristate soap, and uniformly stirring to obtain a sol-alcohol solution;
(4) adding diisopropylethanolamine into deionized water with the weight of 130-140 times that of the diisopropylethanolamine, uniformly stirring, adding epoxy resin E44 and hard silane emulsion, and stirring for 10-20 minutes at the temperature of 50-60 ℃ to obtain resin silane emulsion;
(5) and mixing the sol-alcohol solution and the carboxyl graphene dispersion solution, uniformly stirring, stirring for 2-3 hours at the temperature of 90-95 ℃, adding the resin silane emulsion, stirring to normal temperature, mixing with the rest raw materials, stirring for 30-40 minutes at 1600 revolutions per minute and 2000 minutes to obtain the hard anti-stripping graphene water-based paint.
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| CN105949576A (en) * | 2016-06-22 | 2016-09-21 | 安徽电信器材贸易工业有限责任公司 | High-strength heat-resistant optical cable material and preparation method thereof |
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