CN117165130B - Processing technology of high-strength nut - Google Patents
Processing technology of high-strength nut Download PDFInfo
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- CN117165130B CN117165130B CN202311137782.9A CN202311137782A CN117165130B CN 117165130 B CN117165130 B CN 117165130B CN 202311137782 A CN202311137782 A CN 202311137782A CN 117165130 B CN117165130 B CN 117165130B
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- 238000005516 engineering process Methods 0.000 title claims abstract description 14
- 238000012545 processing Methods 0.000 title claims abstract description 14
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 claims abstract description 55
- 229920000767 polyaniline Polymers 0.000 claims abstract description 53
- 238000000576 coating method Methods 0.000 claims abstract description 46
- 239000011248 coating agent Substances 0.000 claims abstract description 45
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 42
- 238000003756 stirring Methods 0.000 claims abstract description 42
- 239000002002 slurry Substances 0.000 claims abstract description 34
- 238000001035 drying Methods 0.000 claims abstract description 31
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 28
- 229920002037 poly(vinyl butyral) polymer Polymers 0.000 claims abstract description 25
- 229910001220 stainless steel Inorganic materials 0.000 claims abstract description 25
- 239000010935 stainless steel Substances 0.000 claims abstract description 25
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims abstract description 24
- 239000002131 composite material Substances 0.000 claims abstract description 22
- 239000004408 titanium dioxide Substances 0.000 claims abstract description 21
- 229920003229 poly(methyl methacrylate) Polymers 0.000 claims abstract description 20
- 239000004926 polymethyl methacrylate Substances 0.000 claims abstract description 20
- 239000006185 dispersion Substances 0.000 claims abstract description 17
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims abstract description 16
- 238000002156 mixing Methods 0.000 claims abstract description 16
- 239000002202 Polyethylene glycol Substances 0.000 claims abstract description 14
- 229920001223 polyethylene glycol Polymers 0.000 claims abstract description 14
- VVQNEPGJFQJSBK-UHFFFAOYSA-N Methyl methacrylate Chemical compound COC(=O)C(C)=C VVQNEPGJFQJSBK-UHFFFAOYSA-N 0.000 claims abstract description 13
- GCSJLQSCSDMKTP-UHFFFAOYSA-N ethenyl(trimethyl)silane Chemical compound C[Si](C)(C)C=C GCSJLQSCSDMKTP-UHFFFAOYSA-N 0.000 claims abstract description 13
- 238000000034 method Methods 0.000 claims abstract description 12
- 239000007788 liquid Substances 0.000 claims abstract description 11
- OZAIFHULBGXAKX-UHFFFAOYSA-N 2-(2-cyanopropan-2-yldiazenyl)-2-methylpropanenitrile Chemical compound N#CC(C)(C)N=NC(C)(C)C#N OZAIFHULBGXAKX-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000005238 degreasing Methods 0.000 claims abstract description 10
- 238000001132 ultrasonic dispersion Methods 0.000 claims abstract description 10
- 239000012299 nitrogen atmosphere Substances 0.000 claims abstract description 8
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 claims abstract description 8
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 42
- PAYRUJLWNCNPSJ-UHFFFAOYSA-N Aniline Chemical compound NC1=CC=CC=C1 PAYRUJLWNCNPSJ-UHFFFAOYSA-N 0.000 claims description 22
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical group [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims description 21
- FUZZWVXGSFPDMH-UHFFFAOYSA-N hexanoic acid Chemical compound CCCCCC(O)=O FUZZWVXGSFPDMH-UHFFFAOYSA-N 0.000 claims description 19
- 229910021389 graphene Inorganic materials 0.000 claims description 18
- 238000005406 washing Methods 0.000 claims description 17
- XRWMGCFJVKDVMD-UHFFFAOYSA-M didodecyl(dimethyl)azanium;bromide Chemical compound [Br-].CCCCCCCCCCCC[N+](C)(C)CCCCCCCCCCCC XRWMGCFJVKDVMD-UHFFFAOYSA-M 0.000 claims description 16
- 239000000243 solution Substances 0.000 claims description 16
- XDLMVUHYZWKMMD-UHFFFAOYSA-N 3-trimethoxysilylpropyl 2-methylprop-2-enoate Chemical compound CO[Si](OC)(OC)CCCOC(=O)C(C)=C XDLMVUHYZWKMMD-UHFFFAOYSA-N 0.000 claims description 15
- 239000013078 crystal Substances 0.000 claims description 14
- 239000008367 deionised water Substances 0.000 claims description 13
- 229910021641 deionized water Inorganic materials 0.000 claims description 13
- DKPFZGUDAPQIHT-UHFFFAOYSA-N Butyl acetate Natural products CCCCOC(C)=O DKPFZGUDAPQIHT-UHFFFAOYSA-N 0.000 claims description 12
- LAQPNDIUHRHNCV-UHFFFAOYSA-N isophthalonitrile Chemical compound N#CC1=CC=CC(C#N)=C1 LAQPNDIUHRHNCV-UHFFFAOYSA-N 0.000 claims description 12
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims description 10
- YHWCPXVTRSHPNY-UHFFFAOYSA-N butan-1-olate;titanium(4+) Chemical compound [Ti+4].CCCC[O-].CCCC[O-].CCCC[O-].CCCC[O-] YHWCPXVTRSHPNY-UHFFFAOYSA-N 0.000 claims description 10
- 239000011259 mixed solution Substances 0.000 claims description 10
- WBIQQQGBSDOWNP-UHFFFAOYSA-N 2-dodecylbenzenesulfonic acid Chemical compound CCCCCCCCCCCCC1=CC=CC=C1S(O)(=O)=O WBIQQQGBSDOWNP-UHFFFAOYSA-N 0.000 claims description 9
- 238000000967 suction filtration Methods 0.000 claims description 9
- 238000001291 vacuum drying Methods 0.000 claims description 9
- 229940060296 dodecylbenzenesulfonic acid Drugs 0.000 claims description 8
- 230000008569 process Effects 0.000 claims description 8
- 239000006228 supernatant Substances 0.000 claims description 8
- 238000004519 manufacturing process Methods 0.000 claims description 7
- 238000002360 preparation method Methods 0.000 claims description 5
- 239000003054 catalyst Substances 0.000 claims description 4
- 229920000642 polymer Polymers 0.000 claims description 3
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical group O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 claims description 2
- 239000002904 solvent Substances 0.000 claims description 2
- 238000003760 magnetic stirring Methods 0.000 abstract 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 19
- 238000005260 corrosion Methods 0.000 description 16
- 230000007797 corrosion Effects 0.000 description 14
- 229910052751 metal Inorganic materials 0.000 description 11
- 239000002184 metal Substances 0.000 description 11
- 230000000052 comparative effect Effects 0.000 description 9
- 230000004048 modification Effects 0.000 description 4
- 238000012986 modification Methods 0.000 description 4
- 239000002121 nanofiber Substances 0.000 description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 230000020477 pH reduction Effects 0.000 description 3
- 230000035515 penetration Effects 0.000 description 3
- 239000011148 porous material Substances 0.000 description 3
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- 239000000835 fiber Substances 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 238000004770 highest occupied molecular orbital Methods 0.000 description 2
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 2
- 238000004768 lowest unoccupied molecular orbital Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 238000002161 passivation Methods 0.000 description 2
- 229920005989 resin Polymers 0.000 description 2
- 239000011347 resin Substances 0.000 description 2
- 238000007581 slurry coating method Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- 239000004593 Epoxy Substances 0.000 description 1
- 238000005299 abrasion Methods 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical class [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000003112 inhibitor Substances 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
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- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention relates to the technical field of nuts and discloses a processing technology of a high-strength nut; the method comprises the following steps: adding methyl methacrylate, vinyl trimethylsilane and azodiisobutyronitrile into tetrahydrofuran, and reacting at 80-85 ℃ in nitrogen atmosphere to obtain polymethyl methacrylate; mixing polymethyl methacrylate, polyethylene glycol and polyvinyl butyral at 190-195 ℃, adding nano titanium dioxide dispersion liquid, and continuously stirring to obtain nano titanium dioxide slurry; dissolving polyvinyl butyral in methanol, adding a graphene-polyaniline composite material, performing ultrasonic dispersion and magnetic stirring to obtain graphene-polyaniline slurry; and (3) putting the pretreated stainless steel nut into nano titanium dioxide slurry, taking out and drying, degreasing in water, drying to obtain a titanium dioxide coating, coating graphene-polyaniline slurry on the surface of the titanium dioxide coating, and drying to obtain the high-strength nut.
Description
Technical Field
The invention relates to the technical field of nuts, in particular to a processing technology of a high-strength nut.
Background
The problem of metal corrosion causes great loss to the production economy, and stainless steel is no exception; the stainless steel nut is used as a fixing structure of key components such as machinery, pipelines, switches, valves and the like, when the stainless steel nut is corroded by metal, the stainless steel nut is easy to rust, the structure is invalid due to rust death, the key parts are damaged, and serious potential safety hazards are caused; the anti-corrosion coating is a common and effective protection means at present, wherein the environment-friendly epoxy polymer coating is widely used, but gaps appear in the coating after moisture evaporation and solidification, water, oxygen, electrolyte and other corrosion mediums cannot be permeated, the wear resistance is poor, abrasion is caused in the use process, and the anti-corrosion coating coated on the surface is easy to fall off and lose efficacy.
Therefore, the invention has important significance in the high-strength nut with corrosion resistance and wear resistance.
Disclosure of Invention
The invention aims to provide a processing technology of a high-strength nut, which aims to solve the problems in the prior art.
In order to solve the technical problems, the invention provides the following technical scheme:
a processing technology of a high-strength nut comprises the following steps:
s1: adding methyl methacrylate, vinyl trimethylsilane and azodiisobutyronitrile into tetrahydrofuran, and reacting for 4-5 hours at 80-85 ℃ in nitrogen atmosphere to obtain polymethyl methacrylate; mixing polymethyl methacrylate, polyethylene glycol and polyvinyl butyral at 190-195 ℃ for 10-15min, adding nano titanium dioxide dispersion liquid, and continuously stirring for 10-15min to obtain nano titanium dioxide slurry;
s2: dissolving polyvinyl butyral in methanol, adding a graphene-polyaniline composite material, performing ultrasonic dispersion for 1-1.5h, and magnetically stirring for 8-12h to obtain graphene-polyaniline slurry; and (3) placing the pretreated stainless steel nut into nano titanium dioxide slurry, taking out and drying, degreasing in water at 50-55 ℃ for 2-2.5h, drying to obtain a titanium dioxide coating, coating graphene-polyaniline slurry on the surface of the titanium dioxide coating, and drying to obtain the high-strength nut.
Further, the preparation method of the nano titanium dioxide dispersion liquid comprises the following steps:
adding tetrabutyl titanate and n-caproic acid into deionized water, reacting for 3-3.5h at 240-250 ℃, centrifuging, washing and drying to obtain nano titanium dioxide crystals; adding the nano titanium dioxide crystal into the mixed solution of 3- (methacryloyloxy) propyl trimethoxy silane and butyl acetate, and reacting for 3-4 hours at 70-75 ℃ to obtain nano titanium dioxide dispersion.
Further, the tetrabutyl titanate: the mass ratio of the n-caproic acid is (5.8-6.4) to (1-1.1); in the mixed solution of 3- (methacryloyloxy) propyl trimethoxysilane and butyl acetate, the mass ratio of the 3- (methacryloyloxy) propyl trimethoxysilane is 14.8-15.6wt%; the mass ratio of the nano titanium dioxide crystal in the mixed solution of 3- (methacryloyloxy) propyl trimethoxy silane and butyl acetate is 2-4wt%.
Further, the preparation method of the graphene-polyaniline composite material comprises the following steps:
dispersing graphene oxide in deionized water by ultrasonic waves, adding a didodecyl dimethyl ammonium bromide solution, stirring uniformly, adding isophthalonitrile, stirring uniformly, standing, removing supernatant, and purifying to obtain modified graphene oxide; mixing aniline, modified graphene oxide and dodecylbenzene sulfonic acid, stirring uniformly, adding a catalyst, reacting for 2-3 hours at 45-50 ℃, performing suction filtration at room temperature, washing, and performing vacuum drying to obtain the graphene-polyaniline composite material.
Further, in the didodecyl dimethyl ammonium bromide solution, the solvent is ethanol water solution with the volume ratio of 1:1, and the concentration is 1-1.2mg/mL; graphene oxide: didodecyl dimethyl ammonium bromide solution: the mass ratio of the isophthalonitrile is (0.8-1.2): 1.
Further, the catalyst is ammonium persulfate; aniline: the mass ratio of the modified graphene oxide is (4-8) 1; the washing step is to wash the polymer after suction filtration to pH 5.0-6.0, and the vacuum drying temperature is 50-55 ℃.
Further, the methyl methacrylate: the mass ratio of the vinyltrimethylsilane is (4-7): 1.
Further, the polymethyl methacrylate: polyethylene glycol: polyvinyl butyral: the mass ratio of the nano titanium dioxide dispersion liquid is 1:0.8:1.2 (0.8-1.2).
Further, the polyvinyl butyral: the mass ratio of the graphene-polyaniline composite material is (1-1.2): 1.
Compared with the prior art, the invention has the following beneficial effects:
according to the preparation method, the graphene oxide is modified through the didodecyl dimethyl ammonium bromide, then polyaniline nanofiber is prepared through a non-hydrochloric acid method, and the modified graphene oxide is grafted on the surface of the polyaniline nanofiber; the dispersibility and compatibility of polyaniline nanofiber and graphene oxide in polyvinyl butyral are greatly improved by utilizing the long carbon chain on the surface of graphene oxide; polyaniline can be used as a metal corrosion inhibitor to effectively shield penetration of a corrosion medium, a compact passivation layer is provided for the metal surface, the requirement of polyaniline on corrosion resistance (polyaniline in an intrinsic state and in a conductive state in a middle oxidation state) is met by adding modified graphene oxide, and the modified graphene oxide is modified by using didodecyl dimethyl ammonium bromide, so that on one hand, the dispersibility and compatibility of the modified graphene oxide and polyaniline in polyvinyl butyral can be enhanced, and on the other hand, the formation of micro-couples is inhibited by using the existence of hydroxyl and carboxyl of the modified graphene oxide, and the corrosion of the micro-couples to metal caused by graphene and metal is avoided. The polyaniline nanofiber prepared by the non-hydrochloric acid method can avoid hydrochloric acid residues caused by the traditional concentrated hydrochloric acid acidification of polyaniline, and avoid the problem of corrosion of metal caused by chloride ions existing in a coating.
The invention carries out modification treatment on nano titanium dioxide through 3- (methacryloyloxy) propyl trimethoxysilane, then prepares nano titanium dioxide slurry by mixing polymethyl methacrylate, polyethylene glycol and polyvinyl butyral which are prepared by the reaction of methyl methacrylate and vinyl trimethyl silane, and is used as a first layer of wear-resistant and corrosion-resistant coating attached to the metal surface of a stainless steel nut; the dispersibility and compatibility of the nano titanium dioxide in the mixed resin can be effectively improved by utilizing siloxane to modify the nano titanium dioxide; on one hand, polyethylene glycol in polymethyl methacrylate, polyethylene glycol and polyvinyl butyral mixed resin is dissolved and removed by water, the surface of a coating forms a continuously distributed pore structure, and the fine pore structures provide penetration points for polyaniline fiber, so that the polyaniline fiber and a modified graphene oxide and nanometer titanium dioxide slurry coating are penetrated mutually to form a compact complex crosslinked network, and the wear resistance and corrosion resistance of the nut are further improved; on the other hand, the water-soluble degreasing of the nano titanium dioxide slurry coating in advance can effectively relieve the occurrence of secondary pore space caused by the water-soluble degreasing of the coating by water in the long-term use process.
Polyaniline is easy to be converted into an oxidation state under the action of external water and oxygen in a reduction state, so that the contact between metal and the external water and oxygen is reduced, and the corrosion resistance of the coating is improved; under the illumination condition, polyaniline can absorb photons to generate electron-holes, and photo-generated electrons HOMO (highest occupied molecular orbital) is transferred to LUMO (lowest unoccupied molecular orbital), so that the electron loss of metal is organized by rewinding transferred to nano titanium dioxide; meanwhile, polyaniline-graphene slurry can form a layer of passivation film on the metal surface under the catalytic coating, so that penetration of corrosive medium is further organized; the three functions are mutually cooperated, so that the wear resistance and corrosion resistance of the nut are greatly improved.
Detailed Description
The following description of the technical solutions in the embodiments of the present invention will be clear and complete, and it is obvious that the described embodiments are only some embodiments of the present invention, but not all embodiments. 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.
In the following examples, polyethylene glycol was purchased from national pharmaceutical chemicals, inc., having a molecular weight of 1500; methyl methacrylate CAS:80-62-6; vinyltrimethylsilane and CAS:754-05-2; polyvinyl butyral is purchased from Shanghai Meilin Biochemical technology Co., ltd, and has a molecular weight of 40000-70000; tetrabutyl titanate CAS:5593-70-4;3- (methacryloxy) propyl trimethoxysilane CAS:2530-85-0; butyl acetate CAS:123-86-4; didodecyl dimethyl ammonium bromide CAS:3282-73-3; graphene oxide is purchased from taiwanese chemical industry development limited; isophthalonitrile CAS:626-17-5; dodecylbenzenesulfonic acid CAS:27176-87-0; ammonium persulfate CAS:7727-54-0.
Example 1: a processing technology of a high-strength nut comprises the following steps: s1: adding 5.8g of tetrabutyl titanate and 1g of n-caproic acid into 100mL of deionized water, reacting for 3h at 240 ℃, centrifuging, washing and drying to obtain nano titanium dioxide crystals; adding 2g of nano titanium dioxide crystal into 100g of mixed solution of 3- (methacryloyloxy) propyl trimethoxy silane and butyl acetate, and reacting for 3 hours at 70 ℃ to obtain nano titanium dioxide dispersion;
s2: dispersing 0.8g of graphene oxide in 100mL of deionized water by ultrasonic, adding 0.8g of 1mg/mL of didodecyl dimethyl ammonium bromide solution, uniformly stirring, adding 1g of isophthalonitrile, uniformly stirring, standing, removing supernatant, and purifying to obtain modified graphene oxide; mixing and stirring 4g of aniline, 1g of modified graphene oxide and 1g of dodecylbenzene sulfonic acid uniformly, adding 2.5g of ammonium persulfate, reacting for 2 hours at 45 ℃, performing suction filtration at room temperature, washing, and vacuum drying to obtain a graphene-polyaniline composite material;
s3: adding 4g of methyl methacrylate, 1g of vinyl trimethylsilane and 0.25g of azodiisobutyronitrile into 100mL of tetrahydrofuran, and reacting for 4 hours at 80 ℃ in a nitrogen atmosphere to obtain polymethyl methacrylate; mixing 10g of polymethyl methacrylate, 8g of polyethylene glycol and 12g of polyvinyl butyral at 190 ℃ for 10min, adding 8g of nano titanium dioxide dispersion liquid, and continuously stirring for 10min to obtain nano titanium dioxide slurry;
s4: dissolving 1.2g of polyvinyl butyral in 20mL of methanol, adding 1g of graphene-polyaniline composite material, performing ultrasonic dispersion for 1h, and magnetically stirring for 8h to obtain graphene-polyaniline slurry; and (3) placing the stainless steel nut with the oil removed from the pretreated surface into nano titanium dioxide slurry, taking out and drying the stainless steel nut, degreasing the stainless steel nut in water at 50 ℃ for 2 hours, drying the stainless steel nut to obtain a titanium dioxide coating, coating graphene-polyaniline slurry on the surface of the titanium dioxide coating, and drying the titanium dioxide coating to obtain the high-strength nut.
Example 2: a processing technology of a high-strength nut comprises the following steps: s1: adding 6g of tetrabutyl titanate and 1.1g of n-caproic acid into 100mL of deionized water, reacting for 3h at 240 ℃, centrifuging, washing and drying to obtain nano titanium dioxide crystals; adding 3g of nano titanium dioxide crystal into 100g of mixed solution of 3- (methacryloyloxy) propyl trimethoxy silane and butyl acetate, and reacting for 3h at 70 ℃ to obtain nano titanium dioxide dispersion;
s2: dispersing 1g of graphene oxide in 100mL of deionized water by ultrasonic, adding 1g of 1mg/mL of didodecyl dimethyl ammonium bromide solution, stirring uniformly, adding 1g of isophthalonitrile, stirring uniformly, standing, removing supernatant, and purifying to obtain modified graphene oxide; mixing and stirring 8g of aniline, 1g of modified graphene oxide and 1g of dodecylbenzene sulfonic acid uniformly, adding 2.5g of ammonium persulfate, reacting for 2 hours at 45 ℃, performing suction filtration at room temperature, washing, and vacuum drying to obtain a graphene-polyaniline composite material;
s3: 6g of methyl methacrylate, 1g of vinyl trimethylsilane and 0.25g of azobisisobutyronitrile are added into 100mL of tetrahydrofuran, and the mixture is reacted for 4 hours at 80 ℃ under the nitrogen atmosphere to obtain polymethyl methacrylate; mixing 10g of polymethyl methacrylate, 8g of polyethylene glycol and 12g of polyvinyl butyral at 190 ℃ for 10min, adding 10g of nano titanium dioxide dispersion liquid, and continuously stirring for 15min to obtain nano titanium dioxide slurry;
s4: dissolving 1.1g of polyvinyl butyral in 20mL of methanol, adding 1g of graphene-polyaniline composite material, performing ultrasonic dispersion for 1h, and magnetically stirring for 8h to obtain graphene-polyaniline slurry; and (3) placing the stainless steel nut with the oil removed from the pretreated surface into nano titanium dioxide slurry, taking out and drying the stainless steel nut, degreasing the stainless steel nut in water at 50 ℃ for 2 hours, drying the stainless steel nut to obtain a titanium dioxide coating, coating graphene-polyaniline slurry on the surface of the titanium dioxide coating, and drying the titanium dioxide coating to obtain the high-strength nut.
Example 3: a processing technology of a high-strength nut comprises the following steps: s1: adding 6.4g of tetrabutyl titanate and 1.1g of n-caproic acid into 100mL of ionized water, reacting for 3h at 240 ℃, centrifuging, washing and drying to obtain nano titanium dioxide crystals; adding 4g of nano titanium dioxide crystal into 100g of mixed solution of 3- (methacryloyloxy) propyl trimethoxy silane and butyl acetate, and reacting for 3 hours at 70 ℃ to obtain nano titanium dioxide dispersion;
s2: dispersing 1.2g of graphene oxide in 100mL of deionized water by ultrasonic, adding 1.2g of 1mg/mL of didodecyl dimethyl ammonium bromide solution, uniformly stirring, adding 1g of isophthalonitrile, uniformly stirring, standing, removing supernatant, and purifying to obtain modified graphene oxide; mixing and stirring 6g of aniline, 1g of modified graphene oxide and 1g of dodecylbenzene sulfonic acid uniformly, adding 2.5g of ammonium persulfate, reacting for 2 hours at 45 ℃, performing suction filtration at room temperature, washing, and vacuum drying to obtain a graphene-polyaniline composite material;
s3: 7g of methyl methacrylate, 1g of vinyl trimethylsilane and 0.25g of azobisisobutyronitrile are added into 100mL of tetrahydrofuran, and the mixture is reacted for 4 hours at 80 ℃ under the nitrogen atmosphere to obtain polymethyl methacrylate; mixing 10g of polymethyl methacrylate, 8g of polyethylene glycol and 12g of polyvinyl butyral at 190 ℃ for 10min, adding 12g of nano titanium dioxide dispersion liquid, and continuously stirring for 15min to obtain nano titanium dioxide slurry;
s4: dissolving 1g of polyvinyl butyral in 20mL of methanol, adding 1g of graphene-polyaniline composite material, performing ultrasonic dispersion for 1h, and magnetically stirring for 8h to obtain graphene-polyaniline slurry; and (3) placing the stainless steel nut with the oil removed from the pretreated surface into nano titanium dioxide slurry, taking out and drying the stainless steel nut, degreasing the stainless steel nut in water at 50 ℃ for 2 hours, drying the stainless steel nut to obtain a titanium dioxide coating, coating graphene-polyaniline slurry on the surface of the titanium dioxide coating, and drying the titanium dioxide coating to obtain the high-strength nut.
Comparative example 1: a processing technology of a high-strength nut comprises the following steps: s2: dispersing 1.2g of graphene oxide in 100mL of deionized water by ultrasonic, adding 1.2g of 1mg/mL of didodecyl dimethyl ammonium bromide solution, uniformly stirring, adding 1g of isophthalonitrile, uniformly stirring, standing, removing supernatant, and purifying to obtain modified graphene oxide; adding 1g of modified graphene oxide into 150mL of 1mol/L hydrochloric acid, adding 1g of aniline, stirring for 1h, performing ultrasonic dispersion for 1h, adding 2.4g of ammonium persulfate and 20mL of 1mol/L hydrochloric acid, stirring for 4h under ice bath, filtering, washing and drying to obtain a graphene-polyaniline composite material;
the remaining steps were the same as in example 1.
Comparative example 2: a processing technology of a high-strength nut comprises the following steps: s2: adding 1g of graphene oxide into 150mL of 1mol/L hydrochloric acid, adding 1g of aniline, stirring for 1h, performing ultrasonic dispersion for 1h, adding 2.4g of ammonium persulfate and 20mL of 1mol/L hydrochloric acid, stirring for 4h under ice bath, filtering, washing and drying to obtain a graphene-polyaniline composite material;
the remaining steps were the same as in example 1.
Comparative example 3: a processing technology of a high-strength nut comprises the following steps: s1: adding 5.8g of tetrabutyl titanate and 1g of n-caproic acid into 100mL of deionized water, reacting for 3h at 240 ℃, centrifuging, washing and drying to obtain nano titanium dioxide crystals; adding 2g of nano titanium dioxide crystal into 100g of mixed solution of 3- (methacryloyloxy) propyl trimethoxy silane and butyl acetate, and reacting for 3 hours at 70 ℃ to obtain nano titanium dioxide dispersion;
s2: dispersing 0.8g of graphene oxide in 100mL of deionized water by ultrasonic, adding 0.8g of 1mg/mL of didodecyl dimethyl ammonium bromide solution, uniformly stirring, adding 1g of isophthalonitrile, uniformly stirring, standing, removing supernatant, and purifying to obtain modified graphene oxide; mixing and stirring 4g of aniline, 1g of modified graphene oxide and 1g of dodecylbenzene sulfonic acid uniformly, adding 2.5g of ammonium persulfate, reacting for 2 hours at 45 ℃, performing suction filtration at room temperature, washing, and vacuum drying to obtain a graphene-polyaniline composite material;
s3: adding 4g of methyl methacrylate, 1g of vinyl trimethylsilane and 0.25g of azodiisobutyronitrile into 100mL of tetrahydrofuran, and reacting for 4 hours at 80 ℃ in a nitrogen atmosphere to obtain polymethyl methacrylate; mixing 10g of polymethyl methacrylate, 8g of polyethylene glycol and 12g of polyvinyl butyral at 190 ℃ for 10min, adding 8g of nano titanium dioxide dispersion liquid, and continuously stirring for 10min to obtain nano titanium dioxide slurry;
s4: dissolving 1.2g of polyvinyl butyral in 20mL of methanol, adding 1g of graphene-polyaniline composite material, performing ultrasonic dispersion for 1h, and magnetically stirring for 8h to obtain graphene-polyaniline slurry; placing the stainless steel nut with the oil removed on the pretreated surface into nano titanium dioxide slurry, taking out and drying to obtain a titanium dioxide coating, coating graphene-polyaniline slurry on the surface of the titanium dioxide coating, and drying to obtain a high-strength nut;
comparative example 4: a processing technology of a high-strength nut comprises the following steps: s1: dispersing 0.8g of graphene oxide in 100mL of deionized water by ultrasonic, adding 0.8g of 1mg/mL of didodecyl dimethyl ammonium bromide solution, uniformly stirring, adding 1g of isophthalonitrile, uniformly stirring, standing, removing supernatant, and purifying to obtain modified graphene oxide; mixing and stirring 4g of aniline, 1g of modified graphene oxide and 1g of dodecylbenzene sulfonic acid uniformly, adding 2.5g of ammonium persulfate, reacting for 2 hours at 45 ℃, performing suction filtration at room temperature, washing, and vacuum drying to obtain a graphene-polyaniline composite material;
s2: adding 4g of methyl methacrylate, 1g of vinyl trimethylsilane and 0.25g of azodiisobutyronitrile into 100mL of tetrahydrofuran, and reacting for 4 hours at 80 ℃ in a nitrogen atmosphere to obtain polymethyl methacrylate; mixing 10g of polymethyl methacrylate, 8g of polyethylene glycol and 12g of polyvinyl butyral at 190 ℃ for 10min, adding 8g of nano titanium dioxide, and continuously stirring for 10min to obtain nano titanium dioxide slurry;
s3: dissolving 1.2g of polyvinyl butyral in 20mL of methanol, adding 1g of graphene-polyaniline composite material, performing ultrasonic dispersion for 1h, and magnetically stirring for 8h to obtain graphene-polyaniline slurry; and (3) placing the stainless steel nut with the oil removed from the pretreated surface into nano titanium dioxide slurry, taking out and drying the stainless steel nut, degreasing the stainless steel nut in water at 50 ℃ for 2 hours, drying the stainless steel nut to obtain a titanium dioxide coating, coating graphene-polyaniline slurry on the surface of the titanium dioxide coating, and drying the titanium dioxide coating to obtain the high-strength nut.
And (3) testing: the surface life Gong Dao of the high strength nuts prepared in examples and comparative examples was uniformly marked with an "X" mark according to ASTM-D1654 scratch test standard, and the scratched sample was immersed in 3.5wt% NaCl solution for 72 hours to observe the corrosion morphology at the scratch.
Conclusion: the high-strength nuts prepared in examples 1-3 have complete surface coatings and no corrosion and coating falling off. Comparative example 1 polyaniline was prepared by acidification with concentrated hydrochloric acid, the scratch of the coating was corroded, and the coating was partially peeled off; comparative example 2 polyaniline was prepared by acidification with concentrated hydrochloric acid without modification of graphene oxide, and the scratch of the coating was severely corroded and the coating was peeled off; comparative example 3 did not undergo water-soluble degreasing, the scratch was slightly corroded, and the coating did not fall off; comparative example 4 the nano titanium dioxide was not modified, the scratch was partially corroded, and the coating was slightly peeled off.
Finally, it should be noted that: the foregoing description is only a preferred embodiment of the present invention, and the present invention is not limited thereto, but it is to be understood that modifications and equivalents of some of the technical features described in the foregoing embodiments may be made by those skilled in the art, although the present invention has been described in detail with reference to the foregoing embodiments. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (7)
1. A processing technology of a high-strength nut is characterized in that: the method comprises the following steps:
s1: adding methyl methacrylate, vinyl trimethylsilane and azodiisobutyronitrile into tetrahydrofuran, and reacting for 4-5 hours at 80-85 ℃ in nitrogen atmosphere to obtain polymethyl methacrylate; mixing polymethyl methacrylate, polyethylene glycol and polyvinyl butyral at 190-195 ℃ for 10-15min, adding nano titanium dioxide dispersion liquid, and continuously stirring for 10-15min to obtain nano titanium dioxide slurry;
s2: dissolving polyvinyl butyral in methanol, adding a graphene-polyaniline composite material, performing ultrasonic dispersion for 1-1.5h, and magnetically stirring for 8-12h to obtain graphene-polyaniline slurry; placing the pretreated stainless steel nut into nano titanium dioxide slurry, taking out and drying, degreasing in water at 50-55 ℃ for 2-2.5h, drying to obtain a titanium dioxide coating, coating graphene-polyaniline slurry on the surface of the titanium dioxide coating, and drying to obtain a high-strength nut;
the preparation method of the nano titanium dioxide dispersion liquid comprises the following steps:
adding tetrabutyl titanate and n-caproic acid into deionized water, reacting for 3-3.5h at 240-250 ℃, centrifuging, washing and drying to obtain nano titanium dioxide crystals; adding nano titanium dioxide crystals into a mixed solution of 3- (methacryloyloxy) propyl trimethoxy silane and butyl acetate, and reacting for 3-4 hours at 70-75 ℃ to obtain nano titanium dioxide dispersion;
the preparation method of the graphene-polyaniline composite material comprises the following steps:
dispersing graphene oxide in deionized water by ultrasonic waves, adding a didodecyl dimethyl ammonium bromide solution, stirring uniformly, adding isophthalonitrile, stirring uniformly, standing, removing supernatant, and purifying to obtain modified graphene oxide; mixing aniline, modified graphene oxide and dodecylbenzene sulfonic acid, uniformly stirring, adding a catalyst, reacting for 2-3 hours at 45-50 ℃, performing suction filtration at room temperature, washing, and performing vacuum drying to obtain a graphene-polyaniline composite material;
the catalyst is ammonium persulfate; aniline: the mass ratio of the modified graphene oxide is (4-8) 1; in the graphene-polyaniline composite material, the washing step is to wash the polymer subjected to suction filtration until the pH value is 5.0-6.0, and the vacuum drying temperature is 50-55 ℃.
2. The process for manufacturing a high strength nut according to claim 1, wherein: tetrabutyl titanate: the mass ratio of the n-caproic acid is (5.8-6.4) to (1-1.1).
3. The process for manufacturing a high strength nut according to claim 1, wherein: in the mixed solution of 3- (methacryloyloxy) propyl trimethoxysilane and butyl acetate, the mass ratio of the 3- (methacryloyloxy) propyl trimethoxysilane is 14.8-15.6wt%; the mass ratio of the nano titanium dioxide crystal in the mixed solution of 3- (methacryloyloxy) propyl trimethoxy silane and butyl acetate is 2-4wt%.
4. The process for manufacturing a high strength nut according to claim 1, wherein: in the didodecyl dimethyl ammonium bromide solution, the solvent is ethanol water solution with the volume ratio of 1:1, and the concentration is 1-1.2mg/mL; graphene oxide: didodecyl dimethyl ammonium bromide solution: the mass ratio of the isophthalonitrile is (0.8-1.2): 1.
5. The process for manufacturing a high strength nut according to claim 1, wherein: the methyl methacrylate: the mass ratio of the vinyltrimethylsilane is (4-7): 1.
6. The process for manufacturing a high strength nut according to claim 1, wherein: polymethyl methacrylate: polyethylene glycol: polyvinyl butyral: the mass ratio of the nano titanium dioxide dispersion liquid is 1:0.8:1.2 (0.8-1.2).
7. The process for manufacturing a high strength nut according to claim 1, wherein: polyvinyl butyral: the mass ratio of the graphene-polyaniline composite material is (1-1.2): 1.
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