Preparation process of pre-warning anti-loose bolt

Abstract

The application discloses a preparation process of a pre-warning anti-loose bolt, and relates to the technical field of bolts.The anti-corrosion sheath containing a polyamide composite material is coated on the outer side of the bolt base body through an injection molding process, so that the corrosion resistance of the bolt is improved.The furan-2,5-diketone is used to modify the graphene oxide, and a maleimide modified graphene oxide is obtained.The maleimide has the characteristics of being sensitive to ultraviolet light, and can react with styrene and methyl methacrylate under ultraviolet light, so that the vinyl graphene oxide is obtained.Then, the polyamide modified glass fiber is added, so that the corrosion resistance of the bolt is further improved.

Description

Technical Field

[0001] The invention relates to the technical field of bolts, and in particular to a preparation process of early warning anti-loosening bolts. Background Art

[0002] Bolts are one of the most commonly used fasteners in mechanical structures and are widely used in various fields, including automotive, construction, and aerospace. The Early Warning Anti-Loosening Bolt combines intelligent materials that can sense external factors such as stress, temperature, and vibration with traditional bolt fasteners to create a self-monitoring bolt system. When a bolt shows signs of loosening during use, the material responds by generating a signal or changing its behavior, alerting maintenance personnel to conduct inspection and maintenance.

[0003] Therefore, preventing bolt loosening is an important part of ensuring the safety of mechanical equipment and structures. However, traditional bolts can loosen over time due to factors such as vibration, mechanical stress, and corrosion, leading to unstable connections, component failure, and even serious accidents.

[0004] In order to solve the above problems and improve the corrosion resistance of bolts, the present invention provides a preparation process of early warning anti-loosening bolts. Summary of the Invention

[0005] The purpose of the present invention is to provide a preparation process of a warning anti-loosening bolt to solve the problems raised in the prior art.

[0006] To achieve the above object, the present invention provides the following technical solutions:

[0007] A preparation process for an early warning anti-loosening bolt comprises the following steps:

[0008] Step 1: Take nylon resin and polytetrafluoroethylene powder, stir them evenly, add graphene oxide-glass fiber composite, melt extrude and granulate to obtain polyamide composite material;

[0009] Step 2: taking a polyamide composite material, a silane coupling agent, and an antioxidant, and mixing them evenly to obtain an anti-corrosion mixture;

[0010] Step 3: Take Fe, Mn, Ni, Si, Ge, C, Ag, Bi, and La, melt, pour, forge, and heat treat to obtain a bolt matrix;

[0011] Step 4: Place the bolt base in a mold, add the anti-corrosion mixture into an injection molding machine, perform injection molding, overmolding, take out, and dry to obtain a warning anti-loosening bolt.

[0012] More optimally, the anti-corrosion mixture is composed of the following substances, calculated by weight: 50-60 parts of polyamide composite material, 4-6 parts of silane coupling agent, and 2-3 parts of antioxidant.

[0013] More optimally, the preparation method of the graphene oxide-glass fiber composite is: take maleimide-modified graphene oxide and N,N-dimethylformamide, ultrasonically disperse them, add styrene and methyl methacrylate under an argon environment, and irradiate them under ultraviolet light for 50-70 minutes, add polyamide-modified glass fiber, stir evenly, irradiate them under ultraviolet light for 50-70 minutes, wash, and dry to obtain the graphene oxide-glass fiber composite.

[0014] More optimally, the preparation method of the polyamide-modified glass fiber is: take deionized water and an emulsifier, stir evenly to obtain a mixed solution; take polyhexamethylene adipamide, thioglycolic acid, and dimethyl sulfoxide, stir evenly, add the mixed solution, and stir for 2-3 hours to obtain a polyhexamethylene adipamide mixed solution; take glass fiber, immerse it in the polyhexamethylene adipamide mixed solution for 20-30 minutes, take it out, and dry it to obtain polyamide-modified glass fiber.

[0015] More optimally, the preparation method of the maleimide-modified graphene oxide is as follows: sodium acetate and deionized water are taken and stirred evenly to obtain a sodium acetate solution; amino-modified graphene oxide, furan-2,5-dione, and chlorobenzene are taken and ultrasonically dispersed for 10-15 minutes, heated to 130-135°C under nitrogen, refluxed for 2-4 hours, cooled to 25-30°C, added with sodium acetate solution, heated to 130-135°C under nitrogen, reacted for 50-70 minutes, cooled to 25-30°C, centrifuged, washed, and dried to obtain maleimide-modified graphene oxide.

[0016] More optimally, the preparation method of the amino-modified graphene oxide is: taking graphene oxide, γ-aminopropyltriethoxysilane, and sodium carbonate, centrifuging, precipitating, washing, and drying at 80-85° C. for 46-50 hours to obtain the amino-modified graphene oxide.

[0017] More optimally, the bolt includes the following components, in percentage by mass: 3.0wt%-4.0wt% Mn, 1.5wt%-2.5wt% Ni, 0.4wt%-0.7wt% Si, 0.01wt%-0.04wt% Ge, 0.3wt%-0.4wt% C, 0.01wt%-0.03wt% Ag, 0.008wt%-0.01wt% Bi, 0.001wt%-0.002wt% La, and the balance is Fe and other inevitable impurities.

[0018] More optimally, the antioxidant is any one or more of antioxidant 1010, antioxidant 164, and antioxidant 1076.

[0019] More optimally, the silane coupling agent is KH550.

[0020] Compared with the prior art, the present invention has the following beneficial effects:

[0021] 1. The present invention coats the outer side of the bolt base with an anti-corrosion sheath containing a polyamide composite material through an injection molding process, thereby achieving the effect of improving the corrosion resistance of the bolt.

[0022] 2. The present invention uses furan-2,5-dione to modify amino-modified graphene oxide to obtain a maleimide-modified graphene oxide. Maleimide is sensitive to ultraviolet light and can react with styrene and methyl methacrylate under ultraviolet light to obtain vinyl graphene oxide. Polyamide-modified glass fiber is then added, stirred evenly, and illuminated under a 365nm ultraviolet lamp to allow the thiol group on the polyamide-modified glass fiber to react with the vinyl group, thereby allowing the vinyl graphene oxide and the polyamide-modified glass fiber to be better composited together, thereby improving the corrosion resistance of the bolt.

[0023] 3. The present invention uses polyamide to modify the glass fiber, so that the graphene oxide-glass fiber composite has good dispersion in the polyamide composite matrix, thereby further improving the corrosion resistance of the bolt. DETAILED DESCRIPTION

[0024] The following is a clear and complete description of the technical solutions in the embodiments of the present invention. Obviously, the embodiments described are only some embodiments of the present invention, not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without making any creative efforts are within the scope of protection of the present invention.

[0025] The raw materials involved in the present invention are derived from models without any specific restrictions, and illustratively include: graphene oxide: model: 796034, which can be purchased from Merck; polyhexamethylene adipamide: model: 132F, which can be purchased from DuPont in the United States; glass fiber: model: S30527, which can be purchased from Shanghai Yuanye Biotechnology Co., Ltd.; nylon resin: model: 1252, which can be purchased from Qingdao Sanli Benno New Materials Co., Ltd.; polytetrafluoroethylene micropowder: model: MP1200, which can be purchased from DuPont in the United States.

[0026] Example 1: A preparation process for a warning anti-loosening bolt, comprising the following steps:

[0027] Step 1: Preparation of polyamide modified glass fiber:

[0028] 300 mL of deionized water and 2 g of emulsifier O-20 were mixed and stirred to obtain a mixed solution; 45 g of polyhexamethylene adipamide, 3 g of thioglycolic acid, and 100 mL of dimethyl sulfoxide were mixed and stirred to obtain a polyhexamethylene adipamide mixed solution; glass fiber was immersed in the polyhexamethylene adipamide mixed solution for 25 min, removed, and dried to obtain a polyamide-modified glass fiber;

[0029] Step 2: Preparation of maleimide-modified graphene oxide:

[0030] Take 0.1 g of graphene oxide, 30 mL of γ-aminopropyltriethoxysilane, and 200 mg of sodium carbonate, incubate at 82°C for 48 h, centrifuge, precipitate, wash, and dry to obtain amino-modified graphene oxide;

[0031] Take 0.2 g of sodium acetate and 10 mL of deionized water, stir evenly to obtain a sodium acetate solution; take 0.1 g of amino-modified graphene oxide, 2 g of furan-2,5-dione, and 30 mL of chlorobenzene, ultrasonically disperse for 12 minutes, heat to 132°C under nitrogen, reflux for 3 hours, cool to 28°C, add 10 mL of sodium acetate solution, heat to 132°C under nitrogen, react for 60 minutes, cool to 27°C, centrifuge, wash, and dry to obtain maleimide-modified graphene oxide;

[0032] Step 3: Preparation of graphene oxide-glass fiber composite:

[0033] Take 0.1g of maleimide-modified graphene oxide and 3mL of N,N-dimethylformamide, ultrasonically disperse them, add 0.3g of styrene and 0.6g of methyl methacrylate under argon environment, and irradiate under 365nm ultraviolet lamp for 60min. Add 3g of polyamide-modified glass fiber, stir evenly, irradiate under 365nm ultraviolet lamp for 60min, wash and dry to obtain graphene oxide-glass fiber composite;

[0034] Step 4: Preparation of polyamide composite material:

[0035] 100 g of nylon resin and 22 g of polytetrafluoroethylene powder were mixed evenly, and 20 g of graphene oxide-glass fiber composite was added, melt-extruded, and granulated to obtain a polyamide composite material;

[0036] Step 5: Preparation of antiseptic mixture:

[0037] Take polyamide composite material, silane coupling agent KH550, and antioxidant, mix them evenly to obtain anti-corrosion mixture;

[0038] Step 6: Preparation of early warning anti-loosening bolts:

[0039] Fe, Mn, Ni, Si, Ge, C, Ag, Bi, and La are melted, poured, forged, and heat-treated to obtain a bolt matrix;

[0040] The bolt comprises the following components, calculated by mass percentage: 3.5 wt% Mn, 1.9 wt% Ni, 0.6 wt% Si, 0.03 wt% Ge, 0.35 wt% C, 0.02 wt% Ag, 0.009 wt% Bi, 0.0015 wt% La, and the balance being Fe and other unavoidable impurities;

[0041] The bolt base is placed in a mold, the anti-corrosion mixture is added to the injection molding machine, injection molding, overmolding, removal, drying, and obtaining a warning anti-loosening bolt;

[0042] The anti-corrosion mixture is composed of the following substances, calculated by weight: 55 parts of polyamide composite material, 5 parts of silane coupling agent KH550, and 2.5 parts of antioxidant 1010.

[0043] Example 2: A preparation process for a warning anti-loosening bolt, comprising the following steps:

[0044] Step 1: Preparation of polyamide modified glass fiber:

[0045] 300 mL of deionized water and 2 g of emulsifier O-20 were mixed and stirred to obtain a mixed solution; 45 g of polyhexamethylene adipamide, 3 g of thioglycolic acid, and 100 mL of dimethyl sulfoxide were mixed and stirred to obtain a polyhexamethylene adipamide mixed solution; glass fiber was immersed in the polyhexamethylene adipamide mixed solution for 20 min, removed, and dried to obtain a polyamide-modified glass fiber;

[0046] Step 2: Preparation of maleimide-modified graphene oxide:

[0047] Take 0.1 g of graphene oxide, 30 mL of γ-aminopropyltriethoxysilane, and 200 mg of sodium carbonate, incubate at 80°C for 46 h, centrifuge, precipitate, wash, and dry to obtain amino-modified graphene oxide;

[0048] Take 0.2 g of sodium acetate and 10 mL of deionized water, stir evenly to obtain a sodium acetate solution; take 0.1 g of amino-modified graphene oxide, 2 g of furan-2,5-dione, and 30 mL of chlorobenzene, ultrasonically disperse for 10 minutes, heat to 130°C under nitrogen, reflux for 2 hours, cool to 25°C, add 10 mL of sodium acetate solution, heat to 130°C under nitrogen, react for 50 minutes, cool to 25°C, centrifuge, wash, and dry to obtain maleimide-modified graphene oxide;

[0049] Step 3: Preparation of graphene oxide-glass fiber composite:

[0050] Take 0.1g of maleimide-modified graphene oxide and 3mL of N,N-dimethylformamide, ultrasonically disperse them, add 0.3g of styrene and 0.6g of methyl methacrylate under argon environment, and irradiate under 365nm ultraviolet lamp for 50min. Add 3g of polyamide-modified glass fiber, stir evenly, irradiate under 365nm ultraviolet lamp for 50min, wash and dry to obtain graphene oxide-glass fiber composite;

[0051] Step 4: Preparation of polyamide composite material:

[0052] 100 g of nylon resin and 22 g of polytetrafluoroethylene powder were mixed evenly, and 20 g of graphene oxide-glass fiber composite was added, melt-extruded, and granulated to obtain a polyamide composite material;

[0053] Step 5: Preparation of antiseptic mixture:

[0054] Take polyamide composite material, silane coupling agent KH550, and antioxidant, mix them evenly to obtain anti-corrosion mixture;

[0055] Step 6: Preparation of early warning anti-loosening bolts:

[0056] Fe, Mn, Ni, Si, Ge, C, Ag, Bi, and La are melted, poured, forged, and heat-treated to obtain a bolt matrix;

[0057] The bolt comprises the following components, calculated by mass percentage: 3.0 wt% Mn, 1.5 wt% Ni, 0.4 wt% Si, 0.01 wt% Ge, 0.3 wt% C, 0.01 wt% Ag, 0.008 wt% Bi, 0.001 wt% La, and the balance being Fe and other unavoidable impurities;

[0058] The bolt base is placed in a mold, the anti-corrosion mixture is added to the injection molding machine, injection molding, overmolding, removal, drying, and obtaining a warning anti-loosening bolt;

[0059] The anti-corrosion mixture is composed of the following substances, calculated by weight: 50 parts of polyamide composite material, 4 parts of silane coupling agent KH550, and 2 parts of antioxidant 164.

[0060] Example 3: A preparation process for a warning anti-loosening bolt, comprising the following steps:

[0061] Step 1: Preparation of polyamide modified glass fiber:

[0062] 300 mL of deionized water and 2 g of emulsifier O-20 were mixed and stirred to obtain a mixed solution; 45 g of polyhexamethylene adipamide, 3 g of thioglycolic acid, and 100 mL of dimethyl sulfoxide were mixed and stirred to obtain a polyhexamethylene adipamide mixed solution; glass fiber was immersed in the polyhexamethylene adipamide mixed solution for 30 min, removed, and dried to obtain a polyamide-modified glass fiber;

[0063] Step 2: Preparation of maleimide-modified graphene oxide:

[0064] Take 0.1 g of graphene oxide, 30 mL of γ-aminopropyltriethoxysilane, and 200 mg of sodium carbonate, incubate at 85°C for 50 h, centrifuge, precipitate, wash, and dry to obtain amino-modified graphene oxide;

[0065] Take 0.2 g of sodium acetate and 10 mL of deionized water, stir evenly to obtain a sodium acetate solution; take 0.1 g of amino-modified graphene oxide, 2 g of furan-2,5-dione, and 30 mL of chlorobenzene, ultrasonically disperse for 15 minutes, heat to 135°C under nitrogen, reflux for 4 hours, cool to 30°C, add 10 mL of sodium acetate solution, heat to 135°C under nitrogen, react for 70 minutes, cool to 30°C, centrifuge, wash, and dry to obtain maleimide-modified graphene oxide;

[0066] Step 3: Preparation of graphene oxide-glass fiber composite:

[0067] Take 0.1g of maleimide-modified graphene oxide and 3mL of N,N-dimethylformamide, ultrasonically disperse them, add 0.3g of styrene and 0.6g of methyl methacrylate under argon environment, and irradiate under 365nm ultraviolet lamp for 70min. Add 3g of polyamide-modified glass fiber, stir evenly, irradiate under 365nm ultraviolet lamp for 70min, wash and dry to obtain graphene oxide-glass fiber composite;

[0068] Step 4: Preparation of polyamide composite material:

[0069] 100 g of nylon resin and 22 g of polytetrafluoroethylene powder were mixed evenly, and 20 g of graphene oxide-glass fiber composite was added, melt-extruded, and granulated to obtain a polyamide composite material;

[0070] Step 5: Preparation of antiseptic mixture:

[0071] Take polyamide composite material, silane coupling agent KH550, and antioxidant, mix them evenly to obtain anti-corrosion mixture;

[0072] Step 6: Preparation of early warning anti-loosening bolts:

[0073] Fe, Mn, Ni, Si, Ge, C, Ag, Bi, and La are melted, poured, forged, and heat-treated to obtain a bolt matrix;

[0074] The bolt comprises the following components, calculated by mass percentage: 4.0 wt% Mn, 2.5 wt% Ni, 0.7 wt% Si, 0.04 wt% Ge, 0.4 wt% C, 0.03 wt% Ag, 0.01 wt% Bi, 0.002 wt% La, and the balance being Fe and other unavoidable impurities;

[0075] The bolt base is placed in a mold, the anti-corrosion mixture is added to the injection molding machine, injection molding, overmolding, removal, drying, and obtaining a warning anti-loosening bolt;

[0076] The anti-corrosion mixture is composed of the following substances, calculated by weight: 60 parts of polyamide composite material, 6 parts of silane coupling agent KH550, and 3 parts of antioxidant 1076.

[0077] Comparative Example 1: No thioglycolic acid was added to the polyamide modified glass fiber, and the rest was the same as in Example 1:

[0078] Step 1: Preparation of polyamide modified glass fiber:

[0079] 300 mL of deionized water and 2 g of emulsifier O-20 were mixed and stirred to obtain a mixed solution; 45 g of polyhexamethylene adipamide and 100 mL of dimethyl sulfoxide were mixed and stirred to obtain a mixed solution of polyhexamethylene adipamide; glass fiber was immersed in the mixed solution of polyhexamethylene adipamide for 25 min, removed and dried to obtain polyamide-modified glass fiber;

[0080] Step 2: Preparation of maleimide-modified graphene oxide:

[0081] Take 0.1 g of graphene oxide, 30 mL of γ-aminopropyltriethoxysilane, and 200 mg of sodium carbonate, incubate at 82°C for 48 h, centrifuge, precipitate, wash, and dry to obtain amino-modified graphene oxide;

[0082] Take 0.2 g of sodium acetate and 10 mL of deionized water, stir evenly to obtain a sodium acetate solution; take 0.1 g of amino-modified graphene oxide, 2 g of furan-2,5-dione, and 30 mL of chlorobenzene, ultrasonically disperse for 12 minutes, heat to 132°C under nitrogen, reflux for 3 hours, cool to 28°C, add 10 mL of sodium acetate solution, heat to 132°C under nitrogen, react for 60 minutes, cool to 27°C, centrifuge, wash, and dry to obtain maleimide-modified graphene oxide;

[0083] Step 3: Preparation of graphene oxide-glass fiber composite:

[0084] Take 0.1g of maleimide-modified graphene oxide and 3mL of N,N-dimethylformamide, ultrasonically disperse them, add 0.3g of styrene and 0.6g of methyl methacrylate under argon environment, and irradiate under 365nm ultraviolet lamp for 60min. Add 3g of polyamide-modified glass fiber, stir evenly, irradiate under 365nm ultraviolet lamp for 60min, wash and dry to obtain graphene oxide-glass fiber composite;

[0085] Step 4: Preparation of polyamide composite material:

[0086] 100 g of nylon resin and 22 g of polytetrafluoroethylene powder were mixed evenly, and 20 g of graphene oxide-glass fiber composite was added, melt-extruded, and granulated to obtain a polyamide composite material;

[0087] Step 5: Preparation of antiseptic mixture:

[0088] Take polyamide composite material, silane coupling agent KH550, and antioxidant, mix them evenly to obtain anti-corrosion mixture;

[0089] Step 6: Preparation of early warning anti-loosening bolts:

[0090] Fe, Mn, Ni, Si, Ge, C, Ag, Bi, and La are melted, poured, forged, and heat-treated to obtain a bolt matrix;

[0091] The bolt comprises the following components, calculated by mass percentage: 3.5 wt% Mn, 1.9 wt% Ni, 0.6 wt% Si, 0.03 wt% Ge, 0.35 wt% C, 0.02 wt% Ag, 0.009 wt% Bi, 0.0015 wt% La, and the balance being Fe and other unavoidable impurities;

[0092] The bolt base is placed in a mold, the anti-corrosion mixture is added to the injection molding machine, injection molding, overmolding, removal, drying, and obtaining a warning anti-loosening bolt;

[0093] The anti-corrosion mixture is composed of the following substances, calculated by weight: 55 parts of polyamide composite material, 5 parts of silane coupling agent KH550, and 2.5 parts of antioxidant 1010.

[0094] Comparative Example 2: No glass fiber was added, and the rest was the same as Example 1:

[0095] Step 1: Preparation of maleimide-modified graphene oxide:

[0096] Take 0.1 g of graphene oxide, 30 mL of γ-aminopropyltriethoxysilane, and 200 mg of sodium carbonate, incubate at 82°C for 48 h, centrifuge, precipitate, wash, and dry to obtain amino-modified graphene oxide;

[0097] Take 0.2 g of sodium acetate and 10 mL of deionized water, stir evenly to obtain a sodium acetate solution; take 0.1 g of amino-modified graphene oxide, 2 g of furan-2,5-dione, and 30 mL of chlorobenzene, ultrasonically disperse for 12 minutes, heat to 132°C under nitrogen, reflux for 3 hours, cool to 28°C, add 10 mL of sodium acetate solution, heat to 132°C under nitrogen, react for 60 minutes, cool to 27°C, centrifuge, wash, and dry to obtain maleimide-modified graphene oxide;

[0098] Step 2: Preparation of vinyl graphene oxide:

[0099] 0.1 g of maleimide-modified graphene oxide and 3 mL of N,N-dimethylformamide were ultrasonically dispersed. 0.3 g of styrene and 0.6 g of methyl methacrylate were added under an argon atmosphere. The mixture was irradiated under a 365 nm ultraviolet lamp for 60 min, washed, and dried to obtain vinyl graphene oxide.

[0100] Step 3: Preparation of polyamide composite material:

[0101] 100 g of nylon resin and 22 g of polytetrafluoroethylene powder were mixed evenly, and 20 g of vinyl graphene oxide was added, melt-extruded, and granulated to obtain a polyamide composite material;

[0102] Step 4: Preparation of antiseptic mixture:

[0103] Take polyamide composite material, silane coupling agent KH550, and antioxidant, mix them evenly to obtain anti-corrosion mixture;

[0104] Step 5: Preparation of early warning anti-loosening bolts:

[0105] Fe, Mn, Ni, Si, Ge, C, Ag, Bi, and La are melted, poured, forged, and heat-treated to obtain a bolt matrix;

[0106] The bolt comprises the following components, calculated by mass percentage: 3.5 wt% Mn, 1.9 wt% Ni, 0.6 wt% Si, 0.03 wt% Ge, 0.35 wt% C, 0.02 wt% Ag, 0.009 wt% Bi, 0.0015 wt% La, and the balance being Fe and other unavoidable impurities;

[0107] The bolt base is placed in a mold, the anti-corrosion mixture is added to the injection molding machine, injection molding, overmolding, removal, drying, and obtaining a warning anti-loosening bolt;

[0108] The anti-corrosion mixture is composed of the following substances, calculated by weight: 55 parts of polyamide composite material, 5 parts of silane coupling agent KH550, and 2.5 parts of antioxidant 1010.

[0109] Comparative Example 3: The glass fiber is not modified with polyamide, and the rest is the same as in Example 1:

[0110] Step 1: Preparation of modified glass fiber:

[0111] 3 g of thioglycolic acid and 100 mL of dimethyl sulfoxide were mixed and uniformly stirred to obtain a thioglycolic acid solution; glass fiber was immersed in the thioglycolic acid solution for 25 minutes, taken out and dried to obtain a modified glass fiber;

[0112] Step 2: Preparation of maleimide-modified graphene oxide:

[0113] Take 0.1 g of graphene oxide, 30 mL of γ-aminopropyltriethoxysilane, and 200 mg of sodium carbonate, incubate at 82°C for 48 h, centrifuge, precipitate, wash, and dry to obtain amino-modified graphene oxide;

[0114] Take 0.2 g of sodium acetate and 10 mL of deionized water, stir evenly to obtain a sodium acetate solution; take 0.1 g of amino-modified graphene oxide, 2 g of furan-2,5-dione, and 30 mL of chlorobenzene, ultrasonically disperse for 12 minutes, heat to 132°C under nitrogen, reflux for 3 hours, cool to 28°C, add 10 mL of sodium acetate solution, heat to 132°C under nitrogen, react for 60 minutes, cool to 27°C, centrifuge, wash, and dry to obtain maleimide-modified graphene oxide;

[0115] Step 3: Preparation of graphene oxide-glass fiber composite:

[0116] Take 0.1g of maleimide-modified graphene oxide and 3mL of N,N-dimethylformamide, ultrasonically disperse them, add 0.3g of styrene and 0.6g of methyl methacrylate under argon environment, and irradiate under 365nm ultraviolet lamp for 60min. Add 3g of modified glass fiber, stir evenly, irradiate under 365nm ultraviolet lamp for 60min, wash and dry to obtain graphene oxide-glass fiber composite;

[0117] Step 4: Preparation of polyamide composite material:

[0118] 100 g of nylon resin and 22 g of polytetrafluoroethylene powder were mixed evenly, and 20 g of graphene oxide-glass fiber composite was added, melt-extruded, and granulated to obtain a polyamide composite material;

[0119] Step 5: Preparation of antiseptic mixture:

[0120] Take polyamide composite material, silane coupling agent KH550, and antioxidant, mix them evenly to obtain anti-corrosion mixture;

[0121] Step 6: Preparation of early warning anti-loosening bolts:

[0122] Fe, Mn, Ni, Si, Ge, C, Ag, Bi, and La are melted, poured, forged, and heat-treated to obtain a bolt matrix;

[0123] The bolt comprises the following components, calculated by mass percentage: 3.5 wt% Mn, 1.9 wt% Ni, 0.6 wt% Si, 0.03 wt% Ge, 0.35 wt% C, 0.02 wt% Ag, 0.009 wt% Bi, 0.0015 wt% La, and the balance being Fe and other unavoidable impurities;

[0124] The bolt base is placed in a mold, the anti-corrosion mixture is added to the injection molding machine, injection molding, overmolding, removal, drying, and obtaining a warning anti-loosening bolt;

[0125] The anti-corrosion mixture is composed of the following substances, calculated by weight: 55 parts of polyamide composite material, 5 parts of silane coupling agent KH550, and 2.5 parts of antioxidant 1010.

[0126] experiment:

[0127] The performance test of the early warning anti-loosening bolts prepared in Examples 1 to 3 and Comparative Examples 1 to 3 was performed. The tensile strength of the early warning anti-loosening bolts was tested with reference to GB / T 228-2010 and GB / T 3098.1-2010. The early warning anti-loosening bolts were immersed in a 15% by mass hydrochloric acid aqueous solution for 1 hour, removed, and the corrosion loss of the early warning anti-loosening bolts before and after immersion was tested. The data obtained are shown below:

[0128] Tensile strength / Mpa Corrosion loss / % Example 1 1521 0.004 Example 2 1517 0.005 Example 3 1523 0.004 Comparative Example 1 1511 0.073 Comparative Example 2 1493 0.162 Comparative Example 3 1506 0.090

[0129] Conclusion: Comparing the data in the table shows that in Comparative Example 1, where thioglycolic acid is not added to the polyamide-modified glass fiber, the composite effect of vinyl graphene oxide and polyamide-modified glass fiber is poor, resulting in a decrease in the corrosion resistance of the bolt. In Comparative Example 2, where glass fiber is not added, the corrosion resistance of the early warning anti-loosening bolt is significantly reduced. In Comparative Example 3, where polyamide is not used to modify the glass fiber, the dispersion of the graphene oxide-glass fiber composite in the polyamide composite matrix is ​​poor, resulting in a decrease in the corrosion resistance of the bolt and an increase in corrosion loss. In Examples 1 to 3 of the present invention, furan-2,5-dione is used to modify amino-modified graphene oxide to obtain a maleimide-modified graphene oxide. Maleimide is sensitive to ultraviolet light and can react with styrene and methyl methacrylate under ultraviolet light to obtain vinyl graphene oxide. Polyamide-modified glass fiber is then added, stirred evenly, and illuminated under a 365nm ultraviolet lamp to cause the thiol group on the polyamide-modified glass fiber to react with the vinyl group, thereby allowing the vinyl graphene oxide and the polyamide-modified glass fiber to be better composited together, thereby improving the corrosion resistance of the bolt.

[0130] It will be apparent to those skilled in the art that the present invention is not limited to the details of the exemplary embodiments described above and that the invention can be embodied in other specific forms without departing from the spirit or essential characteristics of the invention. Therefore, the embodiments should be considered in all respects as illustrative and non-restrictive, and the scope of the invention is defined by the appended claims rather than the foregoing description, and it is intended that all variations that come within the meaning and range of equivalents of the claims be embraced therein.

Claims

1. A preparation process for an early warning anti-loosening bolt, characterized by: The following steps are involved: Step 1: Take nylon resin and polytetrafluoroethylene powder, stir them evenly, add graphene oxide-glass fiber composite, melt extrude and granulate to obtain polyamide composite material; Step 2: taking a polyamide composite material, a silane coupling agent, and an antioxidant, and mixing them evenly to obtain an anti-corrosion mixture; Step 3: Take Fe, Mn, Ni, Si, Ge, C, Ag, Bi, and La, melt, pour, forge, and heat treat to obtain a bolt matrix; Step 4: Place the bolt base in a mold, add the anti-corrosion mixture into an injection molding machine, perform injection molding, overmolding, take out, and dry to obtain a warning anti-loosening bolt; The preparation method of the graphene oxide-glass fiber composite comprises: taking maleimide-modified graphene oxide and N,N-dimethylformamide, ultrasonically dispersing, adding styrene and methyl methacrylate under an argon environment, irradiating under ultraviolet light for 50-70 minutes, adding polyamide-modified glass fiber, stirring evenly, irradiating under ultraviolet light for 50-70 minutes, washing, and drying to obtain the graphene oxide-glass fiber composite; Deionized water and an emulsifier are mixed and stirred to obtain a mixed solution; polyhexamethylene adipamide, thioglycolic acid, and dimethyl sulfoxide are mixed and stirred to obtain a mixed solution of polyhexamethylene adipamide; glass fiber is immersed in the mixed solution of polyhexamethylene adipamide for 20-30 minutes, removed, and dried to obtain a polyamide-modified glass fiber; The preparation method of the maleimide-modified graphene oxide comprises the following steps: taking sodium acetate and deionized water, stirring uniformly to obtain a sodium acetate solution; taking amino-modified graphene oxide, furan-2,5-dione, and chlorobenzene, ultrasonically dispersing for 10-15 minutes, heating to 130-135° C. under nitrogen, reflux for 2-4 hours, cooling to 25-30° C., adding the sodium acetate solution, heating to 130-135° C. under nitrogen, reacting for 50-70 minutes, cooling to 25-30° C., centrifuging, washing, and drying to obtain the maleimide-modified graphene oxide.

2. The process for preparing a warning anti-loosening bolt according to claim 1, characterized in that: The anti-corrosion mixture is composed of the following substances, calculated by weight: 50-60 parts of polyamide composite material, 4-6 parts of silane coupling agent, and 2-3 parts of antioxidant.

3. The process for preparing the early warning anti-loosening bolt according to claim 1, characterized in that: The preparation method of the amino-modified graphene oxide comprises the following steps: taking graphene oxide, γ-aminopropyltriethoxysilane and sodium carbonate, heating at 80-85° C. for 46-50 hours, centrifuging, precipitating, washing and drying to obtain the amino-modified graphene oxide.

4. The process for preparing a warning anti-loosening bolt according to claim 1, characterized in that: The bolt includes the following components, in percentage by mass: 3.0wt%-4.0wt% of Mn, 1.5wt%-2.5wt% of Ni, 0.4wt%-0.7wt% of Si, 0.01wt%-0.04wt% of Ge, 0.3wt%-0.4wt% of C, 0.01wt%-0.03wt% of Ag, 0.008wt%-0.01wt% of Bi, 0.001wt%-0.002wt% of La, and the balance is Fe and other inevitable impurities.

5. The process for preparing a warning anti-loosening bolt according to claim 1, characterized in that: The antioxidant is any one or more of antioxidant 1010, antioxidant 164, and antioxidant 1076.

6. The process for preparing a warning anti-loosening bolt according to claim 1, characterized in that: The silane coupling agent is KH550.

7. An early warning and anti-loosening bolt prepared by the process for preparing an early warning and anti-loosening bolt according to any one of claims 1 to 6.