A rapid-curing anaerobic sealing liquid and its preparation method
By selecting specific ratios of polyurethane acrylate and epoxy acrylate as oligomers and combining them with benzoyl peroxide microcapsule initiators, a fast-curing anaerobic sealing liquid was prepared, which solved the problems of slow curing speed and poor adhesion performance of aluminum tubes, and achieved a high-strength, low-odor, and stable anaerobic sealing effect.
Patent Information
- Application Number
- CN202211706994.X
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2022-12-29
- Publication Date
- 2025-10-28
- Estimated Expiration
- 2042-12-29
AI Technical Summary
Existing anaerobic sealing liquids have slow curing speed, poor adhesion, poor resistance to high and low temperature impacts on aluminum tubes, and have a strong odor during use, which can easily cause allergies.
Polyurethane acrylate and epoxy acrylate were used as vinyl-containing oligomers, with their weight ratio controlled at (2-6):1. Aliphatic polyurethane acrylate and modified epoxy acrylate with different viscosities were combined, and benzoyl peroxide microcapsules and cumene hydroperoxide were used as initiators. Their particle size and mass ratio were controlled to prepare a fast-curing anaerobic sealing liquid.
It improves the adhesion strength and curing speed of anaerobic sealing fluid on aluminum, enhances high and low temperature impact resistance, reduces odor and allergenicity, improves storage stability, and meets the connection requirements of refrigeration appliance pipelines.
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Abstract
Description
Technical Field
[0001] This invention relates to the field of anaerobic adhesive technology, particularly to the field of IPC C09J175, and further to a rapid-curing anaerobic sealing liquid and its preparation method. Background Technology
[0002] Anaerobic adhesives are single-component sealants made using the principle of oxygen inhibiting free radical polymerization. They can be used for both bonding and sealing. When the adhesive surface is isolated from air and under catalytic conditions, it can rapidly polymerize and cure at room temperature. As a solvent-free adhesive, anaerobic adhesives do not volatilize during the curing process, have simple curing film-forming conditions, and are environmentally friendly. They have been widely used in aerospace, military, automotive, machinery, electronics, and electrical industries.
[0003] With economic development and improved living standards, modern people's lives are increasingly inseparable from refrigeration appliances such as refrigerators, freezers, and air conditioners. However, since the refrigerant in the refrigeration system is gaseous at normal temperature and pressure, the pipe connection technology has very high requirements for airtightness. At present, the anaerobic adhesive used for sealing between pipes in refrigeration equipment in my country has good curing speed and bonding performance on copper and iron pipes, but it still has problems such as slow curing speed, poor bonding performance, poor resistance to high and low temperature impact, and strong odor during use, which can easily cause allergies.
[0004] Chinese Patent CN 114032037 A discloses an anaerobic sealing liquid and its preparation method, mainly comprising the following components: polyurethane-modified epoxy resin, methacrylic acid, filler, initiator, first accelerator, second accelerator, first polymerization inhibitor, second polymerization inhibitor, co-accelerator, and metal chelate. The filler is selected from at least one of polybenzoxazole and polytetrafluoroethylene. The above-mentioned anaerobic sealing liquid can withstand temperatures up to 850℃, exhibiting better high-temperature resistance. However, the technical problem solved by this solution is primarily the high-temperature resistance of the anaerobic sealing liquid; it is not suitable for connections between pipes in refrigeration appliances. Summary of the Invention
[0005] The first aspect of the present invention provides a fast-curing anaerobic sealing liquid, which, by weight, comprises the following raw materials: 20-50 parts of vinyl oligomer, 10-30 parts of methacrylate monomer, 10-30 parts of polyol acrylate, 5-15 parts of environmentally friendly diluent, 1-3 parts of accelerator, 0.5-2 parts of polymerization inhibitor, and 0.2-1 parts of initiator.
[0006] In some preferred embodiments, the vinyl-containing oligomer is selected from one or more combinations of polyurethane acrylates, epoxy acrylates, epoxy methacrylates, and polyester acrylates.
[0007] Preferably, the vinyl-containing oligomer is selected from a combination of polyurethane acrylate and epoxy acrylate.
[0008] Preferably, the weight ratio of the polyurethane acrylate to the epoxy acrylate is (2-6):1.
[0009] Preferably, the functionality of the polyurethane acrylate is 2.
[0010] Preferably, the polyurethane acrylate includes aliphatic polyurethane methacrylate, aliphatic polyurethane acrylate A, and aliphatic polyurethane acrylate B.
[0011] Preferably, the weight ratio of the aliphatic polyurethane methacrylate, aliphatic polyurethane acrylate A, and aliphatic polyurethane acrylate B is (1-3):(1-3):(1-3).
[0012] Preferably, the weight ratio of the aliphatic polyurethane methacrylate, aliphatic polyurethane acrylate A, and aliphatic polyurethane acrylate B is 2:2:1.
[0013] Preferably, the viscosity of the aliphatic polyurethane methacrylate is 1000-2500 cps (60°C).
[0014] Preferably, the viscosity of the aliphatic polyurethane acrylate A is 20,000 to 40,000 cps (60°C).
[0015] Preferably, the viscosity of the aliphatic polyurethane acrylate B is 10,000 to 60,000 cps (25°C).
[0016] Preferably, the epoxy acrylate has a functionality of 2.
[0017] Preferably, the epoxy acrylate is a combination of modified epoxy acrylate A and modified epoxy acrylate B.
[0018] Preferably, the weight ratio of the modified epoxy acrylate A to the modified epoxy acrylate B is (3-6):1.
[0019] Preferably, the viscosity of the modified epoxy acrylate A is 2000-6000 (25°C).
[0020] Preferably, the viscosity of the modified epoxy acrylate B is 5000-6200 (25°C).
[0021] Based on the system of this invention, by selecting polyurethane acrylate and epoxy acrylate as vinyl-containing oligomers and controlling the weight ratio of polyurethane acrylate to epoxy acrylate to be (2-6):1, the adhesive strength of the anaerobic sealant is improved while simultaneously enhancing the curing speed and high / low temperature impact resistance. The applicant hypothesizes that the flexible aliphatic long chains in the molecular structure of polyurethane acrylate can effectively transfer curing stress and thermal effects, resulting in uniformly dispersed internal stress and low shrinkage stress. This makes it suitable for preparing anaerobic adhesives with excellent adhesive properties and low-temperature resistance. Epoxy acrylate, while possessing excellent adhesive properties and low curing shrinkage, suffers from poor low-temperature resistance and impact resistance. By using polyurethane acrylate and epoxy acrylate together, the resulting anaerobic adhesive exhibits both good adhesive strength, good curing speed, and high / low temperature impact resistance. When the weight ratio of polyurethane acrylate to epoxy acrylate is (2-6):1, the good compatibility and high crosslinking density of the two materials result in a relatively uniform network structure, further improving their adhesive strength, curing speed, and high / low temperature impact resistance. The applicant has discovered that when the polyurethane acrylate is an aliphatic polyurethane methacrylate with a viscosity of 1000–2500 cps (60°C), an aliphatic polyurethane acrylate A with a viscosity of 20000–40000 cps, and an aliphatic polyurethane acrylate B with a viscosity of 10000–60000 cps (60°C), the adhesive strength is improved, and the storage stability of the anaerobic adhesive is further enhanced. The applicant hypothesizes that, on the one hand, selecting polyurethane acrylates of different viscosities ensures a moderate viscosity in the anaerobic adhesive system, avoiding excessively high viscosity that would prevent air bubbles from escaping and create stress concentration points that reduce adhesive strength; on the other hand, the optimal synergistic effect of polyurethane acrylates of different viscosities with accelerators and polymerization inhibitors in the system further improves the system's storage stability.
[0022] In some preferred embodiments, the methacrylate monomer is selected from one or more combinations of hydroxypropyl methacrylate, lauryl methacrylate, hydroxyethyl methacrylate, isobornyl methacrylate, and tetraethylene glycol dimethacrylate.
[0023] Preferably, the methacrylate monomer is selected from a combination of hydroxyethyl methacrylate and lauryl methacrylate.
[0024] Preferably, the weight ratio of hydroxyethyl methacrylate to lauryl methacrylate is (1-3):1.
[0025] In some preferred embodiments, the polyol acrylate is selected from one or more combinations of polypropylene glycol monomethacrylate, polyethylene glycol dimethacrylate, polyethylene glycol methacrylate, and polypropylene glycol dimethacrylate.
[0026] Preferably, the polyol acrylate is selected from a combination of polypropylene glycol monomethacrylate and polyethylene glycol dimethacrylate.
[0027] Preferably, the weight ratio of polypropylene glycol monomethacrylate to polyethylene glycol dimethacrylate is (1-3):1.
[0028] Preferably, the average molecular weight of the polypropylene glycol monomethacrylate is 350-650 g / mol.
[0029] Preferably, the average molecular weight of the polyethylene glycol dimethacrylate is 200-600 g / mol.
[0030] This invention selects polypropylene glycol monomethacrylate and polyethylene glycol dimethacrylate with an average molecular weight of 350-650 g / mol as polyol acrylates, and controls the weight ratio of polypropylene glycol monomethacrylate to polyethylene glycol dimethacrylate to be (1-3):1. This improves both the flexibility and bonding strength of the anaerobic sealing liquid, while also increasing its curing speed. The applicant hypothesizes that because polypropylene glycol monomethacrylate and polyethylene glycol dimethacrylate contain ether bonds in their molecular structures, they have low cohesive energy and are easily rotated, thus improving the flexibility of the anaerobic sealing liquid. Furthermore, controlling the molecular weight of polypropylene glycol monomethacrylate and polyethylene glycol dimethacrylate helps to increase their reactivity, thereby increasing the curing speed of the anaerobic sealing liquid.
[0031] In some preferred embodiments, the environmentally friendly diluent is a mixed diester.
[0032] Preferably, the mixed diester is methyl nylonate.
[0033] In some preferred embodiments, the polymerization inhibitor is selected from one or more combinations of 1,4-naphthoquinone, hydroquinone, benzoquinone, and p-isopropylphenol.
[0034] In some preferred embodiments, the promoter is selected from one or more combinations of saccharin, acetylphenylhydrazine, triethanolamine, N,N-dimethylaniline, and o-benzoylsulfonylimide.
[0035] Preferably, the promoter is a combination of acetylphenylhydrazine and N,N-dimethylaniline.
[0036] Preferably, the weight ratio of acetylphenylhydrazine to N,N-dimethylaniline is (1-3):(1-3).
[0037] In some preferred embodiments, the material is selected from benzoyl peroxide, cumene hydroperoxide, or a combination thereof.
[0038] Preferably, the initiator is a combination of benzoyl peroxide and cumene hydroperoxide.
[0039] Preferably, the benzoyl peroxide is a benzoyl peroxide microcapsule.
[0040] Preferably, the mass ratio of the benzoyl peroxide microcapsules to cumene peroxide is 1:(5-10).
[0041] Preferably, the method for preparing the benzoyl peroxide microcapsules includes the following steps:
[0042] (1) Formaldehyde aqueous solution, urea and triethanolamine are stirred and reacted at 65-80℃ for 40-100 min to obtain prepolymer;
[0043] (2) Add benzoyl peroxide to deionized water, stir quickly to disperse it evenly, add hydrochloric acid to adjust the pH value to 2-3, and add the prepolymer at a temperature of 30℃-40℃ for 2-4 hours;
[0044] (3) After the reaction is complete, the product is obtained by washing, filtering, drying and sieving.
[0045] Preferably, the formaldehyde aqueous solution has a mass percentage of 35-40%.
[0046] Preferably, the mass ratio of the formaldehyde aqueous solution, urea, and triethanolamine is (2-3):1:(0.005-0.1).
[0047] Preferably, the particle size of the benzoyl peroxide microcapsules is 5-8 μm.
[0048] Preferably, the mass ratio of benzoyl peroxide to deionized water is 1:(10-15).
[0049] In this invention, by using benzoyl peroxide microcapsules and cumene hydroperoxide as initiators, the particle size of the benzoyl peroxide microcapsules is controlled to be 5-8 μm, and the mass ratio of benzoyl peroxide microcapsules to cumene hydroperoxide is controlled to be 1:(5-10). During the use of the anaerobic sealing liquid, the benzoyl peroxide microcapsules will rupture and release benzoyl peroxide. In this formulation system, the density of the benzoyl peroxide microcapsules and the anaerobic sealing liquid is relatively close, and the benzoyl peroxide microcapsules will not float or settle. This not only improves the curing speed of the anaerobic sealing liquid on aluminum, but also improves the storage stability of the anaerobic sealing liquid.
[0050] Another aspect of the present invention provides a method for preparing a rapid curing anaerobic sealing liquid, comprising the following steps: mixing a vinyl-containing oligomer, a methacrylate monomer, a polyol acrylate, an environmentally friendly diluent, and a polymerization inhibitor evenly, stirring at 30-60°C for 2-4 hours, turning off the heating, and then adding an accelerator and an initiator and stirring evenly to obtain the liquid.
[0051] Beneficial effects:
[0052] 1. This invention selects polyurethane acrylate and epoxy acrylate as vinyl-containing oligomers, and controls the weight ratio of polyurethane acrylate to epoxy acrylate to be (2-6):1, thereby improving the adhesion strength of the anaerobic sealant on aluminum materials, as well as the curing speed and high and low temperature impact performance on aluminum materials.
[0053] 2. When the present invention selects aliphatic polyurethane methacrylate with a viscosity of 1000-2500 cps (60℃), aliphatic polyurethane acrylate A with a viscosity of 20000-40000 cps (60℃), and aliphatic polyurethane acrylate B with a viscosity of 10000-60000 cps (25℃), it can improve the adhesion strength of the anaerobic sealing liquid on aluminum materials and further improve the storage stability of the anaerobic sealing liquid.
[0054] 3. This invention selects polypropylene glycol monomethacrylate with an average molecular weight of 350-650 g / mol and polyethylene glycol dimethacrylate with an average molecular weight of 350-650 g / mol as polypolyol acrylates, and controls the weight ratio of polypropylene glycol monomethacrylate to polyethylene glycol dimethacrylate to be (1-3):1. This improves the flexibility and bonding strength of the anaerobic sealing liquid while also increasing the curing speed of the anaerobic sealing liquid.
[0055] 4. This invention uses benzoyl peroxide microcapsules and cumene hydroperoxide as initiators, controls the particle size of the benzoyl peroxide microcapsules to be 5-8 μm, and controls the mass ratio of benzoyl peroxide microcapsules to cumene hydroperoxide to be 1:(5-10). During the use of the anaerobic sealing liquid, the benzoyl peroxide microcapsules will rupture and release benzoyl peroxide. In this formulation system, the density of the benzoyl peroxide microcapsules and the anaerobic sealing liquid is relatively close, and the benzoyl peroxide microcapsules will not float or sink. This improves the curing speed of the anaerobic sealing liquid on aluminum materials and also improves the storage stability of the anaerobic sealing liquid.
[0056] 5. The present invention uses specific vinyl-containing oligomers, methacrylate monomers, polypolyol acrylates, environmentally friendly diluents, accelerators, polymerization inhibitors and initiators to prepare a fast-curing anaerobic sealing liquid that is low in odor, low in allergens, green, environmentally friendly and safe.
[0057] 6. The environmentally friendly diluent used in this invention has a high boiling point, is not easily volatile, has a good dilution effect, and is environmentally friendly and has a low odor. Detailed Implementation
[0058] Example 1
[0059] Example 1 provides a fast-curing anaerobic sealing liquid, which, by weight, includes the following raw materials: 36 parts of vinyl oligomer, 20 parts of methacrylate monomer, 20 parts of polyol acrylate, 10 parts of environmentally friendly diluent, 2 parts of accelerator, 1 part of polymerization inhibitor, and 0.5 parts of initiator.
[0060] The vinyl-containing oligomer is selected from a combination of polyurethane acrylate and epoxy acrylate.
[0061] The weight ratio of the polyurethane acrylate to the epoxy acrylate is 4:1.
[0062] The polyurethane acrylates include aliphatic polyurethane methacrylate, aliphatic polyurethane acrylate A, and aliphatic polyurethane acrylate A.
[0063] The weight ratio of the aliphatic polyurethane methacrylate, aliphatic polyurethane acrylate A, and aliphatic polyurethane acrylate B is 2:2:1.
[0064] The viscosity of the aliphatic polyurethane methacrylate is 1740 cps (60℃), and it is Sartoma CN1963.
[0065] The viscosity of the polyurethane acrylate A is 30000±5000cps (60℃), and it is Changxing Chemical DR-U299.
[0066] The viscosity of the aliphatic polyurethane acrylate A is 30,000 to 50,000 cps (25°C), and it is Changxing Chemical 6164.
[0067] The epoxy acrylate is a combination of modified epoxy acrylate A and modified epoxy acrylate B.
[0068] The weight ratio of modified epoxy acrylate A to modified epoxy acrylate B is 5:1.
[0069] The modified epoxy acrylate A has a viscosity of 4250±1250cps (25℃) and is Changxing Chemical DR-G902.
[0070] The viscosity of the modified epoxy acrylate B is 5000-6200 cps (25℃), which is Changxing Chemical 6215-100.
[0071] The methacrylate monomer is selected from a combination of hydroxyethyl methacrylate and lauryl methacrylate.
[0072] The weight ratio of hydroxyethyl methacrylate to lauryl methacrylate is 2:1.
[0073] The polyol acrylate is selected from a combination of polypropylene glycol monomethacrylate and polyethylene glycol dimethacrylate.
[0074] The weight ratio of polypropylene glycol monomethacrylate to polyethylene glycol dimethacrylate is 2:1.
[0075] The polypropylene glycol monomethacrylate had an average molecular weight of 376 g / mol and was purchased from Shanghai Fushun International Trade Co., Ltd.
[0076] The polyethylene glycol dimethacrylate had an average molecular weight of 330 g / mol and was purchased from Shanghai Fushun International Trade Co., Ltd.
[0077] The environmentally friendly diluent is methyl nylonate.
[0078] The polymerization inhibitor is hydroquinone.
[0079] The accelerator is a combination of acetylphenylhydrazine and N,N-dimethylaniline.
[0080] The weight ratio of acetylphenylhydrazine to N,N-dimethylaniline is 1:2.
[0081] The initiator is a combination of benzoyl peroxide and cumene hydroperoxide.
[0082] The benzoyl peroxide is a benzoyl peroxide microcapsule.
[0083] The mass ratio of benzoyl peroxide microcapsules to cumene peroxide is 1:8.
[0084] The preparation method of the benzoyl peroxide microcapsules includes the following steps:
[0085] (1) Formaldehyde aqueous solution, urea and triethanolamine were stirred at 70°C for 60 min to obtain a prepolymer;
[0086] (2) Add benzoyl peroxide to deionized water, stir quickly to disperse it evenly, add hydrochloric acid to adjust the pH value to 2.5, add the prepolymer at 35℃ and react for 3h;
[0087] (3) After the reaction is complete, the product is obtained by washing, filtering, drying and sieving.
[0088] The formaldehyde aqueous solution has a mass percentage of 38%.
[0089] The mass ratio of the formaldehyde aqueous solution, urea, and triethanolamine is 2.5:1:0.008.
[0090] The mass ratio of benzoyl peroxide to deionized water is 1:12.
[0091] The benzoyl peroxide microcapsules have a particle size of 6 μm.
[0092] A method for preparing a fast-curing anaerobic sealing liquid includes the following steps: mixing a vinyl-containing oligomer, methacrylate monomer, polypolyol acrylate, environmentally friendly diluent, and polymerization inhibitor evenly, stirring at 40°C for 3 hours, turning off the heating, and then adding an accelerator and initiator and stirring evenly to obtain the liquid.
[0093] Example 2
[0094] Example 2 provides a fast-curing anaerobic sealing liquid, which, by weight, includes the following raw materials: 45 parts of vinyl oligomer, 15 parts of methacrylate monomer, 25 parts of polyol acrylate, 8 parts of environmentally friendly diluent, 2.5 parts of accelerator, 1.5 parts of polymerization inhibitor, and 0.5 parts of initiator.
[0095] The vinyl-containing oligomer is selected from a combination of polyurethane acrylate and epoxy acrylate.
[0096] The weight ratio of the polyurethane acrylate to the epoxy acrylate is 3:1.
[0097] The polyurethane acrylates include aliphatic polyurethane methacrylate, aliphatic polyurethane acrylate A, and aliphatic polyurethane acrylate A.
[0098] The weight ratio of the aliphatic polyurethane methacrylate, aliphatic polyurethane acrylate A, and aliphatic polyurethane acrylate B is 2:2:1.
[0099] The viscosity of the aliphatic polyurethane methacrylate is 1740 cps (60℃), and it is Sartoma CN1963.
[0100] The viscosity of the polyurethane acrylate A is 30000±5000cps (60℃), and it is Changxing Chemical DR-U299.
[0101] The viscosity of the aliphatic polyurethane acrylate A is 30,000 to 50,000 cps (25°C), and it is Changxing Chemical 6164.
[0102] The epoxy acrylate is a combination of modified epoxy acrylate A and modified epoxy acrylate B.
[0103] The weight ratio of modified epoxy acrylate A to modified epoxy acrylate B is 5:1.
[0104] The modified epoxy acrylate A has a viscosity of 4250±1250cps (25℃) and is Changxing Chemical DR-G902.
[0105] The viscosity of the modified epoxy acrylate B is 5000-6200 cps (25℃), which is Changxing Chemical 6215-100.
[0106] The methacrylate monomer is selected from a combination of hydroxyethyl methacrylate and lauryl methacrylate.
[0107] The weight ratio of hydroxyethyl methacrylate to lauryl methacrylate is 2:1.
[0108] The polyol acrylate is selected from a combination of polypropylene glycol monomethacrylate and polyethylene glycol dimethacrylate.
[0109] The weight ratio of polypropylene glycol monomethacrylate to polyethylene glycol dimethacrylate is 2:1.
[0110] The polypropylene glycol monomethacrylate had an average molecular weight of 376 g / mol and was purchased from Shanghai Fushun International Trade Co., Ltd.
[0111] The polyethylene glycol dimethacrylate had an average molecular weight of 330 g / mol and was purchased from Shanghai Fushun International Trade Co., Ltd.
[0112] The environmentally friendly diluent is methyl nylonate.
[0113] The polymerization inhibitor is hydroquinone.
[0114] The accelerator is a combination of acetylphenylhydrazine and N,N-dimethylaniline.
[0115] The weight ratio of acetylphenylhydrazine to N,N-dimethylaniline is 1:2.
[0116] The initiator is a combination of benzoyl peroxide and cumene hydroperoxide.
[0117] The benzoyl peroxide is a benzoyl peroxide microcapsule.
[0118] The mass ratio of benzoyl peroxide microcapsules to cumene peroxide is 1:8.
[0119] The preparation method of the benzoyl peroxide microcapsules includes the following steps:
[0120] (1) Formaldehyde aqueous solution, urea and triethanolamine were stirred at 70°C for 60 min to obtain a prepolymer;
[0121] (2) Add benzoyl peroxide to deionized water, stir quickly to disperse it evenly, add hydrochloric acid to adjust the pH value to 2.5, add the prepolymer at 35℃ and react for 3h;
[0122] (3) After the reaction is complete, the product is obtained by washing, filtering, drying and sieving.
[0123] The formaldehyde aqueous solution has a mass percentage of 38%.
[0124] The mass ratio of the formaldehyde aqueous solution, urea, and triethanolamine is 2.5:1:0.008.
[0125] The mass ratio of benzoyl peroxide to deionized water is 1:12.
[0126] The benzoyl peroxide microcapsules have a particle size of 6 μm.
[0127] A method for preparing a fast-curing anaerobic sealing liquid includes the following steps: mixing a vinyl-containing oligomer, methacrylate monomer, polypolyol acrylate, environmentally friendly diluent, and polymerization inhibitor evenly, stirring at 40°C for 3 hours, turning off the heating, and then adding an accelerator and initiator and stirring evenly to obtain the liquid.
[0128] Example 3
[0129] Example 3 provides a fast-curing anaerobic sealing liquid, the specific implementation of which is the same as that of Example 1, except that the weight ratio of the polyurethane acrylate and epoxy acrylate is 2:1.
[0130] Example 4
[0131] Example 4 provides a fast-curing anaerobic sealing liquid, the specific implementation of which is the same as that of Example 1, except that the polyurethane acrylate includes aliphatic polyurethane acrylate A and aliphatic polyurethane acrylate B; the weight ratio of aliphatic polyurethane acrylate A to aliphatic polyurethane acrylate B is 2:1.
[0132] Example 5
[0133] Example 5 provides a fast-curing anaerobic sealing liquid, the specific implementation of which is the same as that of Example 1, except that the weight ratio of the aliphatic polyurethane methacrylate, aliphatic polyurethane acrylate A and aliphatic polyurethane acrylate is 1:2:4.
[0134] Example 6
[0135] Example 6 provides a fast-curing anaerobic sealing liquid, the specific implementation of which is the same as that of Example 1, except that the epoxy acrylate is modified epoxy acrylate B.
[0136] Example 7
[0137] Example 7 provides a commercially available Lokprep sealing fluid, purchased from Qingdao Punai Technology Co., Ltd.
[0138] Performance testing:
[0139] 1. Viscosity: Refer to GB / T2794 2013 to test the rapid curing anaerobic sealing liquids prepared in Examples 1 to 5.
[0140] 2. Non-volatile content % (after 180 min at 105℃): Refer to GB / T2793 1995 to test the rapid curing anaerobic sealing liquids prepared in Examples 1 to 5.
[0141] 3. Initial curing time: The rapid curing anaerobic sealing liquid prepared in Examples 1 to 5 was used to seal the 1060 aluminum sleeve and cured at 15°C. The time until the 1060 aluminum sleeve could not be turned by hand was counted as the initial curing time.
[0142] 4. Shear strength: The rapid curing anaerobic sealing liquid prepared in Examples 1-5 was used to seal 1060 aluminum sleeves, and the shear strength was tested after curing at 25°C for 24 hours.
[0143] 5. High and low temperature impact performance: The rapid curing anaerobic sealing liquid prepared in Examples 1 to 5 was used to seal 1060 aluminum sleeves. After curing at 25℃ for 24 hours, the high and low temperature impact performance was tested (-55℃×1h-70℃×1h)×3 times. After standing for 24 hours, a water test was performed at 4.5MPa pressure for 10 minutes to observe whether there were bubbles. No bubbles meant it was qualified, and the presence of bubbles meant it was unqualified.
[0144] 6. Storage stability: Place the rapid curing anaerobic sealing liquids prepared in Examples 1 to 5 in a 50°C oven for 1 month and observe whether gelation occurs. If no gelation occurs, it is considered qualified; if gelation occurs, it is considered unqualified.
[0145] Test results:
[0146] Table 1
[0147]
Claims
1. A rapidly curing anaerobic sealing liquid, characterized in that, By weight, it includes the following ingredients: The mixture contains 20-50 parts of vinyl oligomer, 10-30 parts of methacrylate monomer, 10-30 parts of polypolyol acrylate, 5-15 parts of environmentally friendly diluent, 1-3 parts of accelerator, 0.5-2 parts of polymerization inhibitor, and 0.2-1 parts of initiator. The vinyl-containing oligomer is a polyurethane acrylate and an epoxy acrylate in a weight ratio of (2-6):
1. The polyurethane acrylates include aliphatic polyurethane methacrylate, aliphatic polyurethane acrylate A, and aliphatic polyurethane acrylate B. The weight ratio of the aliphatic polyurethane methacrylate, aliphatic polyurethane acrylate A, and aliphatic polyurethane acrylate B is (1-3):(1-3):(1-3), wherein the viscosity of the aliphatic polyurethane methacrylate is 1000-2500 cps at 60°C, the viscosity of the aliphatic polyurethane acrylate A is 20000-40000 cps at 60°C, and the viscosity of the aliphatic polyurethane acrylate B is 20000-40000 cps at 25°C. The epoxy acrylate is a combination of modified epoxy acrylate A and modified epoxy acrylate B, with a weight ratio of (3-6):
1. The viscosity of modified epoxy acrylate A is 2000-6000 cps at 25°C, and the viscosity of modified epoxy acrylate B is 5000-6200 cps at 25°C.
2. The rapid-curing anaerobic sealing liquid according to claim 1, characterized in that, The functionality of the polyurethane acrylate is 2.
3. The rapid-curing anaerobic sealing liquid according to claim 1, characterized in that, The methacrylate monomer is selected from one or more combinations of hydroxypropyl methacrylate, lauryl methacrylate, hydroxyethyl methacrylate, isobornyl methacrylate, and tetraethylene glycol dimethacrylate.
4. The rapid-curing anaerobic sealing liquid according to claim 1, characterized in that, The polyol acrylate is selected from one or more combinations of polypropylene glycol monomethacrylate, polyethylene glycol dimethacrylate, polyethylene glycol methacrylate, and polypropylene glycol dimethacrylate.
5. The rapid-curing anaerobic sealing liquid according to claim 1, characterized in that, The accelerator is selected from one or more combinations of saccharin, acetylphenylhydrazine, triethanolamine, N,N-dimethylaniline, and o-benzoylsulfonylimide.
6. The rapid-curing anaerobic sealing liquid according to claim 1, characterized in that, The polymerization inhibitor is selected from one or more combinations of 1,4-naphthoquinone, hydroquinone, benzoquinone, and p-isopropylphenol.
7. The rapid-curing anaerobic sealing liquid according to claim 1, characterized in that, The initiator is selected from benzoyl peroxide, cumene hydroperoxide, or a combination thereof.
8. A method for preparing a rapid-curing anaerobic sealing liquid according to any one of claims 1 to 7, characterized in that, Includes the following steps: Mix the vinyl-containing oligomer, methacrylate monomer, polyol acrylate, environmentally friendly diluent, and polymerization inhibitor evenly, stir at 30-60°C for 2-4 hours, turn off the heating, and then add the accelerator and initiator and stir evenly to obtain the final product.
Citation Information
Patent Citations
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