Anaerobic sealing fluid, its preparation method and application

Abstract

This invention belongs to the field of sealing material technology, specifically relating to an anaerobic sealing liquid and its preparation method and application. The anaerobic sealing liquid comprises the following components by weight: 20-50 parts monomer, 0.5-2 parts initiator, 0.1-1 parts accelerator, and 0.1-1 parts co-accelerator. The monomer includes one or more of polyurethane acrylate, bisphenol A epoxy acrylate, (4) ethylene oxide bisphenol A dimethacrylate, triethylene glycol dimethacrylate, hydroxyethyl methacrylate, and hydroxypropyl methacrylate. Due to the rational formulation of monomers and various additives, the obtained anaerobic sealing liquid has a fast curing rate and excellent airtightness, pull-out resistance, storage stability, and corrosion resistance, meeting the airtightness requirements of pipe connection technology.

Description

Technical Field

[0001] This invention belongs to the field of sealing material technology, and specifically relates to an anaerobic sealing liquid, its preparation method and application. Background Technology

[0002] Anaerobic adhesives and sealants (or anaerobic adhesives for short) are adhesives that inhibit curing in the presence of oxygen and cure on their own when isolated from air. Due to their unique anaerobic curing properties, they have been widely used in thread tightening, pipe bonding, leak sealing, and flange sealing, and have become an important industrial adhesive.

[0003] In refrigeration appliances such as refrigerators, freezers, and air conditioners, the refrigerant in the refrigeration system is gaseous at room temperature and pressure, so the pipe connection technology has very high requirements for airtightness. Currently, anaerobic adhesives commonly used for sealing pipes in refrigeration equipment have good curing speed and adhesion performance to copper pipes, but still suffer from slow curing speed and poor adhesion performance to aluminum pipes (or aluminum pipes mixed with other metal pipes). In addition, different formulation ratios also have a significant impact on the performance of anaerobic adhesives.

[0004] Therefore, existing anaerobic adhesives still need improvement. Summary of the Invention

[0005] The main objective of this invention is to propose an anaerobic sealing liquid, its preparation method, and its application. Due to the rational formulation of monomers and various additives, the anaerobic sealing liquid obtained in this invention has a fast curing rate and excellent airtightness, pull-out resistance, storage stability, and corrosion resistance, thus meeting the airtightness requirements of pipe connection technology.

[0006] The first aspect of the present invention provides an anaerobic sealing liquid, the anaerobic sealing liquid comprising the following components in parts by weight: 20 to 50 parts of monomer, 0.5 to 2 parts of initiator, 0.1 to 1 part of accelerator and 0.1 to 1 part of co-accelerator; wherein the monomer comprises one or more of polyurethane acrylate, bisphenol A epoxy acrylate, (4) ethoxylated bisphenol A dimethacrylate, triethylene glycol dimethacrylate, hydroxyethyl methacrylate and hydroxypropyl methacrylate.

[0007] In some embodiments of the present invention, the monomer comprises a combination of at least two of bisphenol A epoxy acrylate, (4) bisphenol A dimethacrylate ethoxylate and hydroxypropyl methacrylate.

[0008] In some embodiments of the present invention, the weight ratio of (4) bisphenol A dimethacrylate and hydroxypropyl methacrylate is 19-21:12-16; and / or the weight ratio of bisphenol A epoxy acrylate and hydroxypropyl methacrylate is 4-21:12-18.

[0009] In some embodiments of the present invention, the initiator includes one or more of benzoyl peroxide, cumene hydroperoxide, and tert-butyl hydroperoxide.

[0010] In some embodiments of the present invention, the promoter includes one or more of acetylphenylhydrazine, triethanolamine, and N,N-dimethylaniline.

[0011] In some embodiments of the present invention, the co-promoter includes at least one of o-benzoylsulfonylimide and substituted saccharin.

[0012] In some embodiments of the present invention, the anaerobic sealing liquid further includes at least one of the following components in parts by weight: 0.4 to 2 parts of polymerization inhibitor and 0.03 to 1 part of metal chelating agent.

[0013] In some embodiments of the present invention, the polymerization inhibitor includes one or more of p-benzoquinone, p-tert-butylcatechol, hydroquinone, and p-isopropylphenol.

[0014] In some embodiments of the present invention, the metal chelating agent includes at least one of oxalic acid and disodium ethylenediaminetetraacetate.

[0015] In some embodiments of the present invention, the anaerobic sealing liquid further includes 0.1 to 1 part of organic acid.

[0016] In some embodiments of the present invention, the organic acid includes one or more of methacrylic acid, acetoacetic acid, oxalic acid, and pyruvic acid.

[0017] The second aspect of the present invention provides a method for preparing the anaerobic sealing liquid described in the first aspect, the method comprising: weighing each raw material according to the weight parts and mixing them evenly, and then stirring to prepare the anaerobic sealing liquid.

[0018] In some embodiments of the present invention, the preparation method includes: mixing monomers, polymerization inhibitors, metal chelating agents and organic acids, heating and stirring, cooling and then adding accelerators, co-accelerators and initiators while continuing to stir.

[0019] In some embodiments of the present invention, the heating and stirring temperature is 30°C to 60°C, the heating and stirring speed is 300 rpm to 600 rpm, and the heating and stirring time is 2 h to 5 h.

[0020] In some embodiments of the present invention, the stirring speed after cooling is 300 rpm to 600 rpm, and the stirring time is 1 h to 3 h.

[0021] The third aspect of this invention provides the application of the anaerobic sealing liquid described in the first aspect or the anaerobic sealing liquid prepared by the method described in the second aspect in any of the sealing, retaining, bonding and plugging processes.

[0022] The anaerobic sealing liquid of this invention features a rationally selected composition and proportion of each component, with a significant synergistic mechanism among them, greatly improving the airtightness of the anaerobic sealing liquid and meeting the airtightness requirements of pipe connection technology. Simultaneously, it exhibits a fast curing rate and excellent pull-out strength, storage stability, and corrosion resistance.

[0023] In this invention, by rationally blending monomers and various additives, the obtained anaerobic sealing liquid has a fast curing rate in copper / aluminum / steel pipe joints, approximately 5 to 8 minutes.

[0024] The anaerobic sealing liquid obtained by rationally blending monomers and various additives in this invention has excellent airtightness, pull-out resistance, storage stability and long-term salt spray corrosion resistance, which far exceeds similar products and meets the airtightness requirements of pipe connection technology.

[0025] The above description is merely an overview of the technical solution of the present invention. In order to better understand the technical means of the present invention and to implement it in accordance with the contents of the specification, and in order to make the above and other objects, features and advantages of the present invention more apparent and understandable, specific embodiments of the present invention are described below. Attached Figure Description

[0026] To more clearly illustrate the specific embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the specific embodiments or the prior art will be briefly introduced below. Obviously, the drawings described below are some embodiments of the present invention. For those skilled in the art, other drawings can be obtained from these drawings without creative effort.

[0027] Figure 1 Digital photographs of the anaerobic sealing liquids prepared in Examples 1 to 4 of this invention;

[0028] Figure 2 A digital photograph of a sample of the anaerobic sealing liquid prepared in Example 1 of this invention after a corrosion resistance test.

[0029] Figure 3 A digital photograph showing the sticky residue after the anaerobic sealing liquid prepared in Example 2 of this invention was used to seal a metal sleeve.

[0030] Figure 4 This is a digital photograph of the anaerobic sealing liquid prepared in Example 4 of the present invention used to seal the interface of a metal sleeve. Detailed Implementation

[0031] Exemplary embodiments of the invention will now be described in more detail with reference to the accompanying drawings. While exemplary embodiments of the invention are shown in the drawings, it should be understood that the invention can be implemented in various forms and should not be limited to the embodiments set forth herein. Rather, these embodiments are provided to enable a more thorough understanding of the invention and to fully convey the scope of the invention to those skilled in the art.

[0032] It should be understood that the terminology used herein is for the purpose of describing particular exemplary embodiments only and is not intended to be limiting. Unless the context clearly indicates otherwise, the singular forms “a,” “an,” and “described” as used herein may also include the plural forms. The terms “comprising,” “including,” “containing,” and “having” are inclusive and therefore indicate the presence of the stated features, steps, operations, elements, and / or components, but do not exclude the presence or addition of one or more other features, steps, operations, elements, components, and / or combinations thereof. The method steps, processes, and operations described herein are not construed as requiring them to be performed in a particular order described or illustrated unless the order of performance is explicitly indicated. It should also be understood that additional or alternative steps may be used.

[0033] Although terms such as first, second, third, etc., may be used in this document to describe multiple elements, components, regions, layers, and / or segments, these elements, components, regions, layers, and / or segments should not be limited by these terms. These terms may be used only to distinguish one element, component, region, layer, or segment from another. Unless the context clearly indicates otherwise, terms such as "first," "second," and other numerical terms used herein do not imply order or sequence. Therefore, the first element, component, region, layer, or segment discussed below may be referred to as the second element, component, region, layer, or segment without departing from the teachings of the exemplary embodiments.

[0034] In the description of the embodiments of this invention, the term "and / or" is merely a description of the association relationship between related objects, indicating that three relationships can exist. For example, A and / or B can represent: A exists, A and B exist simultaneously, and B exists. Additionally, the character " / " in this document generally indicates that the preceding and following related objects have an "or" relationship.

[0035] In the description of the embodiments of the present invention, the term "multiple" refers to two or more (including two), similarly, "multiple sets" refers to two or more (including two sets), and "multiple pieces" refers to two or more (including two pieces).

[0036] The first aspect of the present invention provides an anaerobic sealing liquid comprising the following components in parts by weight: 20 to 50 parts of monomer, 0.5 to 2 parts of initiator, 0.1 to 1 part of accelerator, and 0.1 to 1 part of co-accelerator; wherein the monomer comprises one or more of polyurethane acrylate, bisphenol A epoxy acrylate, (4) ethylene oxide bisphenol A diacrylate, triethylene glycol dimethacrylate, hydroxyethyl methacrylate, and hydroxypropyl methacrylate.

[0037] Compared with traditional anaerobic sealing liquids, the anaerobic sealing liquid provided by this invention exhibits excellent airtightness, pull-out resistance, storage stability, and corrosion resistance due to the rational formulation of monomers and various additives. It also has a fast curing rate, meeting the airtightness requirements of pipe connection technology.

[0038] monomer

[0039] Monomers are the main components of anaerobic sealing fluids, and the properties of monomers have a significant impact on the performance of anaerobic sealing fluids.

[0040] In some embodiments of the present invention, the monomer comprises a combination of at least two of bisphenol A epoxy acrylate, (4) bisphenol A dimethacrylate ethoxylate and hydroxypropyl methacrylate.

[0041] In some embodiments, the monomer comprises (4) bisphenol A dimethacrylate ester ethoxylated and hydroxypropyl methacrylate, wherein the weight ratio of (4) bisphenol A dimethacrylate ester ethoxylated and hydroxypropyl methacrylate is 19-21:12-16; in some embodiments, the monomer comprises bisphenol A epoxy acrylate and hydroxypropyl methacrylate, wherein the weight ratio of bisphenol A epoxy acrylate and hydroxypropyl methacrylate is 4-21:12-18, for example, about 19-21:16-18; in some embodiments, the monomer comprises bisphenol A epoxy acrylate, (4) bisphenol A dimethacrylate ester ethoxylated and hydroxypropyl methacrylate.

[0042] In embodiments of the present invention, the weight fractions of the monomer provided by the present invention can be any value within the range formed by any two values ​​in the above-mentioned range, such as 20 to 35 parts, or 35 to 50 parts, and so on. The weight fractions of the monomer provided by the present invention can also be one of 20, 21, 22, 23, 24, 25, 26, 27, 28, 29, 30, 31, 32, 33, 34, 35, 36, 37, 38, 39, 40, 41, 42, 43, 44, 45, 46, 47, 48, 49, and 50 parts, or any value that satisfies the above-mentioned range.

[0043] Initiator

[0044] Initiators are primarily used to initiate monomer polymerization. Initiators generate free radicals or radicals, thereby initiating monomer polymerization.

[0045] In some embodiments of the present invention, the initiator may be one or more of benzoyl peroxide, cumene hydroperoxide, and tert-butyl hydroperoxide.

[0046] In embodiments of the present invention, the weight fraction of the initiator provided by the present invention can be any value within the range formed by any two values ​​in the above-mentioned range, such as 0.5 parts to 1 part, or 1 part to 2 parts, and so on. The weight fraction of the initiator provided by the present invention can also be one of 0.5 parts, 0.6 parts, 0.7 parts, 0.8 parts, 0.9 parts, 1.0 parts, 1.1 parts, 1.2 parts, 1.3 parts, 1.4 parts, 1.5 parts, 1.6 parts, 1.7 parts, 1.8 parts, 1.9 parts, or 2 parts, or any value that satisfies the above-mentioned range.

[0047] Accelerator

[0048] The main function of accelerators is to speed up the curing process.

[0049] In some embodiments of the present invention, the promoter may be one or more of acetylphenylhydrazine, triethanolamine and N,N-dimethylaniline.

[0050] In embodiments of the present invention, the weight percentage of the accelerator provided by the present invention can be any value within the range formed by any two values ​​in the above-mentioned range, such as 0.1 parts to 0.5 parts, or 0.5 parts to 1 part, and so on. The weight percentage of the accelerator provided by the present invention can also be one of 0.1 parts, 0.2 parts, 0.3 parts, 0.4 parts, 0.5 parts, 0.6 parts, 0.7 parts, 0.8 parts, 0.9 parts, and 1 part, or any value satisfying the above-mentioned range.

[0051] Promoter

[0052] The main function of a promoter is to enhance the effect of a promoter.

[0053] In some embodiments of the present invention, the co-promoter may be at least one of o-benzoylsulfonylimide and substituted saccharin.

[0054] In embodiments of the present invention, the weight fraction of the accelerator provided by the present invention can be any value within the range formed by any two values ​​in the above-mentioned range, such as 0.1 parts to 0.5 parts, or 0.5 parts to 1 part, and so on. The weight fraction of the accelerator provided by the present invention can also be one of 0.1 parts, 0.2 parts, 0.3 parts, 0.4 parts, 0.5 parts, 0.6 parts, 0.7 parts, 0.8 parts, 0.9 parts, and 1 part, or any value satisfying the above-mentioned range.

[0055] In embodiments of the present invention, the anaerobic sealing liquid further includes at least one of the following components in parts by weight: 0.4 to 2 parts of a polymerization inhibitor and 0.03 to 1 part of a metal chelating agent.

[0056] In embodiments of the present invention, the raw materials of the anaerobic sealing liquid include monomers, initiators, accelerators, co-accelerators, polymerization inhibitors, metal chelating agents, and organic acids. Due to the rational formulation of monomers and various additives, the obtained anaerobic sealing liquid has a fast curing rate and excellent airtightness, pull-out strength, storage stability, and corrosion resistance.

[0057] Polymerization inhibitor

[0058] The polymerization inhibitor mainly acts as an antioxidant, which can prevent oxygen from being consumed too quickly.

[0059] In some embodiments of the present invention, the polymerization inhibitor may be one or more of p-benzoquinone, p-tert-butylcatechol, hydroquinone, and p-isopropylphenol.

[0060] In embodiments of the present invention, the weight percentage of the polymerization inhibitor provided by the present invention can be any value within the range formed by any two values ​​in the above-mentioned range, such as 0.4 parts to 1 part, or 1 part to 2 parts, and so on. The weight percentage of the polymerization inhibitor provided by the present invention can also be one of 0.4 parts, 0.5 parts, 0.6 parts, 0.7 parts, 0.8 parts, 0.9 parts, 1 part, 1.1 parts, 1.2 parts, 1.3 parts, 1.4 parts, 1.5 parts, 1.6 parts, 1.7 parts, 1.8 parts, 1.9 parts, or 2 parts, or any value that satisfies the above-mentioned range.

[0061] Metal chelating agents

[0062] Metal chelating agents can remove excess metal ions present in the adhesive, preventing the initiator from decomposing.

[0063] In some embodiments of the present invention, the metal chelating agent may be at least one of oxalic acid and disodium ethylenediaminetetraacetate.

[0064] In embodiments of the present invention, the weight parts of the metal chelating agent provided by the present invention can be any value within the range formed by any two values ​​in the above-mentioned range, for example, it can be 0.03 parts to 0.1 parts, or 0.1 parts to 1 part, and so on. The weight parts of the metal chelating agent provided by the present invention can also be one of 0.03 parts, 0.04 parts, 0.05 parts, 0.06 parts, 0.07 parts, 0.08 parts, 0.09 parts, 0.1 parts, 0.2 parts, 0.3 parts, 0.4 parts, 0.5 parts, 0.6 parts, 0.7 parts, 0.8 parts, 0.9 parts, and 1 part, or any value that satisfies the above-mentioned range.

[0065] In embodiments of the present invention, the anaerobic sealing liquid further includes 0.1 to 1 part of organic acid.

[0066] organic acids

[0067] Organic acids can promote the curing of anaerobic sealing liquids and increase the initial curing time.

[0068] In some embodiments of the present invention, the organic acid may be one or more of methacrylic acid, acetoacetic acid, oxalic acid, and pyruvic acid.

[0069] In embodiments of the present invention, the weight parts of the organic acid provided by the present invention can be any value within the range formed by any two values ​​in the above-mentioned range, such as 0.1 parts to 0.6 parts, or 0.6 parts to 1 part, and so on. The weight parts of the organic acid provided by the present invention can also be one of 0.6 parts, 0.2 parts, 0.3 parts, 0.4 parts, 0.5 parts, 0.6 parts, 0.7 parts, 0.8 parts, 0.9 parts, and 1 part, or any value that satisfies the above-mentioned range.

[0070] In embodiments of the present invention, the anaerobic sealing liquid comprises the following components by weight: 20 to 50 parts of monomer, 0.5 to 2 parts of initiator, 0.1 to 1 part of accelerator, 0.1 to 1 part of co-accelerator, 0.4 to 2 parts of polymerization inhibitor, 0.03 to 1 part of metal chelating agent, and 0.1 to 1 part of organic acid.

[0071] The second aspect of the present invention provides a method for preparing an anaerobic sealing liquid, wherein the anaerobic sealing liquid is obtained by mixing and stirring monomers and various additives in a certain proportion.

[0072] The preparation method of the anaerobic sealing liquid in this invention is carried out according to the following steps.

[0073] (1) Mix the monomer, polymerization inhibitor, metal chelating agent and organic acid according to the ratio, and heat and stir.

[0074] In some embodiments of the present invention, the heating and stirring temperature is 30°C to 60°C. For example, the heating and stirring temperature can be one of 30°C, 35°C, 40°C, 45°C, 50°C, 55°C, and 60°C, or any value satisfying the above range.

[0075] In some embodiments of the present invention, the heating and stirring speed is 300 rpm to 600 rpm. For example, the heating and stirring speed can be one of 300 rpm, 350 rpm, 400 rpm, 450 rpm, 500 rpm, 550 rpm, 600 rpm, or any value satisfying the above range.

[0076] In some embodiments of the present invention, the heating and stirring time is 2h to 5h. For example, the heating and stirring time can be one of 2h, 2.5h, 3h, 3.5h, 4h, 4.5h, and 5h, or any value that satisfies the above range.

[0077] (2) Stop heating, cool down, add accelerator, co-accelerator and initiator and continue stirring.

[0078] In some embodiments of the present invention, the stirring speed after cooling is 300 rpm to 600 rpm, and the stirring time is 1 h to 3 h. Exemplarily, the stirring speed can be one of 300 rpm, 350 rpm, 400 rpm, 450 rpm, 500 rpm, 550 rpm, or 600 rpm, or any value satisfying the above range. The stirring time can be one of 1 h, 1.5 h, 2 h, 2.5 h, or 3 h, or any value satisfying the above range.

[0079] In some embodiments of the present invention, an accelerator, a co-accelerator, and an initiator are added after cooling to room temperature, wherein room temperature usually refers to a state without active heating and cooling, for example, it can be 20°C to 30°C.

[0080] The anaerobic sealing liquid provided by the present invention, or the anaerobic sealing liquid prepared by the above preparation method, can be applied to any of the following: sealing, retaining, bonding, and plugging.

[0081] Unless otherwise defined, the technical terms used in the following embodiments have the same meaning as commonly understood by those skilled in the art. Unless otherwise specified, the experimental reagents used in the following embodiments are all conventional biochemical reagents; the raw materials, instruments, and equipment used in the following embodiments can all be obtained commercially or through existing methods; unless otherwise specified, the amounts of experimental reagents used are the amounts used in conventional experimental operations; unless otherwise specified, the experimental methods are all conventional methods.

[0082] Example 1

[0083] An anaerobic sealing liquid, by weight, comprises the following raw materials: 37 parts monomer, 1 part initiator, 0.5 parts accelerator, 0.5 parts co-accelerator, 0.4 parts polymerization inhibitor, and 0.03 parts metal chelating agent. The monomer is a combination of (4) bisphenol A dimethacrylate and hydroxypropyl methacrylate, with a weight ratio of (4) bisphenol A dimethacrylate to hydroxypropyl methacrylate of 21:16, and the viscosity of (4) bisphenol A dimethacrylate is 500 cps to 700 cps (25°C); the initiator is cumene hydroperoxide; the accelerator is acetylphenylhydrazine; the co-accelerator is o-benzoylsulfonylimide (saccharin); the polymerization inhibitor is hydroquinone; and the metal chelating agent is disodium ethylenediaminetetraacetate.

[0084] The preparation method of anaerobic sealing fluid includes the following steps:

[0085] 1) Prepare the raw materials according to the proportion, mix the monomer, polymerization inhibitor and metal chelating agent, stir at 50°C for 4 hours, and stir at 500 rpm.

[0086] 2) Stop heating, cool to room temperature, then add accelerator, co-accelerator and initiator, stir for 2 hours at a stirring speed of 500 rpm.

[0087] Example 2

[0088] The remaining operations are the same as in Example 1. The difference in Example 2 is that the monomer is a combination of bisphenol A epoxy acrylate and hydroxypropyl methacrylate, with a weight ratio of bisphenol A epoxy acrylate to hydroxypropyl methacrylate of 21:16; the viscosity of bisphenol A epoxy acrylate is 60,000 cps to 90,000 cps (25°C), and it was purchased from Guangdong Boxin New Materials Co., Ltd.

[0089] Example 3

[0090] The remaining operations are the same as in Example 1. The difference in Example 3 is that the monomer is a combination of bisphenol A epoxy acrylate and hydroxypropyl methacrylate in a weight ratio of 19:18; the viscosity of bisphenol A epoxy acrylate is 60,000 cps to 90,000 cps (25°C), and it was purchased from Guangdong Boxin New Materials Co., Ltd.

[0091] Furthermore, 0.8 parts of an organic acid, namely methacrylic acid, were added in Example 3.

[0092] Example 4

[0093] An anaerobic sealing liquid, by weight, comprises the following raw materials: 37 parts monomer, 0.8 parts initiator, 0.3 parts accelerator, 0.3 parts co-accelerator, 1 part polymerization inhibitor, 0.1 parts metal chelating agent, and 0.6 parts organic acid. Among them, the monomers are a combination of (4) bisphenol A dimethacrylate, bisphenol A epoxy acrylate and hydroxypropyl methacrylate, the weight ratio of (4) bisphenol A dimethacrylate, bisphenol A epoxy acrylate and hydroxypropyl methacrylate is 21:4:12, the viscosity of (4) bisphenol A dimethacrylate is 500cps~700cps (25℃) and the viscosity of bisphenol A epoxy acrylate is 5500cps~7500cps (25℃); the initiator is cumene hydroperoxide; the accelerator is acetylphenylhydrazine; the co-accelerator is o-benzoylsulfonylimide (saccharin); the polymerization inhibitor is hydroquinone; the metal chelating agent is disodium ethylenediaminetetraacetate; and the organic acid is methacrylic acid.

[0094] The preparation method of anaerobic sealing fluid includes the following steps:

[0095] 1) Prepare the raw materials according to the proportion, mix the monomer, polymerization inhibitor and metal chelating agent, stir at 50°C for 4 hours, and stir at 500 rpm.

[0096] 2) Stop heating, cool to room temperature, then add accelerator, co-accelerator and initiator, stir for 2 hours at a stirring speed of 500 rpm.

[0097] The proportions of each component added to the anaerobic sealing liquid in Examples 1 to 4 of this invention are detailed in Table 1.

[0098] Table 1. Components of Anaerobic Sealing Fluid

[0099]

[0100] Performance testing

[0101] Initial curing time: Anaerobic sealing liquid is used to seal steel / copper / aluminum sleeves. It is cured at an ambient temperature of (23±2)℃. The time until the sleeve cannot be turned by hand is called the initial curing time.

[0102] Viscosity: Measured using a rotational viscometer (test temperature: 25℃).

[0103] Pull-out resistance: After the sleeve to be tested is fully solidified, the test shall be carried out in accordance with the provisions of GB / T 228.

[0104] Corrosion resistance: After the sleeve to be tested is fully solidified and sealed at both ends, it is placed in a salt spray test chamber with a pH of 6.5 to 7.2, 5% ± 1% NaCl, and a temperature of 35℃ ± 2℃. The test is carried out according to the corrosion resistance time requirements of the connected pipe fittings. The sleeve is removed and observed. If there is no discoloration or corrosion spots on the outer surface of the sleeve, it is qualified; otherwise, it is unqualified.

[0105] Sealing performance: The prepared anaerobic sealing liquid is used to seal the metal sleeve. It is placed horizontally for 24 hours in an environment with a temperature of 23℃±2℃ and a relative humidity of 50%±5%. After it is completely solidified, pressure gauges and air inflators are connected to both ends of the sleeve and placed in water. Nitrogen or dry air is introduced into the sleeve and the pressure gauge is brought to the specified pressure and maintained for 3 minutes. If there are no bubbles, leaks or obvious deformation, it is considered qualified; otherwise, it is considered unqualified.

[0106] Gel time: The prepared anaerobic sealing liquid was placed in an 80℃ oven, and the time required for gelation to occur was taken as the gel time. If the gel time is 1 hour, it indicates that the anaerobic sealing liquid can be stably stored for 1 year.

[0107] The test results are shown in Table 2.

[0108] Table 2 Summary of the performance of anaerobic sealing fluid

[0109]

[0110]

[0111] Combined with appendix Figures 1-4 As shown in Table 2, the viscosity of the anaerobic sealing liquid prepared in Example 1 is 42 cps (25℃). The viscosity of the anaerobic sealing liquid is too low and it is easy to flow, resulting in insufficient adhesive at the joint. This causes a small amount of air to enter the adhesive joint (i.e., the conditions for sufficient anaerobic bonding are not met), resulting in poor curing effect. In addition, since (4) bisphenol A dimethacrylate contains ethoxy groups, the rotation of CO bonds is easier than that of C-C bonds. Therefore, the higher the CO bond content, the greater the flexibility of the polymer. The bonding strength and corrosion resistance of the anaerobic sealing liquid prepared by it will be worse, and the corrosion resistance will be unqualified.

[0112] The anaerobic sealing liquid prepared in Example 2 exhibits excellent adhesion, corrosion resistance, and bonding properties due to the presence of epoxy groups in the bisphenol A epoxy acrylate. The corrosion resistance of the prepared anaerobic sealing liquid is satisfactory. However, the residue left by the prepared anaerobic sealing liquid after sealing metal sleeves is sticky. Furthermore, the initial curing time on steel and aluminum pipes is excessively long, exceeding 30 minutes in both cases.

[0113] The anaerobic sealing liquid prepared in Example 3 exhibited satisfactory corrosion resistance. The addition of methacrylic acid indirectly promoted the curing of the anaerobic sealing liquid by generating metal ions on the metal surface, significantly increasing the initial curing time, without noticeable changes in storage stability. Furthermore, the anaerobic sealing liquid with added methacrylic acid showed significantly better curing performance on inert substrates (stainless steel, aluminum) compared to the anaerobic adhesive without methacrylic acid. However, due to the excessively high adhesive strength of bisphenol A epoxy acrylate, the residue left by the prepared anaerobic sealing liquid after sealing metal sleeves was sticky.

[0114] The anaerobic sealing liquid prepared in Example 4 has a fast initial solidification time on metal pipes and the residual adhesive is not sticky. It also meets the requirements for tensile strength, storage stability, corrosion resistance and sealing performance.

[0115] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention, and not to limit them. Although the present invention has been described in detail with reference to the foregoing embodiments, those skilled in the art should understand that modifications can still be made to the technical solutions described in the foregoing embodiments, or equivalent substitutions can be made to some or all of the technical features therein. Such modifications or substitutions do not cause the essence of the corresponding technical solutions to deviate from the scope of the technical solutions of the embodiments of the present invention.

Claims

1. An anaerobic sealing fluid, characterized in that, The anaerobic sealing fluid comprises the following components in parts by weight: 20 to 50 parts monomer, 0.5 to 2 parts initiator, 0.1 to 1 part accelerator, and 0.1 to 1 part co-accelerator; The monomers include one or more of polyurethane acrylate, bisphenol A epoxy acrylate, (4) ethylene oxide bisphenol A dimethacrylate, triethylene glycol dimethacrylate, hydroxyethyl methacrylate and hydroxypropyl methacrylate.

2. The anaerobic sealing liquid as described in claim 1, characterized in that, The monomers include a combination of at least two of the following: (4) bisphenol A epoxy acrylate, (5) ethoxylated bisphenol A dimethacrylate, and hydroxypropyl methacrylate.

3. The anaerobic sealing liquid as described in claim 2, characterized in that, The weight ratio of bisphenol A dimethacrylate and hydroxypropyl methacrylate in (4) is 19–21:12–16; and / or, The weight ratio of bisphenol A epoxy acrylate to hydroxypropyl methacrylate is 4–21:12–18.

4. The anaerobic sealing liquid as described in claim 1, characterized in that, The initiator includes one or more of benzoyl peroxide, cumene hydroperoxide, and tert-butyl hydroperoxide; and / or, The accelerator includes one or more of acetylphenylhydrazine, triethanolamine, and N,N-dimethylaniline; and / or, The co-promoter includes at least one of o-benzoylsulfonylimide and substituted saccharin.

5. The anaerobic sealing liquid according to any one of claims 1 to 4, characterized in that, The anaerobic sealing liquid further includes at least one of the following components in parts by weight: 0.4 to 2 parts of polymerization inhibitor; the polymerization inhibitor includes one or more of p-benzoquinone, p-tert-butylcatechol, hydroquinone, and p-isopropylphenol; The metal chelating agent is 0.03 to 1 part; the metal chelating agent includes at least one of oxalic acid and disodium ethylenediaminetetraacetate.

6. The anaerobic sealing liquid according to any one of claims 1 to 4, characterized in that, The anaerobic sealing liquid also includes 0.1 to 1 part of organic acid; the organic acid includes one or more of methacrylic acid, acetoacetic acid, oxalic acid and pyruvic acid.

7. A method for preparing the anaerobic sealing liquid according to any one of claims 1 to 6, characterized in that, The preparation method includes: weighing each raw material according to the weight proportions and mixing them evenly, and then stirring to prepare the anaerobic sealing liquid.

8. The method for preparing the anaerobic sealing liquid as described in claim 7, characterized in that, The preparation method includes: The anaerobic sealing liquid is prepared by mixing monomers, polymerization inhibitors, metal chelating agents and organic acids, heating and stirring, cooling, adding accelerators, co-accelerators and initiators and stirring continuously.

9. The method for preparing the anaerobic sealing liquid as described in claim 8, characterized in that, The heating and stirring temperature is 30℃~60℃, the heating and stirring speed is 300rpm~600rpm, and the heating and stirring time is 2h~5h; The stirring speed after cooling is 300 rpm to 600 rpm, and the stirring time is 1 h to 3 h.

10. The use of an anaerobic sealing liquid according to any one of claims 1 to 6, or an anaerobic sealing liquid prepared by the preparation method of the anaerobic sealing liquid according to any one of claims 7 to 9, in any of the following applications: sealing, retaining, bonding, and plugging.

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