Modified high-wear-resistance rapid repair material and preparation method thereof

Abstract

The invention relates to a modified high-wear-resistance rapid repair material and a preparation method thereof, and belongs to the technical field of composite materials. According to the invention, a long-chain alkyl structure is innovatively introduced into the curing agent, so that the hydrophobicity of the surface after the epoxy resin-based repairing material is cured can be effectively improved, and a slippage boundary effect is generated, so that the flow resistance of a fluid medium in repaired equipment is effectively reduced, and the friction force on the surface of the equipment is further reduced; the hydrophobic surface is also beneficial to inhibiting corrosion of an acid medium in the equipment to the repairing layer and the surface of the equipment and improving the durability of the repairing layer, in addition, a silane coupling agent kh-570 is grafted on the surface of the hard filler to modify the hard filler, the compatibility of the filler and an epoxy resin matrix is effectively improved, and the repairing effect is improved. The interaction between the filler and the epoxy resin matrix is enhanced, and the wear resistance of the epoxy resin repair material is effectively improved.

Description

Technical Field

[0001] This invention belongs to the field of composite material technology, specifically relating to a modified high-wear-resistant rapid repair material and its preparation method. Background Technology

[0002] In the petrochemical industry, the low-temperature reactive sulfuric acid alkylation process is one of the key technologies for producing high-octane gasoline blending components. Its core equipment, the reactor, operates continuously at high speed in a strong acid environment. Within the reactor, these media are subjected to high-speed turbulence through efficient stirring or circulating pumps to achieve thorough mixing and reaction. The high-speed flowing and highly corrosive fluid in the reactor inevitably causes continuous mechanical wear on the lining surface. Simultaneously, the strong acid in the fluid preferentially corrodes these freshly exposed surfaces or microscopic defects, accelerating the material degradation process and even leading to the complete detachment of the lining. Epoxy resin-based repair materials have the advantages of fast curing speed and resistance to acid and alkali corrosion, enabling rapid repair of worn linings and providing a reliable chemical protective barrier for damaged lining areas. However, the hardness and wear resistance of pure epoxy resin cured products are relatively limited, making it difficult to meet the stringent requirements of continuous scouring and friction by high-speed fluids inside the reactor. Introducing wear-resistant fillers with high hardness or lubricating properties can effectively improve the wear resistance of epoxy resin. However, the compatibility between wear-resistant fillers and epoxy resin matrix is ​​poor, the interfacial bonding force is usually weak, and there is a lack of effective chemical bonding or strong physical adsorption, resulting in a significant weak interfacial layer. The direct consequence of this poor compatibility is that the wear-resistant filler cannot fully exert its reinforcing effect. When subjected to high-speed fluid scouring friction or thermal stress cycling, the weak points of the interface bonding are prone to become the starting point for the initiation and propagation of microcracks, causing the filler particles to debond and peel off from the resin matrix. This not only accelerates the wear and failure of the repair layer itself, but the peeled hard particles may also become new abrasives, further aggravating the secondary wear and damage to the repair layer and even the surrounding intact lining. To solve the above technical defects, this invention provides a modified high wear-resistant rapid repair material and its preparation method. Summary of the Invention

[0003] The purpose of this invention is to provide a modified high-wear-resistant rapid repair material and its preparation method, in order to solve the problems mentioned in the background art.

[0004] The objective of this invention can be achieved through the following technical solutions:

[0005] A method for preparing a modified high-wear-resistant rapid repair material includes the following steps:

[0006] Step 1: Mix 2,5-dimethylpyrrole, long-chain olefin, sodium ethoxide, and anhydrous ethanol in a three-necked flask equipped with a condenser, thermometer, and magnetic stirrer. After turning on the magnetic stirrer, react at a temperature of 40-80℃ for 6-24 hours. After the reaction is completed, filter the mixture, remove the solvent by rotary evaporation of the filtrate, and then elute by silica gel column chromatography to obtain the hydrophobic monomer.

[0007] The second step involves mixing the hydrophobic monomer, N-bromosuccinimide, and carbon tetrachloride in a three-necked flask equipped with a condenser, thermometer, and magnetic stirrer. After turning on the magnetic stirrer, the system temperature is raised to 60–80°C. Then, an initiator is added to the three-necked flask, and the reaction is carried out at 60–80°C for 20–28 hours. After the reaction is completed, the mixture is filtered, and the solvent is removed by rotary evaporation of the chlorine solution to obtain the curing agent precursor.

[0008] Step 3: Mix hexamethylenetetramine and toluene in a three-necked flask equipped with a condenser, thermometer, and magnetic stirrer. After turning on the magnetic stirrer, add the curing agent precursor to the three-necked flask in batches. After the addition is complete, react at a temperature of 80-110℃ for 4-6 hours. Then cool to room temperature and filter under vacuum. Wash the obtained solid with anhydrous ethanol and dry it. Then transfer the product to a three-necked flask containing anhydrous ethanol and concentrated hydrochloric acid. Attach a condenser and thermometer, turn on the magnetic stirrer, and continue to react at a temperature of 75-85℃ for 6-8 hours. After the reaction is complete, remove the solvent by rotary evaporation. Wash the remaining solid with deionized water and dry it to obtain the curing agent for later use.

[0009] Step 4: Mix silane coupling agent KH-570, hard filler, and ethanol aqueous solution in a three-necked flask equipped with a condenser, thermometer, and magnetic stirrer. After turning on the magnetic stirrer, react at a temperature of 40-80℃ for 3-12 hours. After the reaction is completed, filter out the solid, wash it with anhydrous ethanol and deionized water in sequence, and then dry it to obtain the modified filler.

[0010] Step 5: Under nitrogen protection, add bisphenol F epoxy resin, trimethylolpropane triglycidyl ether, and naphthalene-type epoxy resin to a planetary mixer and mix. Then add modified filler to the planetary mixer, mix evenly, and vacuum degas before filling into a light-proof container to obtain the matrix resin for later use.

[0011] Step 6: Preheat the base resin, then add the curing agent to the base resin, stir and mix evenly to obtain the modified high wear-resistant fast repair material.

[0012] Furthermore, the long-chain olefin is one of cetene, 1-heptadecene, and 1-octadecene.

[0013] Furthermore, the initiator is one of azobisisobutyronitrile (AIBN) and benzoyl peroxide.

[0014] Furthermore, the concentrated hydrochloric acid has a mass fraction of 32-38%.

[0015] Furthermore, the hard filler is composed of a mixture of silicon carbide micro powder, micronized alumina, and molybdenum disulfide.

[0016] Preferably, the hard filler is composed of 24 to 30 parts by weight of silicon carbide micro powder, 12 to 15 parts by weight of micron-sized alumina, and 4 to 5 parts by weight of molybdenum disulfide.

[0017] Preferably, the volume fraction of the ethanol aqueous solution is 40-60%.

[0018] Furthermore, in step five, the conditions for mixing bisphenol F epoxy resin, trimethylolpropane triglycidyl ether, and naphthalene-type epoxy resin are as follows: stirring at a temperature of 40–50°C and a speed of 150–350 rpm for 10–40 minutes.

[0019] Furthermore, in step five, the conditions for mixing after adding the modified filler are: stirring at a temperature of 50–60°C and a speed of 300–800 rpm for 20–60 minutes.

[0020] Furthermore, in step six, the preheating temperature of the matrix resin is 30–40°C, and the stirring conditions are as follows: stir at a speed of 1000–1200 rpm for 60–90 seconds, then reduce the speed to 200–300 rpm and continue stirring for 30–40 seconds.

[0021] Furthermore, the mass ratio of the raw materials 2,5-dimethylpyrrole, long-chain olefin, sodium ethoxide, and anhydrous ethanol used in the first step is 10.2–11.4: 22.4–25.2: 0.14–0.21: 80–120.

[0022] Furthermore, the mass ratio of the hydrophobic monomer, N-bromosuccinimide, carbon tetrachloride, and initiator used in the second step is 25.6–27.8: 31.6–35.2: 200–240: 5.2–8.8.

[0023] Furthermore, the mass ratio of the raw materials used in the third step—hexamethylenetetramine, toluene, curing agent precursor, anhydrous ethanol, and concentrated hydrochloric acid—is 19.6–22.4: 160–180: 32.4–34.2: 120–140: 80–100.

[0024] Furthermore, in the fourth step, the mass ratio of the raw materials used—silane coupling agent KH-570, hard filler, and ethanol aqueous solution—is 4–5: 40–50: 320–400.

[0025] Furthermore, in step five, the mass ratio of bisphenol F epoxy resin, trimethylolpropane triglycidyl ether, naphthalene-type epoxy resin, and modified filler is 18–24: 5–7: 4–5: 32–44.

[0026] Furthermore, in step six, the mass ratio of the matrix resin to the curing agent is 60–80:15–20.

[0027] A modified high wear-resistant rapid repair material is prepared by any of the above preparation steps.

[0028] The beneficial effects of this invention are:

[0029] 1) This invention uses 2,5-dimethylpyrrole and long-chain olefins as raw materials. The imino group of 2,5-dimethylpyrrole reacts with the double bond of the long-chain olefin under the catalysis of sodium ethoxide to obtain a hydrophobic monomer. Then, using N-bromosuccinimide as a brominating agent, a halogenation reaction occurs under the action of an initiator, replacing the α-hydrogen in the hydrophobic monomer with a bromine atom to obtain a curing agent precursor. Finally, the bromine atom in the curing agent precursor reacts with hexamethylenetetramine via a Delépine reaction to obtain a curing agent containing two amino groups. This invention innovatively introduces a long-chain alkyl structure into the curing agent, which can effectively improve the hydrophobicity of the surface of the epoxy resin-based repair material after curing, generating a slip boundary effect that effectively reduces the flow resistance of the fluid medium inside the repaired equipment, thereby reducing the friction on the equipment surface. In addition, the hydrophobic surface also helps to inhibit the corrosion of the repair layer and the equipment surface by acidic media inside the equipment, improving the durability of the repair layer.

[0030] 2) This invention effectively improves the dispersibility of hard fillers by grafting silane coupling agent KH-570 onto the surface of the hard filler. In addition, the acryloyloxy group on the surface of the modified hard filler (providing double bonds) can undergo a reversible Diels-Alder reaction with the pyrrole structure (providing conjugated double bonds) in the curing agent. This not only effectively improves the compatibility between the filler and the epoxy resin matrix and enhances the interaction between the filler and the epoxy resin matrix, but also enhances the friction-resistant modification effect of the hard filler on the epoxy resin matrix. Furthermore, after the repair layer is subjected to friction damage, it can promptly repair the microcracks caused by friction damage, block the chain damage caused by friction loss, realize internal self-repair and reorganization, and effectively improve the wear resistance of the repair layer.

[0031] 3) The repair material of the present invention, after curing, produces a repair layer with both good hydrophobicity and self-healing properties. The hydrophobicity of the repair layer itself helps to shield the external environment (mainly water molecules) from interference with the self-healing reaction inside the repair layer, thereby improving the repair efficiency of the material itself. Meanwhile, the self-healing ability of the repair layer itself can effectively improve the stability of the hydrophobic surface under high friction rate. The synergistic effect of the two effects can effectively suppress the frictional damage of high flow rate media to the surface of the repair layer. Detailed Implementation

[0032] The technical solutions of the embodiments of this application will be clearly and completely described below. Obviously, the described embodiments are only some, not all, of the embodiments of this application. Based on the embodiments in this application specification, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection claimed in this application.

[0033] The raw materials used in this invention are not particularly restricted in terms of their source; they can be purchased from the market or prepared using conventional methods known to those skilled in the art.

[0034] Example 1

[0035] Step 1: Mix 10.2 parts by mass of 2,5-dimethylpyrrole, 22.4 parts by mass of cetene, 0.14 parts by mass of sodium ethoxide, and 80 parts by mass of anhydrous ethanol in a three-necked flask equipped with a condenser, thermometer, and magnetic stirrer. After turning on the magnetic stirrer, react at 40°C for 24 hours. After the reaction is completed, filter the mixture, remove the solvent by rotary evaporation of the filtrate, and then elute by silica gel column chromatography to obtain the hydrophobic monomer.

[0036] Step 2: By mass, 25.6 parts of hydrophobic monomer, 31.6 parts of N-bromosuccinimide, and 200 parts of carbon tetrachloride were mixed in a three-necked flask equipped with a condenser, thermometer, and magnetic stirrer. After turning on the magnetic stirrer, the system temperature was raised to 80°C. Then, 5.2 parts of benzoyl peroxide were added to the three-necked flask, and the reaction was carried out at 80°C for 28 hours. After the reaction was completed, the mixture was filtered, and the solvent was removed by rotary evaporation of chlorine to obtain the curing agent precursor.

[0037] Step 3: According to the mass fraction, 19.6 parts of hexamethylenetetramine and 160 parts of toluene were mixed in a three-necked flask equipped with a condenser, thermometer, and magnetic stirrer. After turning on the magnetic stirrer, 32.4 parts of curing agent precursor were added to the three-necked flask in batches. After the addition was completed, the mixture was reacted at 80°C for 6 hours. Then, it was cooled to room temperature and vacuum filtered. The obtained solid was washed with anhydrous ethanol and dried. The product was then transferred to a three-necked flask containing 120 parts of anhydrous ethanol and 80 parts of 38% hydrochloric acid. A condenser and thermometer were installed, and the mixture was stirred with a magnetic stirrer. The mixture was then reacted at 75°C for 8 hours. After the reaction was completed, the solvent was removed by rotary evaporation. The remaining solid was washed with deionized water and dried to obtain the curing agent for later use.

[0038] Step 4: According to the mass fraction, 4 parts of silane coupling agent KH-570, 24 parts of silicon carbide micro powder, 12 parts of micron-sized alumina, 4 parts of molybdenum disulfide, and 320 parts of 60% ethanol aqueous solution are mixed in a three-necked flask equipped with a condenser, thermometer, and magnetic stirrer. After turning on the magnetic stirrer, the mixture is reacted at 40°C for 12 hours. After the reaction is completed, the solid is filtered out and washed with anhydrous ethanol and deionized water in sequence, and then dried to obtain the modified filler.

[0039] Step 5: According to the mass fraction, under nitrogen protection, add 18 parts of bisphenol F epoxy resin, 5 parts of trimethylolpropane triglycidyl ether, and 4 parts of naphthalene-type epoxy resin to a planetary mixer and stir for 40 minutes at 40°C and 150 rpm. Then add 32 parts of modified filler to the planetary mixer and stir for 60 minutes at 50°C and 300 rpm. After vacuum degassing, fill the mixture into a light-proof container to obtain the matrix resin for later use.

[0040] Step 6: Preheat 60 parts of the base resin to 30°C by weight, then add 15 parts of the curing agent to the base resin. Stir at 1000 rpm for 90 seconds, then reduce the speed to 200 rpm and continue stirring for 40 seconds to obtain the modified high wear-resistant fast repair material.

[0041] A modified high wear-resistant rapid repair material is prepared by the above preparation steps.

[0042] Example 2

[0043] Step 1: By mass fraction, 10.8 parts of 2,5-dimethylpyrrole, 23.8 parts of 1-heptadecene, 0.175 parts of sodium ethoxide, and 100 parts of anhydrous ethanol were mixed in a three-necked flask equipped with a condenser, thermometer, and magnetic stirrer. After turning on the magnetic stirrer, the mixture was reacted at 60°C for 15 hours. After the reaction was completed, the mixture was filtered, and the solvent was removed by rotary evaporation of the filtrate. The hydrophobic monomer was then obtained by silica gel column chromatography.

[0044] Step 2: According to the mass fraction, 26.7 parts of hydrophobic monomer, 33.4 parts of N-bromosuccinimide, and 220 parts of carbon tetrachloride are mixed in a three-necked flask equipped with a condenser, thermometer, and magnetic stirrer. After turning on the magnetic stirrer, the system temperature is raised to 70°C. Then, 7 parts of azobisisobutyronitrile are added to the three-necked flask, and the reaction is carried out at 70°C for 24 hours. After the reaction is completed, the mixture is filtered, and the solvent is removed by rotary evaporation of chlorine to obtain the curing agent precursor.

[0045] Step 3: According to the mass fraction, 21 parts of hexamethylenetetramine and 170 parts of toluene were mixed in a three-necked flask equipped with a condenser, thermometer, and magnetic stirrer. After turning on the magnetic stirrer, 33.3 parts of curing agent precursor were added to the three-necked flask in batches. After the addition was completed, the mixture was reacted at 95°C for 5 hours. Then, it was cooled to room temperature and vacuum filtered. The obtained solid was washed with anhydrous ethanol and dried. The product was then transferred to a three-necked flask containing 130 parts of anhydrous ethanol and 90 parts of 35% hydrochloric acid. A condenser and thermometer were installed, and the mixture was stirred with a magnetic stirrer. The mixture was then reacted at 80°C for 7 hours. After the reaction was completed, the solvent was removed by rotary evaporation. The remaining solid was washed with deionized water and dried to obtain the curing agent for later use.

[0046] Step 4: According to the mass fraction, 4.5 parts of silane coupling agent KH-570, 27 parts of silicon carbide micro powder, 13.5 parts of micron-sized alumina, 4.5 parts of molybdenum disulfide, and 360 parts of 50% ethanol aqueous solution are mixed in a three-necked flask equipped with a condenser, thermometer, and magnetic stirrer. After turning on the magnetic stirrer, the mixture is reacted at 60°C for 6 hours. After the reaction is completed, the solid is filtered out and washed with anhydrous ethanol and deionized water in sequence, and then dried to obtain the modified filler.

[0047] Step 5: According to the mass fraction, under nitrogen protection, add 21 parts of bisphenol F epoxy resin, 6 parts of trimethylolpropane triglycidyl ether, and 4.5 parts of naphthalene-type epoxy resin to a planetary mixer and stir for 25 minutes at 45°C and 250 rpm. Then add 38 parts of modified filler to the planetary mixer and stir for 40 minutes at 55°C and 550 rpm. After vacuum degassing, fill the mixture into a light-proof container to obtain the matrix resin for later use.

[0048] Step 6: Preheat 70 parts of the base resin to 35°C by weight, then add 17.5 parts of the curing agent to the base resin. Stir at 1100 rpm for 75 seconds, then reduce the speed to 250 rpm and continue stirring for 35 seconds to obtain the modified high wear-resistant fast repair material.

[0049] A modified high wear-resistant rapid repair material is prepared by the above preparation steps.

[0050] Example 3

[0051] Step 1: By mass fraction, 11.4 parts of 2,5-dimethylpyrrole, 25.2 parts of 1-octadecene, 0.21 parts of sodium ethoxide, and 120 parts of anhydrous ethanol were mixed in a three-necked flask equipped with a condenser, thermometer, and magnetic stirrer. After turning on the magnetic stirrer, the mixture was reacted at 80°C for 6 hours. After the reaction was completed, the mixture was filtered, and the solvent was removed by rotary evaporation of the filtrate. The hydrophobic monomer was then obtained by silica gel column chromatography.

[0052] Step 2: According to the mass fraction, 27.8 parts of hydrophobic monomer, 35.2 parts of N-bromosuccinimide, and 240 parts of carbon tetrachloride were mixed in a three-necked flask equipped with a condenser, thermometer, and magnetic stirrer. After turning on the magnetic stirrer, the system temperature was raised to 60°C. Then, 8.8 parts of azobisisobutyronitrile were added to the three-necked flask, and the reaction was carried out at 60°C for 20 hours. After the reaction was completed, the mixture was filtered, and the solvent was removed by rotary evaporation of chlorine to obtain the curing agent precursor.

[0053] Step 3: According to the mass fraction, 22.4 parts of hexamethylenetetramine and 180 parts of toluene were mixed in a three-necked flask equipped with a condenser, thermometer, and magnetic stirrer. After turning on the magnetic stirrer, 34.2 parts of curing agent precursor were added to the three-necked flask in batches. After the addition was completed, the mixture was reacted at 110°C for 4 hours. Then, it was cooled to room temperature and vacuum filtered. The obtained solid was washed with anhydrous ethanol and dried. The product was then transferred to a three-necked flask containing 140 parts of anhydrous ethanol and 100 parts of 32% hydrochloric acid. A condenser and thermometer were installed, and the mixture was stirred with a magnetic stirrer. The mixture was then reacted at 85°C for 6 hours. After the reaction was completed, the solvent was removed by rotary evaporation. The remaining solid was washed with deionized water and dried to obtain the curing agent for later use.

[0054] Step 4: According to the mass fraction, mix 5 parts of silane coupling agent KH-570, 30 parts of silicon carbide micro powder, 15 parts of micron-sized alumina, 5 parts of molybdenum disulfide, and 400 parts of 40% ethanol aqueous solution in a three-necked flask equipped with a condenser, thermometer, and magnetic stirrer. After turning on the magnetic stirrer, react at 80°C for 3 hours. After the reaction is completed, filter out the solid, wash it with anhydrous ethanol and deionized water in sequence, and then dry it to obtain the modified filler.

[0055] Step 5: According to the mass fraction, under nitrogen protection, add 24 parts of bisphenol F epoxy resin, 7 parts of trimethylolpropane triglycidyl ether, and 5 parts of naphthalene-type epoxy resin to a planetary mixer and stir for 10 minutes at 50°C and 350 rpm. Then add 44 parts of modified filler to the planetary mixer and stir for 20 minutes at 60°C and 800 rpm. After vacuum degassing, fill the mixture into a light-proof container to obtain the matrix resin for later use.

[0056] Step 6: According to the mass fraction, preheat 80 parts of the base resin to 40°C, then add 20 parts of the curing agent to the base resin, stir at 1200 rpm for 60 seconds, then reduce the speed to 300 rpm and continue stirring for 30 seconds to obtain the modified high wear-resistant fast repair material.

[0057] A modified high wear-resistant rapid repair material is prepared by the above preparation steps.

[0058] Comparative Example 1

[0059] The difference between this comparative example and Example 3 is that hydrophobic long-chain alkyl groups are not introduced into the curing agent.

[0060] Step 1: By mass, 7.6 parts of 2,5-dimethylpyrrole (the amount of substance is the same as the hydrophobic monomer in Example 3), 35.2 parts of N-bromosuccinimide, and 240 parts of carbon tetrachloride were mixed in a three-necked flask equipped with a condenser, thermometer, and magnetic stirrer. After turning on the magnetic stirrer, the system temperature was raised to 60°C. Then, 8.8 parts of azobisisobutyronitrile were added to the three-necked flask, and the reaction was carried out at 60°C for 20 hours. After the reaction was completed, the mixture was filtered, and the solvent was removed by rotary evaporation of chlorine to obtain the curing agent precursor.

[0061] Step 2: According to the mass fraction, 22.4 parts of hexamethylenetetramine and 180 parts of toluene were mixed in a three-necked flask equipped with a condenser, thermometer, and magnetic stirrer. After turning on the magnetic stirrer, 17.1 parts of curing agent precursor (the amount of substance is the same as the curing agent precursor in Example 3) were added to the three-necked flask in batches. After the addition was completed, the reaction was carried out at 110°C for 4 hours. Then, it was cooled to room temperature and vacuum filtered. The obtained solid was washed with anhydrous ethanol and dried. The product was then transferred to a three-necked flask containing 140 parts of anhydrous ethanol and 100 parts of 32% concentrated hydrochloric acid. A condenser and thermometer were installed, and the magnetic stirrer was turned on. The reaction was continued at 85°C for 6 hours. After the reaction was completed, the solvent was removed by rotary evaporation. The remaining solid was washed with deionized water and dried to obtain the curing agent for later use.

[0062] Step 3: According to the mass fraction, 5 parts of silane coupling agent KH-570, 30 parts of silicon carbide micro powder, 15 parts of micron-sized alumina, 5 parts of molybdenum disulfide, and 400 parts of 40% ethanol aqueous solution are mixed in a three-necked flask equipped with a condenser, thermometer, and magnetic stirrer. After turning on the magnetic stirrer, the mixture is reacted at 80°C for 3 hours. After the reaction is completed, the solid is filtered out and washed with anhydrous ethanol and deionized water in sequence, and then dried to obtain the modified filler.

[0063] Step 4: According to the mass fraction, under nitrogen protection, add 24 parts of bisphenol F epoxy resin, 7 parts of trimethylolpropane triglycidyl ether, and 5 parts of naphthalene-type epoxy resin to a planetary mixer and stir for 10 minutes at 50°C and 350 rpm. Then add 44 parts of modified filler to the planetary mixer and stir for 20 minutes at 60°C and 800 rpm. After vacuum degassing, fill the mixture into a light-proof container to obtain the matrix resin for later use.

[0064] Step 5: According to the mass fraction, preheat 80 parts of the base resin to 40°C, then add 20 parts of the curing agent to the base resin, stir at 1200 rpm for 60 seconds, then reduce the speed to 300 rpm and continue stirring for 30 seconds to obtain the modified high wear-resistant fast repair material.

[0065] A modified high wear-resistant rapid repair material is prepared by the above preparation steps.

[0066] Comparative Example 2

[0067] The difference between this comparative example and Example 3 is that a curing agent is not prepared separately, but a commercially available sulfamic acid curing agent is used.

[0068] Step 1: According to the mass fraction, 5 parts of silane coupling agent KH-570, 30 parts of silicon carbide micro powder, 15 parts of micron-sized alumina, 5 parts of molybdenum disulfide, and 400 parts of 40% ethanol aqueous solution are mixed in a three-necked flask equipped with a condenser, thermometer, and magnetic stirrer. After turning on the magnetic stirrer, the mixture is reacted at 80°C for 3 hours. After the reaction is completed, the solid is filtered out and washed with anhydrous ethanol and deionized water in sequence, and then dried to obtain the modified filler.

[0069] Step 2: According to the mass fraction, under nitrogen protection, add 24 parts of bisphenol F epoxy resin, 7 parts of trimethylolpropane triglycidyl ether, and 5 parts of naphthalene-type epoxy resin to a planetary mixer and stir for 10 minutes at 50°C and 350 rpm. Then add 44 parts of modified filler to the planetary mixer and stir for 20 minutes at 60°C and 800 rpm. After vacuum degassing, fill the mixture into a light-proof container to obtain the matrix resin for later use.

[0070] Third step: According to the mass fraction, preheat 80 parts of the matrix resin to 40℃, then add 20 parts of sulfamic acid to the matrix resin, stir at 1200 rpm for 60 seconds, then reduce the speed to 300 rpm and continue stirring for 30 seconds to obtain the modified high wear-resistant fast repair material.

[0071] A modified high wear-resistant rapid repair material is prepared by the above preparation steps.

[0072] Experimental Example 1

[0073] After the modified high-wear-resistant rapid repair materials in Examples 1-3 and Comparative Examples 1-2 were cured, the water contact angle of the cured layer surface of each component was tested using a water contact angle tester. The higher the water contact angle, the stronger the surface hydrophobicity. A scouring resistance test was also conducted to measure the wear rate of each component cured layer after scouring. The test results are shown in Table 1.

[0074] Erosion resistance test: After weighing each component sample, record the initial weight m1 of each component sample. Then, immerse each component sample in a reaction vessel containing the test medium (the test medium is 95% concentrated sulfuric acid and isobutane with a small amount of iron sulfide impurities, and the volume ratio of concentrated sulfuric acid to isobutane is 1:1). The reaction vessel speed is 1500 rpm, the test time is 30 min, and the test is repeated 4 times. After that, take out the sample, clean and dry it, and weigh each component sample m2. Calculate the erosion wear rate e = (m1 - m2) / m1.

[0075] Table 1

[0076] project Surface water contact angle / ° Erosion wear rate / % Example 1 113 0.26 Example 2 114 0.24 Example 3 116 0.21 Comparative Example 1 72 0.45 Comparative Example 2 74 0.63

[0077] As can be seen from Table 1, the modified high wear-resistant rapid repair materials of the present invention in Examples 1 to 3 have good hydrophobic and wear-resistant properties after curing. However, the modified high wear-resistant rapid repair material in Comparative Example 1, due to the lack of hydrophobic modification, cannot reduce the resistance of the fluid medium and lacks effective protection for the interior of the repair layer, so the cured repair layer cannot fully exert its self-healing effect.

[0078] The descriptions of the above embodiments are merely illustrative of the methods and core ideas of the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the general principles defined herein may be implemented in other embodiments without departing from the spirit or scope of the invention. Therefore, the present invention is not to be limited to the embodiments shown herein, but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.

Claims

1. A method for preparing a modified high-wear-resistant rapid repair material, characterized in that, Includes the following steps: A hydrophobic monomer was obtained by Michael addition reaction of 2,5-dimethylpyrrole with a long-chain olefin. The hydrophobic monomer was then halogenated with N-bromosuccinimide to obtain a curing agent precursor. The curing agent precursor was then reacted with hexamethylenetetramine via a Delépine reaction to obtain the curing agent. A modified filler was obtained by modifying a hard filler with a silane coupling agent KH-570. Bisphenol F epoxy resin, trimethylolpropane triglycidyl ether, and naphthalene-type epoxy resin were mixed under nitrogen protection. The modified filler was then added and the mixture was stirred to obtain a matrix resin. The matrix resin was preheated and then stirred together with the curing agent to obtain a modified high-wear-resistant, fast-repairing material.

2. The method for preparing a modified high-wear-resistant rapid repair material according to claim 1, characterized in that, The long-chain olefin is one of cetene, 1-heptadecene, and 1-octadecene.

3. The method for preparing a modified high-wear-resistant rapid repair material according to claim 1, characterized in that, The initiator is one of azobisisobutyronitrile (AIBN) and benzoyl peroxide.

4. The method for preparing a modified high-wear-resistant rapid repair material according to claim 1, characterized in that, By mass fraction, the rigid filler is composed of 24-30 parts silicon carbide micro powder, 12-15 parts micron alumina, and 4-5 parts molybdenum disulfide. The mass fraction ratio of bisphenol F epoxy resin, trimethylolpropane triglycidyl ether, naphthalene-type epoxy resin, and modified filler is 18-24:5-7:4-5:32-44, and the mass fraction ratio of matrix resin to curing agent is 60-80:15-20.

5. The method for preparing a modified high-wear-resistant rapid repair material according to claim 1, characterized in that, The mixing conditions after adding bisphenol F epoxy resin, trimethylolpropane triglycidyl ether, and naphthalene-type epoxy resin are: stirring at a temperature of 40–50°C and a speed of 150–350 rpm for 10–40 minutes.

6. The method for preparing a modified high-wear-resistant rapid repair material according to claim 1, characterized in that, The mixing conditions after adding the modified filler are: stirring at a temperature of 50–60℃ and a speed of 300–800 rpm for 20–60 minutes.

7. The method for preparing a modified high-wear-resistant rapid repair material according to claim 1, characterized in that, The preheating temperature of the matrix resin is 30-40℃. The mixing conditions are: stirring at 1000-1200 rpm for 60-90 seconds, then reducing the speed to 200-300 rpm and continuing to stir for 30-40 seconds.

8. The method for preparing a modified high-wear-resistant rapid repair material according to claim 1, characterized in that, The mass ratio of 2,5-dimethylpyrrole to long-chain olefin is 10.2–11.4:22.4–25.2, the mass ratio of hydrophobic monomer to N-bromosuccinimide is 25.6–27.8:31.6–35.2, and the mass ratio of hexamethylenetetramine to curing agent precursor is 19.6–22.4:32.4–34.

2.

9. The method for preparing a modified high-wear-resistant rapid repair material according to claim 1, characterized in that, The mass ratio of silane coupling agent KH-570 to rigid filler is 4-5:40-50.

10. A modified high-wear-resistant and rapid repair material, characterized in that, The modified high wear-resistant and fast-repairing material is prepared by the preparation method described in any one of claims 1 to 9.