Concrete wetting agent, method of preparation and use

Abstract

The present application relates to the technical field of concrete admixtures, in particular to a concrete wetting agent, a preparation method and application. The present application overcomes the problem of poor effect of existing wetting agents in improving the early strength and flow performance of concrete. The present application obtains a pre-complex mother liquor by adding an auxiliary component and triethanolamine to deionized water under normal temperature conditions and stirring; keeps stirring, adds a polyether component to the pre-complex mother liquor and stirs again, then raises the temperature for heat preservation treatment, and after the end, cools to obtain a concrete wetting agent; wherein the auxiliary component is prepared from polyethylene glycol monomethyl ether as a raw material; the polyether component is prepared by mixing an alkali catalyst and an alcohol amine, adding a fatty acid methyl ester to obtain a mixture intermediate, then mixing the mixture intermediate with a magnesium-aluminum composite catalyst and reacting with ethylene oxide. The concrete wetting agent prepared by the present application has strong effect in improving the early strength and flow performance of concrete, and is suitable for application in early strength concrete.

Description

Technical Field

[0001] This invention relates to the field of concrete admixture technology, specifically to a concrete wetting agent, its preparation method, and its application. Background Technology

[0002] The production process of novel wall materials, such as the casting and molding of precast panels, places special requirements on the performance of the concrete mixture. In this field, polyether compounds are often used as wetting agents to improve the dispersibility of the concrete paste and ensure its smooth filling of the mold. These wetting agents adsorb onto the surface of cement particles through polyether segments in their molecular structure, creating a steric hindrance effect that imparts excellent initial fluidity to the concrete. However, while pursuing fluidity, existing polyether wetting agents have limited contribution to improving the early strength of concrete. The production efficiency of novel wall materials directly depends on the demolding speed, and slow early strength development has become a key technical bottleneck restricting rapid demolding and improving production turnover.

[0003] Existing polyether wetting agents primarily focus on physical dispersion, while insufficiently considering their chemical promoting effect on accelerating the early hydration reaction of cement. Although some modification schemes introduce functional groups that can promote hydration, this often comes at the cost of reduced dispersibility, leading to decreased concrete fluidity and failure to meet molding process requirements. This contradiction between early strength and flowability stems from the relatively simple molecular structure and mechanism of action of existing polyether wetting agents. Therefore, developing polyether wetting agents that can significantly improve the early hydration rate and strength of concrete without reducing fluidity is a pressing technical problem to be solved in the field of preparing high-performance new wall materials.

[0004] Therefore, a concrete wetting agent, its preparation method, and its application are proposed. Summary of the Invention

[0005] The purpose of this invention is to provide a concrete wetting agent, its preparation method, and its application. This invention involves adding an additive component and triethanolamine to deionized water at room temperature and stirring to obtain a pre-complex mother liquor. While maintaining stirring, a polyether component is added to the pre-complex mother liquor and stirred again. The temperature is then increased and maintained for heat treatment. After cooling, the concrete wetting agent is obtained. The additive component is prepared from polyethylene glycol monomethyl ether and maleic anhydride. The polyether component is prepared by first mixing an alkaline catalyst and an alcoholic amine, then adding fatty acid methyl ester to obtain a mixture intermediate. This mixture intermediate is then mixed with a magnesium-aluminum composite catalyst and reacted with ethylene oxide. The concrete wetting agent finally prepared by this invention has a strong effect on improving the early strength and flow properties of concrete, making it suitable for application in early-strength concrete.

[0006] To achieve the above objectives, the present invention provides the following technical solution:

[0007] Unless otherwise specified in the instructions, all parts are by mass.

[0008] On one hand, the present invention provides a method for preparing a concrete wetting agent, specifically including the following steps:

[0009] At room temperature, add 4-8 parts of additive components and 6-12 parts of triethanolamine to 70-90 parts of deionized water and stir for 30-40 minutes at room temperature to obtain a pre-complex mother liquor; while stirring, add 30-40 parts of polyether components to the pre-complex mother liquor and stir again for 30-40 minutes, then raise the temperature to 50-80℃ and keep it warm for 1-3 hours, and then cool to obtain a concrete wetting agent;

[0010] The auxiliary component is prepared from polyethylene glycol monomethyl ether and maleic anhydride as raw materials;

[0011] The polyether component is prepared from fatty acid methyl esters, alkanolamines, and ethylene oxide.

[0012] Preferably, the preparation method of the auxiliary component is as follows: polyethylene glycol monomethyl ether (number average molecular weight 2000 g / mol) is added to a reaction vessel, hydroquinone monomethyl ether is added under nitrogen protection and heated to 80-90°C; p-toluenesulfonic acid is added to the melt and stirred again; then maleic anhydride is added in two portions, with an interval of 30 min between the two portions; the reaction temperature is raised to 110-130°C and reacted under nitrogen protection for 2-4 h; after the reaction is completed, heating is stopped, and the product is cooled under continuous stirring and nitrogen protection to obtain the auxiliary component, wherein the molar ratio of maleic anhydride to polyethylene glycol monomethyl ether is 1.05-1.15:1; the amount of hydroquinone monomethyl ether added is 0.06%-0.1% of the total mass of polyethylene glycol monomethyl ether and maleic anhydride; and the amount of p-toluenesulfonic acid added is 0.1%-0.2% of the total mass of polyethylene glycol monomethyl ether and maleic anhydride.

[0013] Preferably, the preparation method of the polyether component is as follows: An alkaline catalyst and an alkanolamine are added to a reaction vessel and stirred. After purging with nitrogen three times, the temperature is raised to 60°C and reacted for 30 minutes. Then, fatty acid methyl ester is added to the reaction vessel, purged again with nitrogen, and evacuated to a vacuum, maintaining a vacuum degree of -0.06 to -0.09 MPa. The temperature of the reaction vessel is raised to a constant temperature, maintained at 80-120°C, for a reaction time of 3-6 hours. After the reaction is completed, heating is stopped, nitrogen is introduced to break the vacuum, and the mixture is cooled to 60°C before being discharged to obtain a mixed intermediate. The molar ratio of fatty acid methyl ester to alkanolamine is 1.1-1.2:1; the amount of alkaline catalyst is 0.2%-0.6% of the total mass of fatty acid methyl ester and alkanolamine.

[0014] The intermediate mixture and the magnesium-aluminum composite catalyst (catalyst structure 2.5MgO.Al2O3.nH2O, model Kyowado 300, manufactured by Kyowa Chemical Industry Co., Ltd.) were added together into a high-pressure ethoxylation reactor. After purging with nitrogen, the reactor was heated and vacuum dehydrated at 120°C until the moisture content was ≤0.05%. After dehydration, the temperature was raised to 140°C, and ethylene oxide was slowly introduced. After the ethylene oxide was introduced, the reactor was kept at this temperature for 30-40 minutes for aging. After the reaction was completed, heating was stopped, and the temperature was lowered to 60°C before the product was discharged from the reactor under nitrogen pressure to obtain the polyether component. The ratio of the sum of the molar numbers of ethylene oxide and fatty acid alkanolamide and fatty acid methyl ester in the intermediate mixture was 3-6:1. The amount of magnesium-aluminum composite catalyst was 0.2%-0.5% of the total mass of fatty acid methyl ester, alkanolamide, and ethylene oxide.

[0015] Preferably, the alkaline catalyst is one or more of potassium hydroxide, sodium hydroxide, sodium methoxide, or potassium methoxide.

[0016] Preferably, the fatty acid methyl ester is a C12-C14 fatty acid methyl ester or a C16-C18 fatty acid methyl ester.

[0017] Preferably, the alcohol amine is ethanolamine or diethanolamine.

[0018] Secondly, the present invention provides a concrete wetting agent, specifically comprising the following components: the concrete wetting agent includes an additive component, triethanolamine, a polyether component, and deionized water;

[0019] The auxiliary components include polyethylene glycol monomethyl ether, maleic anhydride, and hydroquinone monomethyl ether.

[0020] The polyether components include fatty acid methyl esters, alkanolamines, and ethylene oxide.

[0021] Thirdly, the present invention provides an application of a concrete wetting agent, which is applied to early-strength concrete.

[0022] Compared with the prior art, the beneficial effects of the present invention are as follows:

[0023] 1. This invention prepares a core polyether surfactant with both wetting and steric hindrance effects through amidation and ethoxylation reactions. Excess fatty acid methyl ester reacts with ethylene oxide to generate a surfactant that reduces the surface tension of the mixing water. When incorporated into concrete, it can control the air content of the concrete and has good wetting function. It can quickly penetrate into the interior of cement particles, shorten the cement hydration time, and improve early strength. At the same time, the fatty acid alkanolamide polyether increases the hydrophilicity and steric hindrance of fatty acid alkanolamide, which is more conducive to the dispersion and hydration process between cement particles.

[0024] 2. To overcome the mutual interference between different components, carboxyl-terminated polyether ester, as an auxiliary component, is premixed to preferentially form a pre-complex by utilizing the strong interaction between its terminal carboxyl group and the synergistic synergist triethanolamine. This pre-positions the chemical coagulation core and the foam stabilizing and enhancing agent at the molecular level, creating the necessary conditions for the subsequent efficient and orderly combination with the core polyether.

[0025] 3. This invention employs a stepwise method to prepare the wetting agent. Through heat preservation treatment, the polyether component can effectively achieve efficient intermolecular association with the polyether chains of the additive component in the pre-complex via its polyether chains, forming an ordered structure with the steric hindrance chains of the polyether component as the shell and the additive component-triethanolamine complex as the core. This process ensures that the final product is a structurally stable and synergistically performing ternary composite, enabling it to function as a functional unit in concrete, thus improving the reliability and batch stability of product performance.

[0026] 4. The ternary composite prepared by this invention has a structure in which the polyether component is precisely positioned around the chemically accelerating component, triethanolamine. In concrete, the polyether component of this structure disperses cement particles, creating channels for the triethanolamine to contact the surface of the cement minerals. This synergistic effect of steric dispersion and chemical acceleration in time and space reduces the mutual interference between water-reducing and early-strength components in traditional admixtures, simultaneously improving the early strength and flowability of concrete.

[0027] 5. During concrete mixing, the ternary composite of this invention can self-assemble at the gas-liquid interface to form a composite adsorption membrane consisting of a core gas-entraining polyether component with molecular intercalation and enhanced by an additive component and a triethanolamine complex. This composite membrane has high mechanical strength and viscoelasticity, and can form stable microbubble walls, effectively resisting physical shear and chemical damage. This results in the construction of a uniformly sized, durable, and stable microbubble system in concrete, solving the problems of poor gas entrainment stability and difficulty in controlling gas content. Attached Figure Description

[0028] Figure 1 The bar chart shows the gas content test results of Examples 1-5 and Comparative Examples 1-2, 5-6 and 8 of the present invention. Detailed Implementation

[0029] The technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.

[0030] Please see Figure 1 This invention provides a concrete wetting agent, its preparation method, and its application. The technical solution is as follows:

[0031] Example 1

[0032] Preparation of auxiliary components

[0033] 100 parts of polyethylene glycol monomethyl ether were added to a reaction vessel, and the polymerization inhibitor hydroquinone monomethyl ether was added under nitrogen protection and heated to 80°C. The catalyst p-toluenesulfonic acid was added to the melt and stirred again. Then, 5.15 parts of maleic anhydride were added in two portions, with a 30-minute interval between the two additions. The reaction temperature was raised to 110°C and the reaction was carried out under nitrogen protection for 4 hours. After the reaction was completed, heating was stopped, and the product was cooled under continuous stirring and nitrogen protection before being discharged. The amount of hydroquinone monomethyl ether added was 0.06% of the total mass of polyethylene glycol monomethyl ether and maleic anhydride; the amount of p-toluenesulfonic acid added was 0.1% of the total mass of polyethylene glycol monomethyl ether and maleic anhydride.

[0034] Preparation of polyether components

[0035] Potassium hydroxide and 100 parts of ethanolamine were added to a reaction vessel and stirred. After purging with nitrogen three times, the temperature was raised to 60℃ and reacted for 30 minutes. After the potassium hydroxide was completely dissolved, 411 parts of C12-C14 fatty acid methyl esters were added to the vessel. After purging with nitrogen again, a vacuum was drawn and maintained at -0.06 MPa. The temperature of the reaction vessel was increased and the reaction was carried out at a constant temperature of 80℃ for 6 hours. After the reaction was completed, heating was stopped, nitrogen was introduced to break the vacuum, and the temperature was lowered to 60℃ before discharging to obtain the intermediate mixture. The amount of potassium hydroxide used was 0.2% of the total mass of fatty acid methyl esters and ethanolamine.

[0036] The intermediate mixture and the magnesium-aluminum composite catalyst were added together into a high-pressure ethoxylation reactor. After purging with nitrogen, the reactor was heated and vacuum dehydrated at 120°C until the moisture content was ≤0.05%. After dehydration, the temperature was raised to 140°C, and 357 parts of ethylene oxide were slowly introduced. After the ethylene oxide was introduced, the reactor was kept at the same temperature for 30 minutes for aging. After the reaction was completed, heating was stopped, and the temperature was lowered to 60°C before the product was discharged from the reactor under nitrogen pressure to obtain the polyether component. The ratio of the molar amounts of ethylene oxide to the sum of the molar amounts of fatty acid alkanolamide and fatty acid methyl ester in the intermediate mixture was 4.5:1. The amount of magnesium-aluminum composite catalyst was 0.2% of the total mass of C12-C14 fatty acid methyl ester, ethanolamine, and ethylene oxide.

[0037] Preparation of concrete wetting agent

[0038] At room temperature, 4 parts of additive components and 6 parts of triethanolamine were added to 70 parts of deionized water and stirred at room temperature for 30 minutes to obtain a pre-complex mother liquor. While stirring, 30 parts of polyether components were added to the pre-complex mother liquor and stirred again for 30 minutes. Then, the temperature was raised to 50°C and kept for 3 hours. After the treatment, the mixture was cooled to obtain a concrete wetting agent.

[0039] Example 2

[0040] Preparation of auxiliary components

[0041] 100 parts of polyethylene glycol monomethyl ether were added to a reaction vessel, and hydroquinone monomethyl ether was added under nitrogen protection and heated to 85°C. p-Toluenesulfonic acid was added to the melt and stirred again. Then, 5.39 parts of maleic anhydride were added in two portions, with a 30-minute interval between the two additions. The reaction temperature was raised to 120°C and the reaction was carried out under nitrogen protection for 3 hours. After the reaction was completed, heating was stopped, and the product was cooled under continuous stirring and nitrogen protection before being discharged. The amount of hydroquinone monomethyl ether added was 0.08% of the total mass of polyethylene glycol monomethyl ether and maleic anhydride; the amount of p-toluenesulfonic acid added was 0.15% of the total mass of polyethylene glycol monomethyl ether and maleic anhydride.

[0042] Preparation of polyether components

[0043] Sodium methoxide and 100 parts of diethanolamine were added to a reaction vessel and stirred. After purging with nitrogen three times, the temperature was raised to 60°C and reacted for 30 minutes. After the sodium methoxide was completely dissolved, 249 parts of C12-C14 fatty acid methyl esters were added to the vessel. After purging with nitrogen again, a vacuum was drawn and maintained at -0.09 MPa. The temperature of the reaction vessel was raised and kept at 100°C for 4.5 hours. After the reaction was completed, heating was stopped, nitrogen was introduced to break the vacuum, and the temperature was lowered to 60°C before discharging to obtain the intermediate mixture. The amount of sodium methoxide used was 0.4% of the total mass of fatty acid methyl esters and diethanolamine.

[0044] The intermediate mixture and the magnesium-aluminum composite catalyst were added together into a high-pressure ethoxylation reactor. After purging with nitrogen, the reactor was heated and vacuum dehydrated at 120°C until the moisture content was ≤0.05%. After dehydration, the temperature was raised to 140°C, and 289 parts of ethylene oxide were slowly introduced. After the ethylene oxide was introduced, the reactor was kept at the same temperature for 30 minutes for aging. After the reaction was completed, heating was stopped, and the temperature was lowered to 60°C before the product was discharged from the reactor under nitrogen pressure to obtain the polyether component. The ratio of the sum of the molar amounts of ethylene oxide and fatty acid alkanolamide and fatty acid methyl ester in the intermediate mixture was 6:1. The amount of magnesium-aluminum composite catalyst was 0.2% of the total mass of C12-C14 fatty acid methyl ester, diethanolamine, and ethylene oxide.

[0045] Preparation of concrete wetting agent

[0046] At room temperature, 6 parts of additive components and 10 parts of triethanolamine were added to 80 parts of deionized water and stirred at room temperature for 35 minutes to obtain a pre-complex mother liquor. While stirring, 35 parts of polyether components were added to the pre-complex mother liquor and stirred again for 35 minutes. Then, the temperature was raised to 65°C and kept warm for 2 hours. After the treatment, the mixture was cooled to obtain a concrete wetting agent.

[0047] Example 3

[0048] Preparation of auxiliary components

[0049] 100 parts of polyethylene glycol monomethyl ether were added to a reaction vessel, and hydroquinone monomethyl ether was added under nitrogen protection and heated to 85°C. p-Toluenesulfonic acid was added to the melt and stirred again. Then, 5.39 parts of maleic anhydride were added in two portions, with a 30-minute interval between the two additions. The reaction temperature was raised to 120°C and the reaction was carried out under nitrogen protection for 3 hours. After the reaction was completed, heating was stopped, and the product was cooled under continuous stirring and nitrogen protection before being discharged. The amount of hydroquinone monomethyl ether added was 0.08% of the total mass of polyethylene glycol monomethyl ether and maleic anhydride; the amount of p-toluenesulfonic acid added was 0.15% of the total mass of polyethylene glycol monomethyl ether and maleic anhydride.

[0050] Preparation of polyether components

[0051] Sodium methoxide and 100 parts of ethanolamine were added to a reaction vessel and stirred. After purging with nitrogen three times, the temperature was raised to 60°C and reacted for 30 minutes. After the sodium methoxide was completely dissolved, 554 parts of C16-C18 fatty acid methyl esters were added to the vessel. After purging with nitrogen again, a vacuum was drawn and maintained at -0.09 MPa. The temperature of the reaction vessel was raised and kept at 100°C for 4.5 hours. After the reaction was completed, heating was stopped, nitrogen was introduced to break the vacuum, and the temperature was lowered to 60°C before discharging to obtain the intermediate mixture. The amount of sodium methoxide used was 0.4% of the total mass of fatty acid methyl esters and ethanolamine.

[0052] The intermediate mixture and the magnesium-aluminum composite catalyst were added together into a high-pressure ethoxylation reactor. After purging with nitrogen, the reactor was heated and vacuum dehydrated at 120°C until the moisture content was ≤0.05%. After dehydration, the temperature was raised to 140°C, and 519 parts of ethylene oxide were slowly introduced. After the ethylene oxide was introduced, the reactor was kept at the same temperature for 30 minutes for aging. After the reaction was completed, heating was stopped, and the temperature was lowered to 60°C before the product was discharged from the reactor under nitrogen pressure to obtain the polyether component. The ratio of the sum of the molar amounts of ethylene oxide and fatty acid alkanolamide and fatty acid methyl ester in the intermediate mixture was 6:1. The amount of magnesium-aluminum composite catalyst was 0.2% of the total mass of C12-C14 fatty acid methyl ester, ethanolamine, and ethylene oxide.

[0053] Preparation of concrete wetting agent

[0054] At room temperature, 6 parts of additive components and 10 parts of triethanolamine were added to 80 parts of deionized water and stirred at room temperature for 40 minutes to obtain a pre-complex mother liquor. While stirring, 35 parts of polyether components were added to the pre-complex mother liquor and stirred again for 35 minutes. Then, the temperature was raised to 65°C and kept for 2 hours. After the treatment, the concrete wetting agent was obtained by cooling.

[0055] Example 4

[0056] Preparation of auxiliary components

[0057] 100 parts of polyethylene glycol monomethyl ether were added to a reaction vessel, and hydroquinone monomethyl ether was added under nitrogen protection and heated to 90°C. p-Toluenesulfonic acid was added to the melt and stirred again. Then, 5.64 parts of maleic anhydride were added in two portions, with a 30-minute interval between the two additions. The reaction temperature was raised to 130°C and the reaction was carried out under nitrogen protection for 4 hours. After the reaction was completed, heating was stopped, and the product was cooled under continuous stirring and nitrogen protection before being discharged. The amount of hydroquinone monomethyl ether added was 0.1% of the total mass of polyethylene glycol monomethyl ether and maleic anhydride; the amount of p-toluenesulfonic acid added was 0.2% of the total mass of polyethylene glycol monomethyl ether and maleic anhydride.

[0058] Preparation of polyether components

[0059] Sodium hydroxide and 100 parts of diethanolamine were added to a reaction vessel and stirred. After purging with nitrogen three times, the temperature was raised to 60°C and reacted for 30 minutes. After the sodium hydroxide was completely dissolved, 249 parts of C12-C14 fatty acid methyl esters were added to the vessel. After purging with nitrogen again, a vacuum was drawn and maintained at -0.09 MPa. The temperature of the reaction vessel was raised and kept at 120°C for 3 hours. After the reaction was completed, heating was stopped, nitrogen was introduced to break the vacuum, and the temperature was lowered to 60°C before discharging to obtain the intermediate mixture. The amount of sodium hydroxide used was 0.6% of the total mass of fatty acid methyl esters and diethanolamine.

[0060] The intermediate mixture and the magnesium-aluminum composite catalyst were added together into a high-pressure ethoxylation reactor. After purging with nitrogen, the reactor was heated and vacuum dehydrated at 120°C until the moisture content was ≤0.05%. After dehydration, the temperature was raised to 140°C, and 144 parts of ethylene oxide were slowly introduced. After the ethylene oxide was introduced, the reactor was kept at the same temperature for 30 minutes for aging. After the reaction was completed, heating was stopped, and the temperature was lowered to 60°C before the product was discharged from the reactor under nitrogen pressure to obtain the polyether component. The ratio of the sum of the molar amounts of ethylene oxide and fatty acid alkanolamide and fatty acid methyl ester in the intermediate mixture was 3:1. The amount of magnesium-aluminum composite catalyst was 0.5% of the total mass of C16-C18 fatty acid methyl ester, diethanolamine, and ethylene oxide.

[0061] Preparation of concrete wetting agent

[0062] At room temperature, 8 parts of additive components and 12 parts of triethanolamine were added to 90 parts of deionized water and stirred at room temperature for 40 minutes to obtain a pre-complex mother liquor. While stirring, 40 parts of polyether components were added to the pre-complex mother liquor and stirred again for 40 minutes. Then, the temperature was raised to 80°C and kept warm for 1 hour. After the treatment, the mixture was cooled to obtain a concrete wetting agent.

[0063] Example 5

[0064] Preparation of auxiliary components

[0065] 100 parts of polyethylene glycol monomethyl ether were added to a reaction vessel, and hydroquinone monomethyl ether was added under nitrogen protection and heated to 90°C. p-Toluenesulfonic acid was added to the melt and stirred again. Then, 5.64 parts of maleic anhydride were added in two portions, with a 30-minute interval between the two additions. The reaction temperature was raised to 130°C and the reaction was carried out under nitrogen protection for 4 hours. After the reaction was completed, heating was stopped, and the product was cooled under continuous stirring and nitrogen protection before being discharged. The amount of hydroquinone monomethyl ether added was 0.1% of the total mass of polyethylene glycol monomethyl ether and maleic anhydride; the amount of p-toluenesulfonic acid added was 0.2% of the total mass of polyethylene glycol monomethyl ether and maleic anhydride.

[0066] Preparation of polyether components

[0067] Sodium hydroxide and 100 parts of ethanolamine were added to a reaction vessel and stirred. After purging with nitrogen three times, the temperature was raised to 60°C and reacted for 30 minutes. After the sodium hydroxide was completely dissolved, 531 parts of C16-C18 fatty acid methyl esters were added to the vessel. After purging with nitrogen again, a vacuum was drawn and maintained at -0.09 MPa. The temperature of the reaction vessel was increased and the reaction was carried out at a constant temperature of 120°C for 3 hours. After the reaction was completed, heating was stopped, nitrogen was introduced to break the vacuum, and the temperature was lowered to 60°C before discharging to obtain the intermediate mixture. The amount of sodium hydroxide used was 0.6% of the total mass of fatty acid methyl esters and ethanolamine.

[0068] The intermediate mixture and the magnesium-aluminum composite catalyst were added together into a high-pressure ethoxylation reactor. After purging with nitrogen, the reactor was heated and vacuum dehydrated at 120°C until the moisture content was ≤0.05%. After dehydration, the temperature was raised to 140°C, and 249 parts of ethylene oxide were slowly introduced. After the ethylene oxide was introduced, the reactor was kept at the same temperature for 30 minutes for aging. After the reaction was completed, heating was stopped, and the temperature was lowered to 60°C before the product was discharged from the reactor under nitrogen pressure to obtain the polyether component. The ratio of the molar amounts of ethylene oxide to the sum of the molar amounts of fatty acid alkanolamide and fatty acid methyl ester in the intermediate mixture was 3:1. The amount of magnesium-aluminum composite catalyst was 0.5% of the total mass of C16-C18 fatty acid methyl ester, ethanolamine, and ethylene oxide.

[0069] Preparation of concrete wetting agent

[0070] At room temperature, 8 parts of additive components and 12 parts of triethanolamine were added to 90 parts of deionized water and stirred at room temperature for 40 minutes to obtain a pre-complex mother liquor. While stirring, 40 parts of polyether components were added to the pre-complex mother liquor and stirred again for 40 minutes. Then, the temperature was raised to 80°C and kept warm for 1 hour. After the treatment, the mixture was cooled to obtain a concrete wetting agent.

[0071] The only difference between Comparative Example 1 and Example 1 is that no additives are added during the preparation of the concrete wetting agent.

[0072] The only difference between Comparative Example 2 and Example 1 is that triethanolamine is not added during the preparation of the concrete wetting agent.

[0073] The only difference between Comparative Example 3 and Example 1 is that in the preparation process of the concrete wetting agent, the polyether component, the auxiliary component, and the triethanolamine are directly mixed and then the temperature is raised to 50°C for heat preservation for 3 hours.

[0074] The only difference between Comparative Example 4 and Example 1 is that no heat preservation treatment is performed during the preparation of the concrete wetting agent.

[0075] The only difference between Comparative Example 5 and Example 1 is that hydroquinone monomethyl ether is not added during the preparation of the auxiliary component.

[0076] The only difference between Comparative Example 6 and Example 1 is that the molar ratio of fatty acid methyl ester to alkanolamine is 0.9:1 during the preparation of the polyether component.

[0077] The only difference between Comparative Example 7 and Example 1 is that no magnesium-aluminum composite catalyst is added during the preparation of the polyether component.

[0078] The only difference between Comparative Example 8 and Example 1 is that, in the preparation process of the polyether component, when mixing the original mixture intermediate and the magnesium-aluminum composite catalyst, an equal amount of potassium hydroxide is used to replace the magnesium-aluminum composite catalyst.

[0079] Test Example 1

[0080] Test subjects: Concrete wetting agents prepared in Examples 1-5 and Comparative Examples 1-3 and 6-8.

[0081] Test method: The compressive strength was determined according to the "Concrete Early Strength Agent" standard T / CECS 10124-2021. The concrete mix proportion was: cement 211 kg / m³. 3 70kg / m³ of fly ash 3 70kg / m³ of mineral powder 3 , sand 836kg / m 3 Stone 1073kg / m 3 159 kg / m³ of water 3The water-reducing agent was a polycarboxylate-based high-performance water-reducing agent (model ZT1906-CP01, manufactured by Wanwoxin Technology Branch of China Railway 19th Bureau Group Sixth Engineering Co., Ltd.). The final test results are shown in Table 1.

[0082] Table 1. Results of Concrete Compressive Strength Test

[0083]

[0084] This set of comparative examples aims to verify the mechanism by which the present invention enhances the early compressive strength of concrete. Comparative Example 1 lacks a molecular bridging agent, resulting in the inability to effectively pre-locate triethanolamine, making it easily adsorbed and deactivated by cement minerals, thus weakening its hydration-promoting effect. Comparative Example 2 removes triethanolamine, causing the system to lose its chemical setting-promoting function and slowing down early strength development. Comparative Example 3 uses an incorrect mixing sequence, resulting in the polyether component failing to be precisely positioned around the triethanolamine, leading to disordered molecular assembly structure and weakening the synergistic channel construction effect of physical dispersion on chemical setting. In Comparative Example 6, due to the insufficient amount of fatty acid methyl ester, the final polyether component lacks a crucial wetting component, reducing its physical effects of penetrating cement particles and promoting initial hydration. Comparative Example 8 uses potassium hydroxide instead of a magnesium-aluminum composite catalyst, and similarly, due to catalytic selectivity issues, the polyether component lacks the wetting component generated from excess fatty acid methyl ester. Comparative Example 7 lacks a catalyst, resulting in a reduced yield of the polyether component and affecting the final performance.

[0085] There is a logical connection between the comparative examples in this group. Comparative Examples 6 and 8 demonstrate from the source of material preparation that a specific composite polyether structure is the foundation for achieving physical coagulation. The lack of key points such as raw material ratios or specific catalysts will lead to the loss of this basic function. Building on this, Comparative Examples 1 and 2 demonstrate that even with qualified polyether components, a synergistic system for chemical coagulation cannot be constructed without molecular bridging agents or triethanolamine. Finally, Comparative Example 3, through a comparison of process paths, demonstrates that even with all components present, an ordered supramolecular structure capable of spatiotemporal synergy can only be formed through the specific multi-step coupling process of this invention. From the functional basis of a single component to the synergistic construction of a ternary system, and then to the optimization of synergistic efficiency by a specific process, this group of comparative examples progressively and systematically demonstrates the technical structure of this invention in improving early strength.

[0086] Test Example 2

[0087] Test subjects: Concrete wetting agents prepared in Examples 1-5 and Comparative Examples 1-5.

[0088] Test method: The test method refers to GB / T 50080-2016 "Standard for Test Methods of Performance of Ordinary Concrete Mixtures". The concrete mix proportion is: cement 211 kg / m³ 3 70kg / m³ of fly ash3 70kg / m³ of mineral powder 3 , sand 836kg / m 3 Stone 1073kg / m 3 159 kg / m³ of water 3 The water-reducing agent was a polycarboxylate-based high-performance water-reducing agent (model ZT1906-CP01, manufactured by Wanwoxin Technology Branch of China Railway 19th Bureau Group Sixth Engineering Co., Ltd.). The final test results are shown in Table 2.

[0089] Table 2. Test Results of Concrete Workability

[0090]

[0091] This set of comparative examples aims to verify the effect of the present invention in improving the flowability of concrete. Comparative Example 1 lacks a molecular bridging agent, causing free triethanolamine molecules to compete with the polyether component for adsorption sites on the cement particle surface, disrupting the integrity of the steric hindrance layer of the polyether component and reducing the dispersion effect. Comparative Example 2, although removing triethanolamine, failed to achieve its optimized steric hindrance effect as a whole because it could not form a complete ternary synergistic complex. Comparative Example 3, due to an incorrect mixing sequence, resulted in a poor supramolecular conformation of the final synergistic complex, with insufficient extension of its steric arms, weakening its dispersion ability for cement particles. Comparative Example 4 lacked insulation treatment, resulting in an unstable molecular assembly structure that easily dissociated in the concrete mixing environment, failing to sustain its steric hindrance effect. In Comparative Example 5, due to defects in the preparation process of the molecular bridging agent, its structure was impure or its activity decreased, affecting its efficiency in forming a stable pre-complex with triethanolamine, thus weakening the structural integrity and dispersion performance of the final complex.

[0092] The interconnectedness of these comparative examples demonstrates the multi-level synergistic logic of this invention in improving flowability. Comparative Examples 1 and 2 first establish that the presence of triethanolamine interferes with flowability, and the solution of this invention is to introduce molecular bridging agents. Comparative Example 5 proves from the perspective of raw material quality that high-quality molecular bridges are needed to ensure the effect. Building on this, Comparative Examples 3 and 4 further demonstrate the path to achieving the synergistic effect from a process perspective. Comparative Example 3 shows that an incorrect mixing sequence leads to structural disorder and performance degradation; Comparative Example 4 shows that the lack of a thermal activation step results in structural instability and similarly affected performance. This series of comparative examples, from component selection and component quality control to process path and steps, comprehensively demonstrates that this invention ultimately achieves flowability performance through an interconnected design.

[0093] Test Example 3

[0094] Test subjects: Concrete wetting agents prepared in Examples 1-5 and Comparative Examples 1-2, 5-6 and 8.

[0095] Test method: The test method refers to GB / T 50080-2016 "Standard for Test Methods of Performance of Ordinary Concrete Mixtures". The concrete mix proportion is: cement 211 kg / m³ 3 70kg / m³ of fly ash 3 70kg / m³ of mineral powder 3 , sand 836kg / m 3 Stone 1073kg / m 3 159 kg / m³ of water 3 The water-reducing agent was a polycarboxylate-based high-performance water-reducing agent (model ZT1906-CP01, manufactured by Wanwoxin Technology Branch of the Sixth Engineering Co., Ltd. of China Railway 19th Bureau Group). The final test results are shown in Table 3 and... Figure 1 As shown.

[0096] Table 3 Gas content test results

[0097]

[0098] This set of comparative examples aims to verify the mechanism by which the present invention regulates the air content of concrete. Comparative Example 1 lacks the complex formed by the molecular bridging agent and triethanolamine, resulting in ineffective reinforcement of the adsorption film at the gas-liquid interface and insufficient mechanical strength and viscoelasticity of the bubble walls. Comparative Example 2 directly lacks triethanolamine, a component that enhances the viscoelasticity of the liquid film, similarly leading to insufficient strength of the composite adsorption film. In Comparative Example 5, the quality defects of the molecular bridging agent affect its efficiency in complexing with triethanolamine, thereby weakening its reinforcing effect on the adsorption film at the gas-liquid interface. The common problem with Comparative Examples 6 and 8 is that, due to improper raw material ratios or catalyst selection, the final polyether components lack the key wetting component generated from excess fatty acid methyl esters. The absence of this component not only weakens the gas-entraining capacity of the polyether component itself but also disrupts its synergistic effect in forming a dense and complete adsorption film at the gas-liquid interface.

[0099] The interconnectedness of these comparative examples reveals the dual synergistic mechanism by which the present invention achieves stable air entrainment. First, Comparative Examples 6 and 8 demonstrate that the material basis for the air entrainment performance is a structurally composite polyether component. They prove that only by preparing a composite polyether with multiple surfactants through specific raw material ratios and catalyst selection can a foundation be provided for air entrainment and the formation of a stable adsorption membrane. Second, based on this material basis, Comparative Examples 1 and 2 demonstrate that the source of stability is an independent reinforcement system. They demonstrate that the polyether component alone is insufficient to resist the complex environment of concrete; a complex formed by a molecular bridging agent and triethanolamine is needed. This complex, through co-assembly with the polyether component at the gas-liquid interface, constructs a composite adsorption membrane with high strength and elasticity. Comparative Example 5 indirectly confirms the dependence of the reinforcement system's construction on raw material quality. Therefore, these comparative examples demonstrate that the stable air entrainment effect of the present invention is the result of the synergistic effect of the high-performance air entrainment basis and the independent foam-stabilizing reinforcement system.

[0100] Although embodiments of the invention have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and alterations can be made to these embodiments without departing from the principles and spirit of the invention, the scope of which is defined by the appended claims and their equivalents.

Claims

1. A method of preparing a concrete wetting agent, characterized by: Specifically, the steps include the following: At room temperature, the additive components and triethanolamine are added to deionized water and stirred to obtain a pre-complex mother liquor; while stirring, the polyether component is added to the pre-complex mother liquor and stirred again, then heat preservation treatment is performed, and after the treatment, the concrete wetting agent is obtained by cooling. The auxiliary component is prepared from polyethylene glycol monomethyl ether and maleic anhydride as raw materials. The preparation method of the auxiliary component is as follows: polyethylene glycol monomethyl ether is added to a reaction vessel, hydroquinone monomethyl ether is added under nitrogen protection and heated; p-toluenesulfonic acid is added to the melt and stirred; then maleic anhydride is added in batches; then the reaction is carried out under nitrogen protection; after the reaction is completed, heating is stopped, and the product is cooled under continuous stirring and nitrogen protection before being discharged to obtain the auxiliary component. The polyether component is prepared from fatty acid methyl ester, alkanolamine, and ethylene oxide as raw materials. The preparation method of the polyether component is as follows: an alkaline catalyst and the alkanolamine are added to a reaction vessel, purged with nitrogen, and then heated to react. After the alkaline catalyst is completely dissolved, the fatty acid methyl ester is added to the reaction vessel, purged with nitrogen again, and then evacuated to a vacuum for constant temperature reaction. After the reaction is completed, heating is stopped, nitrogen is introduced to break the vacuum, and the mixture is cooled and discharged to obtain a mixed intermediate. The intermediate mixture and the magnesium-aluminum composite catalyst were fed into a high-pressure ethoxylation reactor, purged with nitrogen, and then dehydrated under vacuum. After dehydration, the temperature was raised and ethylene oxide was slowly introduced. After the ethylene oxide was introduced, the reaction was continued at a constant temperature for aging. After the reaction was completed, heating was stopped, and the mixture was cooled and discharged from the reactor under nitrogen pressure to obtain the polyether component.

2. A method of preparing a concrete wetting agent according to claim 1, characterised in that: The fatty acid methyl ester is a C12-C14 fatty acid methyl ester or a C16-C18 fatty acid methyl ester.

3. A method of preparing a concrete wetting agent according to claim 1, characterized in that: The alcoholamine is ethanolamine or diethanolamine.

4. A concrete wetting agent prepared by the method of claim 1, characterized by: Specifically, it includes the following components: the concrete wetting agent includes additive components, triethanolamine, polyether components, and deionized water; The auxiliary components include polyethylene glycol monomethyl ether, maleic anhydride, and hydroquinone monomethyl ether. The polyether component includes fatty acid methyl esters, alkanolamines, and ethylene oxide.

5. Use of a concrete wetting agent prepared according to the method of claim 1, characterized in that: The concrete wetting agent is applied to early-strength concrete.

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