Preparation method of concrete pavement curing agent

Abstract

The invention provides a preparation method of a concrete pavement curing agent, and belongs to the technical field of concrete. The preparation method comprises the following steps: preparing a modified beta-cyclodextrin solution, preparing a polyurethane emulsion 1, preparing a polyurethane emulsion 2, and mixing. The mixing method comprises the following steps: adding potash water glass into deionized water, sequentially adding a water-based stabilizer, a polyurethane emulsion 1, a polyurethane emulsion 2 and decyl glucoside in a stirring state, and then transferring the mixture into an ultrasonic oscillator for ultrasonic dispersion for 25-35 minutes to obtain the concrete pavement curing agent. The effective water retention rate of the curing agent is 92-96%, the compressive strength ratio is 95-97% in 7d and 98-99% in 28d, the abrasion loss is 0.7-1.1 kg / m < 2 >, the solid content is 27-30%, and the drying time is 1.1-1.4 h.

Description

Technical Field

[0001] The invention belongs to the technical field of concrete, and particularly relates to a method for preparing a concrete pavement curing agent. Background Art

[0002] The invention belongs to the technical field of concrete, and particularly relates to a method for preparing a concrete pavement curing agent. Summary of the Invention

[0003] In response to the problems existing in the prior art, the present invention provides a method for preparing a concrete pavement curing agent to achieve the following invention objectives: while having the characteristics of a water glass curing agent that can quickly harden the surface and has strong wear resistance, it also has a good water retention effect.

[0004] In order to solve the above technical problems, the technical solutions adopted by the present invention are as follows: A method for preparing a concrete pavement curing agent comprises the following steps: 1. Preparation of modified β-cyclodextrin solution Potassium water glass is added to deionized water, stirred evenly, and H2SO4 solution is added dropwise to adjust the pH value to 2.8-3.2. Then, β-cyclodextrin is added and reacted in a water bath at 55-65°C for 0.8-1.2h to obtain a modified β-cyclodextrin solution; The mass ratio of the potassium silicate, deionized water, and β-cyclodextrin is 0.8-1.2:6-8:2.6-3.4; The mass fraction of the H2SO4 solution is 8-12%.

[0005] 2. Preparation of polyurethane emulsion 1 Polypropylene glycol 1000, isophorone diisocyanate, and catalyst dibutyltin dilaurate were uniformly mixed, heated to 70-90°C at a rate of 1-3°C / min, reacted at constant temperature for 1.9-2.1 hours, cooled to 50-70°C, and then added with modified β-cyclodextrin solution and chain extender 1,4-butanediol. After constant temperature reaction for 2.5-3.5 hours, triethylamine was added for neutralization for 15-25 minutes, and deionized water was added at a rate of 700-900 r / min. After 10-20 minutes, polyurethane emulsion 1 was obtained. The mass ratio of the polypropylene glycol-1000, isophorone diisocyanate, dibutyltin dilaurate, modified beta-cyclodextrin solution, 1,4-butanediol, triethylamine and deionized water is 8-12:2.8-3.2:0.023-0.029:3-5:0.5-0.7:1.2-1.4:20-30.

[0006] 3. Preparation of polyurethane emulsion 2 Polypropylene glycol 1000, isophorone diisocyanate, and catalyst dibutyltin dilaurate were uniformly mixed, heated to 70-90°C at a rate of 1-3°C / min, reacted at constant temperature for 0.7-0.9h, cooled to 50-70°C, and then added with chain extender 2,2-bis(hydroxymethyl)propionic acid. The mixture was reacted at constant temperature for 1.4-1.8h, and triethylamine was added for neutralization for 15-25min. Deionized water was then added at a rate of 700-900r / min, and polyurethane emulsion 2 was obtained after 10-20min. The mass ratio of the polypropylene glycol-1000, isophorone diisocyanate, dibutyltin dilaurate, 2,2-bis(hydroxymethyl)propionic acid, triethylamine and deionized water is 8-12:2.8-3.2:0.023-0.029:0.7-1.3:1.4-1.6:15-25.

[0007] 4. Mix Potassium water glass is added to deionized water, and under stirring, a water-based stabilizer, polyurethane emulsion 1, polyurethane emulsion 2, and decyl glucoside are added in sequence, and then transferred to an ultrasonic oscillator for ultrasonic dispersion for 25 to 35 minutes to obtain a concrete pavement curing agent; The mass ratio of the potassium silicate, deionized water, aqueous stabilizer, polyurethane emulsion 1, polyurethane emulsion 2, and decyl glucoside is 15-25:13-17:0.008-0.012:1.7-1.9:0.3-0.5:0.09-0.11; The aqueous stabilizer is LOPON ST; The stirring rate is 40-60 r / min.

[0008] Compared with the prior art, the present invention has the following beneficial effects: Potassium water glass is a colloid in a metastable structure and is strongly alkaline. When a strong acid is added to it, the silicate radicals can be converted to form Si(OH)4, i.e., silanols, based on the theory that strong acid can produce weak acid. The silanols (Si-OH) in silanols are highly active, and the hydroxyl groups in β-cyclodextrin are also highly active. Silanols undergo dehydration condensation with β-cyclodextrin to produce modified β-cyclodextrin. The modified β-cyclodextrin can react with the hydroxyl groups in the polyurethane emulsion during the preparation process, and then link to the polyurethane chain to produce polyurethane emulsion 1. The curing agent of the present invention mainly comprises potassium water glass, deionized water, a water-based stabilizer, polyurethane emulsion 1, polyurethane emulsion 2, and decyl glucoside. After being sprayed on the concrete surface, as the water evaporates, the potassium water glass comes into contact with the air and absorbs carbon dioxide and water in the air, reacting to generate silicic acid containing active hydroxyl groups. The silicic acids undergo a dehydration condensation reaction to form a three-dimensional network structure. Simultaneously, the hydroxyl groups in the silicic acid also undergo a dehydration condensation reaction with the Si-OH groups in the polyurethane emulsion 1, connecting the network structure formed by the polyurethane emulsion 1 to the three-dimensional network structure formed by the potassium water glass. Compared with polyurethane emulsion 1, polyurethane emulsion 2 reduces the reaction temperature and time during its preparation, resulting in shorter polyurethane chains and more active intermolecular movement. Under the action of the hydrophilic chain extender 2, 2-bis(hydroxymethyl)propionic acid, the chains interpenetrate and cross-link in the network structure while moving downward. The resulting curing agent film surface can harden quickly and has strong wear resistance. At the same time, the network structure is dense and has good water retention effect. The curing agent of the present invention is evaluated according to the JC901-2002 standard, and the measured effective water retention rate is 92-96%, the compressive strength is 95-97% at 7 days and 98-99% at 28 days, the abrasion loss is 0.7-1.1 kg / m2, the solid content is 27-30%, and the drying time is 1.1-1.4 hours. DETAILED DESCRIPTION

[0009] Example 1 1. Preparation of modified β-cyclodextrin solution Potassium water glass was added to deionized water, stirred evenly, and H2SO4 solution was added dropwise to adjust the pH value to 3. β-cyclodextrin was then added and reacted in a water bath at 60°C for 1 hour to obtain a modified β-cyclodextrin solution. The mass ratio of the potassium silicate, deionized water and β-cyclodextrin is 1:7:3; The mass fraction of the H2SO4 solution is 10%.

[0010] 2. Preparation of polyurethane emulsion 1 Polypropylene glycol-1000, isophorone diisocyanate, and catalyst dibutyltin dilaurate were mixed uniformly, heated to 80°C at a rate of 2°C / min, reacted at constant temperature for 2 hours, cooled to 60°C, and then added with modified β-cyclodextrin solution and chain extender 1,4-butanediol. After constant temperature reaction for 3 hours, triethylamine was added for neutralization for 20 minutes, and deionized water was added at a rate of 800 r / min. After 15 minutes, polyurethane emulsion 1 was obtained. The mass ratio of the polypropylene glycol-1000, isophorone diisocyanate, dibutyltin dilaurate, modified beta-cyclodextrin solution, 1,4-butanediol, triethylamine and deionized water is 10:3:0.026:4:0.6:1.3:25.

[0011] 3. Preparation of polyurethane emulsion 2 Polypropylene glycol 1000, isophorone diisocyanate, and catalyst dibutyltin dilaurate were mixed uniformly, heated to 80°C at a rate of 2°C / min, reacted at constant temperature for 0.8h, cooled to 60°C, and then a chain extender, 2,2-bis(hydroxymethyl)propionic acid, was added. After constant temperature reaction for 1.6h, triethylamine was added for neutralization for 20min, and deionized water was added at a rate of 800r / min. After 15min, polyurethane emulsion 2 was obtained. The mass ratio of the polypropylene glycol-1000, isophorone diisocyanate, dibutyltin dilaurate, 2,2-bis(hydroxymethyl)propionic acid, triethylamine and deionized water is 10:3:0.026:1:1.5:20.

[0012] 4. Mix Potassium water glass was added to deionized water, and an aqueous stabilizer, polyurethane emulsion 1, polyurethane emulsion 2, and decyl glucoside were added in sequence under stirring, and then the mixture was transferred to an ultrasonic oscillator for ultrasonic dispersion for 30 minutes to obtain a concrete pavement curing agent; The mass ratio of the potassium silicate, deionized water, aqueous stabilizer, polyurethane emulsion 1, polyurethane emulsion 2, and decyl glucoside is 20:15:0.01:1.8:0.4:0.1; The aqueous stabilizer is LOPON ST; The stirring rate is 50 r / min.

[0013] Example 2 1. Preparation of modified β-cyclodextrin solution Potassium water glass was added to deionized water, stirred evenly, and H2SO4 solution was added dropwise to adjust the pH value to 2.8. β-cyclodextrin was then added and reacted in a water bath at 55°C for 0.8h to obtain a modified β-cyclodextrin solution. The mass ratio of the potassium silicate, deionized water, and β-cyclodextrin is 0.8:6:2.6; The mass fraction of the H2SO4 solution is 8%.

[0014] 2. Preparation of polyurethane emulsion 1 Polypropylene glycol 1000, isophorone diisocyanate, and catalyst dibutyltin dilaurate were mixed uniformly, heated to 70°C at a rate of 1°C / min, reacted at constant temperature for 1.9 hours, cooled to 50°C, and then added with modified β-cyclodextrin solution and chain extender 1,4-butanediol. After constant temperature reaction for 2.5 hours, triethylamine was added for neutralization for 15 minutes, and deionized water was added at a rate of 700 r / min. After 10 minutes, polyurethane emulsion 1 was obtained. The mass ratio of the polypropylene glycol-1000, isophorone diisocyanate, dibutyltin dilaurate, modified beta-cyclodextrin solution, 1,4-butanediol, triethylamine and deionized water is 8:2.8:0.023:3:0.5:1.2:20.

[0015] 3. Preparation of polyurethane emulsion 2 Polypropylene glycol 1000, isophorone diisocyanate, and catalyst dibutyltin dilaurate were mixed uniformly, heated to 70°C at a rate of 1°C / min, and reacted at this temperature for 0.7h. The mixture was then cooled to 50°C, and then a chain extender, 2,2-bis(hydroxymethyl)propionic acid, was added. The mixture was reacted at this temperature for 1.4h. Triethylamine was added for neutralization for 15min, and deionized water was added at a rate of 700r / min. After 10min, polyurethane emulsion 2 was obtained. The mass ratio of the polypropylene glycol-1000, isophorone diisocyanate, dibutyltin dilaurate, 2,2-bis(hydroxymethyl)propionic acid, triethylamine and deionized water is 8:2.8:0.023:0.7:1.4:15.

[0016] 4. Mix Potassium water glass was added to deionized water, and an aqueous stabilizer, polyurethane emulsion 1, polyurethane emulsion 2, and decyl glucoside were added in sequence under stirring, and then the mixture was transferred to an ultrasonic oscillator for ultrasonic dispersion for 25 minutes to obtain a concrete pavement curing agent; The mass ratio of the potassium silicate, deionized water, aqueous stabilizer, polyurethane emulsion 1, polyurethane emulsion 2, and decyl glucoside is 15:13:0.008:1.7:0.3:0.09; The aqueous stabilizer is LOPON ST; The stirring rate is 40 r / min.

[0017] Example 3 1. Preparation of modified β-cyclodextrin solution Potassium water glass was added to deionized water, stirred evenly, and H2SO4 solution was added dropwise to adjust the pH value to 3.2. Then, β-cyclodextrin was added and reacted in a water bath at 65°C for 1.2 h to obtain a modified β-cyclodextrin solution. The mass ratio of the potassium silicate, deionized water, and β-cyclodextrin is 1.2:8:3.4; The mass fraction of the H2SO4 solution is 12%.

[0018] 2. Preparation of polyurethane emulsion 1 Polypropylene glycol 1000, isophorone diisocyanate, and catalyst dibutyltin dilaurate were mixed uniformly, heated to 90°C at a rate of 3°C / min, reacted at constant temperature for 2.1 hours, cooled to 70°C, and then added with modified β-cyclodextrin solution and chain extender 1,4-butanediol. After constant temperature reaction for 3.5 hours, triethylamine was added for neutralization for 25 minutes, and deionized water was added at a rate of 900 r / min. After 20 minutes, polyurethane emulsion 1 was obtained. The mass ratio of the polypropylene glycol-1000, isophorone diisocyanate, dibutyltin dilaurate, modified beta-cyclodextrin solution, 1,4-butanediol, triethylamine and deionized water is 12:3.2:0.029:5:0.7:1.4:30.

[0019] 3. Preparation of polyurethane emulsion 2 Polypropylene glycol 1000, isophorone diisocyanate, and catalyst dibutyltin dilaurate were mixed uniformly, heated to 90°C at a rate of 3°C / min, and reacted at a constant temperature for 0.9h. The mixture was then cooled to 70°C, and then a chain extender, 2,2-bis(hydroxymethyl)propionic acid, was added and reacted at a constant temperature for 1.8h. Triethylamine was added for neutralization for 25min, and deionized water was added at a rate of 900r / min. After 20min, polyurethane emulsion 2 was obtained. The mass ratio of the polypropylene glycol-1000, isophorone diisocyanate, dibutyltin dilaurate, 2,2-bis(hydroxymethyl)propionic acid, triethylamine and deionized water is 12:3.2:0.029:1.3:1.6:25.

[0020] 4. Mix Potassium water glass was added to deionized water, and an aqueous stabilizer, polyurethane emulsion 1, polyurethane emulsion 2, and decyl glucoside were added in sequence under stirring, and then the mixture was transferred to an ultrasonic oscillator for ultrasonic dispersion for 35 minutes to obtain a concrete pavement curing agent; The mass ratio of the potassium silicate, deionized water, aqueous stabilizer, polyurethane emulsion 1, polyurethane emulsion 2, and decyl glucoside is 25:17:0.012:1.9:0.5:0.11; The aqueous stabilizer is LOPON ST; The stirring rate is 60 r / min.

[0021] Example 4 1. Preparation of polyurethane emulsion 1 Polypropylene glycol-1000, isophorone diisocyanate, and catalyst dibutyltin dilaurate were mixed uniformly, heated to 80°C at a rate of 2°C / min, reacted at constant temperature for 2 hours, cooled to 60°C, and then β-cyclodextrin and chain extender 1,4-butanediol were added. After constant temperature reaction for 3 hours, triethylamine was added for neutralization for 20 minutes, and deionized water was added at a rate of 800 r / min. After 15 minutes, polyurethane emulsion 1 was obtained. The mass ratio of the polypropylene glycol-1000, isophorone diisocyanate, dibutyltin dilaurate, beta-cyclodextrin, 1,4-butanediol, triethylamine and deionized water is 10:3:0.026:1:0.6:1.3:25.

[0022] 2. Preparation of polyurethane emulsion 2 Polypropylene glycol 1000, isophorone diisocyanate, and catalyst dibutyltin dilaurate were mixed uniformly, heated to 80°C at a rate of 2°C / min, reacted at constant temperature for 0.8h, cooled to 60°C, and then a chain extender, 2,2-bis(hydroxymethyl)propionic acid, was added. After constant temperature reaction for 1.6h, triethylamine was added for neutralization for 20min, and deionized water was added at a rate of 800r / min. After 15min, polyurethane emulsion 2 was obtained. The mass ratio of the polypropylene glycol-1000, isophorone diisocyanate, dibutyltin dilaurate, 2,2-bis(hydroxymethyl)propionic acid, triethylamine and deionized water is 10:3:0.026:1:1.5:20.

[0023] 3. Mix Potassium water glass was added to deionized water, and an aqueous stabilizer, polyurethane emulsion 1, polyurethane emulsion 2, and decyl glucoside were added in sequence under stirring, and then the mixture was transferred to an ultrasonic oscillator for ultrasonic dispersion for 30 minutes to obtain a concrete pavement curing agent; The mass ratio of the potassium silicate, deionized water, aqueous stabilizer, polyurethane emulsion 1, polyurethane emulsion 2, and decyl glucoside is 20:15:0.01:1.8:0.4:0.1; The aqueous stabilizer is LOPON ST; The stirring rate is 50 r / min.

[0024] Example 5 1. Preparation of modified β-cyclodextrin solution Potassium water glass was added to deionized water, stirred evenly, and H2SO4 solution was added dropwise to adjust the pH value to 3. β-cyclodextrin was then added and reacted in a water bath at 60°C for 1 hour to obtain a modified β-cyclodextrin solution. The mass ratio of the potassium silicate, deionized water and β-cyclodextrin is 1:7:3; The mass fraction of the H2SO4 solution is 10%.

[0025] 2. Preparation of polyurethane emulsion Polypropylene glycol-1000, isophorone diisocyanate, and catalyst dibutyltin dilaurate were mixed uniformly, heated to 80°C at a rate of 2°C / min, reacted at constant temperature for 2 hours, cooled to 60°C, and then added with modified β-cyclodextrin solution and chain extender 1,4-butanediol. After constant temperature reaction for 3 hours, triethylamine was added for neutralization for 20 minutes, and deionized water was added at a rate of 800 r / min. After 15 minutes, a polyurethane emulsion was obtained. The mass ratio of the polypropylene glycol-1000, isophorone diisocyanate, dibutyltin dilaurate, modified beta-cyclodextrin solution, 1,4-butanediol, triethylamine and deionized water is 10:3:0.026:4:0.6:1.3:25.

[0026] 3. Mixing Potassium water glass was added to deionized water, and a water-based stabilizer, a polyurethane emulsion, and decyl glucoside were added in sequence under stirring, and then the mixture was transferred to an ultrasonic oscillator for ultrasonic dispersion for 30 minutes to obtain a concrete pavement curing agent; The mass ratio of the potassium silicate, deionized water, aqueous stabilizer, polyurethane emulsion 1, and decyl glucoside is 20:15:0.01:1.8:0.1; The aqueous stabilizer is LOPON ST; The stirring rate is 50 r / min.

[0027] Example 6 1. Mix Potassium water glass was added to deionized water, and a water-based stabilizer and decyl glucoside were added in sequence under stirring, and then the mixture was transferred to an ultrasonic oscillator for ultrasonic dispersion for 30 minutes to obtain a concrete pavement curing agent; The mass ratio of the potassium silicate, deionized water, aqueous stabilizer, and decyl glucoside is 20:15:0.01:0.1; The aqueous stabilizer is LOPON ST; The stirring rate is 50 r / min.

[0028] Test example The concrete pavement curing agents prepared in Examples 1 to 6 were evaluated according to the JC901-2002 standard. The evaluation results are shown in Table 1.

[0029] Table 1

[0030] It can be seen from Examples 1 to 6 that: Compared to Example 1, since Example 4 did not modify β-cyclodextrin, when preparing polyurethane emulsion 1, the active hydroxyl groups on β-cyclodextrin participated in the chain extender reaction, and the hydroxyl groups at the remaining positions were less active and had poor connection with the silanol groups. Therefore, during the curing process, the network structure formed by polyurethane emulsion 1 had poor connection with the network structure formed by potassium water glass, resulting in a low effective water retention rate and high abrasion of the cured film. Compared with Example 1, the curing agent prepared in Example 5 does not contain polyurethane emulsion 2, resulting in weak downward penetration of the curing agent, and thus weak bonding with the concrete pavement, poor wear resistance, high wear loss, and low effective water retention rate; Compared with Example 1, the curing agent prepared in Example 6 does not contain polyurethane emulsion 1 and polyurethane emulsion 2, so the solid content is relatively high, and the pores of the formed network structure are larger. Although the drying time is short, the effective water retention rate is low and the abrasion loss is high.

Claims

1. A method for preparing a concrete pavement curing agent, characterized in that: The preparation method comprises preparing a modified β-cyclodextrin solution, preparing polyurethane emulsion 1, preparing polyurethane emulsion 2, and mixing; The method for preparing the modified β-cyclodextrin solution comprises adding potassium water glass to deionized water, stirring uniformly, adding H2SO4 solution dropwise to adjust the pH value to 2.8-3.2, then adding β-cyclodextrin, and reacting at 55-65°C in a water bath for 0.8-1.2 hours to obtain the modified β-cyclodextrin solution; The method for preparing the polyurethane emulsion 1 comprises: uniformly mixing polypropylene glycol-1000, isophorone diisocyanate, and a catalyst, dibutyltin dilaurate; heating the mixture to 70-90° C. at a rate of 1-3° C. / min; reacting the mixture at a constant temperature for 1.9-2.1 hours; cooling the mixture to 50-70° C.; adding a modified β-cyclodextrin solution and a chain extender, 1,4-butanediol; reacting the mixture at a constant temperature for 2.5-3.5 hours; neutralizing the mixture with triethylamine for 15-25 minutes; and adding deionized water at a rate of 700-900 r / min for 10-20 minutes to obtain the polyurethane emulsion 1.

2. The method for preparing a concrete pavement curing agent according to claim 1, characterized in that: In the method for preparing the modified β-cyclodextrin solution, the mass ratio of potassium water glass, deionized water, and β-cyclodextrin is 0.8-1.2:6-8:2.6-3.4, and the mass fraction of the H2SO4 solution is 8-12%.

3. The method for preparing a concrete pavement curing agent according to claim 1, characterized in that: In the method for preparing polyurethane emulsion 1, the mass ratio of polypropylene glycol-1000, isophorone diisocyanate, dibutyltin dilaurate, modified β-cyclodextrin solution, 1,4-butanediol, triethylamine, and deionized water is 8-12:2.8-3.2:0.023-0.029:3-5:0.5-0.7:1.2-1.4:20-30.

4. The method for preparing a concrete pavement curing agent according to claim 1, characterized in that: The method for preparing polyurethane emulsion 2 comprises: uniformly mixing polypropylene glycol-1000, isophorone diisocyanate, and a catalyst, dibutyltin dilaurate; heating the mixture to 70-90° C.; reacting the mixture at a constant temperature for 0.7-0.9 h; cooling the mixture to 50-70° C.; adding a chain extender, 2,2-bis(hydroxymethyl)propionic acid; reacting the mixture at a constant temperature for 1.4-1.8 h; adding triethylamine for neutralization for 15-25 min; and adding deionized water at a rate of 700-900 r / min for 10-20 min to obtain polyurethane emulsion 2.

5. The method for preparing a concrete pavement curing agent according to claim 4, characterized in that: In the method for preparing polyurethane emulsion 2, the mass ratio of polypropylene glycol-1000, isophorone diisocyanate, dibutyltin dilaurate, 2,2-bis(hydroxymethyl)propionic acid, triethylamine, and deionized water is 8-12:2.8-3.2:0.023-0.029:0.7-1.3:1.4-1.6:15-25, and the heating rate is 1-3°C / min.

6. The method for preparing a concrete pavement curing agent according to claim 1, characterized in that: The mixing method comprises the following steps: adding potassium water glass to deionized water, sequentially adding a water-based stabilizer, polyurethane emulsion 1, polyurethane emulsion 2, and decyl glucoside under stirring, and then transferring the mixture to an ultrasonic oscillator for ultrasonic dispersion for 25 to 35 minutes to obtain a concrete pavement curing agent.

7. The method for preparing a concrete pavement curing agent according to claim 6, characterized in that: In the mixing method, the mass ratio of potassium water glass, deionized water, aqueous stabilizer, polyurethane emulsion 1, polyurethane emulsion 2, and decyl glucoside is 15-25:13-17:0.008-0.012:1.7-1.9:0.3-0.5:0.09-0.11, the aqueous stabilizer is LOPON ST, and the stirring rate is 40-60 r / min.

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