CN108658503B - Preparation method of concrete air entraining agent - Google Patents
Preparation method of concrete air entraining agent Download PDFInfo
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- CN108658503B CN108658503B CN201810515600.XA CN201810515600A CN108658503B CN 108658503 B CN108658503 B CN 108658503B CN 201810515600 A CN201810515600 A CN 201810515600A CN 108658503 B CN108658503 B CN 108658503B
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B40/00—Processes, in general, for influencing or modifying the properties of mortars, concrete or artificial stone compositions, e.g. their setting or hardening ability
- C04B40/0028—Aspects relating to the mixing step of the mortar preparation
- C04B40/0039—Premixtures of ingredients
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2103/00—Function or property of ingredients for mortars, concrete or artificial stone
- C04B2103/30—Water reducers, plasticisers, air-entrainers, flow improvers
- C04B2103/304—Air-entrainers
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Abstract
The invention discloses a preparation method of a concrete air entraining agent, and belongs to the technical field of high polymer materials. Mixing an additive and the modified microspheres in a mass ratio of 1: 3-1: and 5, mixing the mixture in a reaction kettle, adding water with the mass 5-8 times of that of the additive into the reaction kettle, stirring and mixing the mixture for 30-45 min at the temperature of 40-50 ℃ to obtain a mixed blank, introducing carbon dioxide into the mixed blank at the speed of 10-20 mL/min at the temperature of 40-45 ℃, standing the mixture for 1-2 h at the temperature of 40-45 ℃, and performing rotary evaporation and concentration for 2-5 h at the temperature of 40-45 ℃, the rotation speed of 120-200 r/min and the pressure of 450-550 kPa to obtain the concrete air entraining agent. The concrete air entraining agent prepared by the technical scheme of the invention has the characteristics of excellent air entraining effect and small number of through holes, and has wide prospect in the development of the polymer material technology industry.
Description
Technical Field
The invention discloses a preparation method of a concrete air entraining agent, and belongs to the technical field of high polymer materials.
Background
The air entraining agent can introduce a proper amount of tiny independently distributed air bubbles in the process of mixing the concrete. The micro bubbles are similar to balls, have wetting and dispersing functions, can improve the workability of concrete, effectively reduce the bleeding of fresh concrete and avoid segregation; in the hardened concrete, the introduced air bubbles enable capillaries in the hardened concrete to become fine, tortuous and dispersed, and the permeation channels are reduced, thereby being beneficial to improving the frost resistance, the compactness and the impermeability of the concrete. A large number of laboratory and field engineering practices show that the concrete air entraining agent has a profound influence on improving the workability and durability of concrete. Most of concrete must be blended with an air entraining agent or an air entraining and water reducing agent, which is mainly used for improving the frost resistance of hydraulic concrete, and the air entraining agent or the air entraining and water reducing agent is gradually used in the concrete in the fields of high-speed rails, ports, airports, nuclear power, high-rise civil buildings and the like at present. Most of the air entraining agent is anionic surfactant, and on the water-air interface, the hydrophobic group is adsorbed to the air surface in a directional way, on the cement-water interface, the cement or hydrated particles thereof are adsorbed with the hydrophilic group, the hydrophobic group deviates from the cement and hydrated particles thereof to form a hydrophobic adsorption layer and tries to approach the air surface, because of the approach of the particles to the air surface and the adsorption of the air entraining agent molecules on the air-water interface, the surface tension of water is obviously reduced, so that the concrete generates a large number of micro bubbles in the mixing process, the micro bubbles have a directional adsorption layer with the same charge, so as to repel each other and distribute uniformly; on the other hand, many anion air entraining agents have calcium salt precipitation in cement aqueous solution with high calcium content, and are adsorbed on bubble films, so that bubbles can be effectively prevented from being broken, and the introduced fine and uniform bubbles can stably exist within a certain time. The air entraining agent primarily serves firstly to introduce air bubbles and secondly to disperse and wet the air. Air entraining agents were used as an admixture for improving the impermeability, frost resistance and salt-frost-erosion resistance of concrete for the first time. The main principle is that small bubbles introduced by the air entraining agent cut off the path of the capillary tube, and the capillary action is reduced, so that the impermeability of the concrete is improved. The micro pores can release the expansion pressure of ice crystals in the capillary during freezing, thereby avoiding generating destructive pressure, reducing and preventing the destructive effect of freeze thawing, and improving the frost resistance of concrete.
Therefore, how to improve the defects of poor air entraining effect and large number of through holes of the traditional concrete air entraining agent to obtain higher comprehensive performance improvement is a problem to be researched and solved.
Disclosure of Invention
The invention mainly solves the technical problems that: aiming at the defects of poor air entraining effect and large number of through holes of the traditional concrete air entraining agent, the preparation method of the concrete air entraining agent is provided.
In order to solve the technical problems, the technical scheme adopted by the invention is as follows:
a preparation method of a concrete air entraining agent comprises the following specific preparation steps:
(1) mixing (N-amidino) dodecyl acrylamide and polyethylene glycol derivatives in a mass ratio of 4: 1-5: 1, mixing, adding p-dichlorobenzene accounting for 0.1-0.2 times of the mass of the polyethylene glycol derivative, ferrocene accounting for 0.08-0.12 times of the mass of the polyethylene glycol derivative and tetrahydrofuran accounting for 10-15 times of the mass of the polyethylene glycol derivative, stirring and mixing, and performing rotary evaporation and concentration to obtain an additive;
(2) mixing styrene and sodium hydroxide solution according to the volume ratio of 1: 1-1: 2, mixing, standing for layering, removing lower layer liquid to obtain upper layer liquid, washing the upper layer liquid with deionized water until the washing liquid is neutral to obtain pretreated styrene, and mixing the pretreated styrene and glycidyl methacrylate according to a mass ratio of 1.0: 1.5-1.0: 1.8, obtaining a styrene mixture, and mixing an initiator and a surfactant according to a mass ratio of 1: 18-1: 20, adding water 90-120 times the mass of potassium persulfate, stirring and mixing to obtain a mixed solution, dripping a styrene mixture 0.3-0.5 times the mass of the mixed solution into the mixed solution, stirring and mixing to obtain a blank material solution, and mixing the blank material solution and an ethanol solution according to the mass ratio of 1: 3-1: 5, mixing, performing centrifugal separation to obtain a pretreatment blank, and mixing the pretreatment blank with an ethanol solution according to a mass ratio of 1: 5-1: 6, mixing, ultrasonically dispersing and filtering to obtain pretreated microspheres;
(3) grinding and sieving the pretreated microspheres to obtain microsphere powder, and mixing the microsphere powder with water according to a mass ratio of 1: 10-1: 15, mixing, performing ultrasonic oscillation to obtain a microsphere mixture, and mixing the microsphere mixture and water according to a mass ratio of 1: 1-2: 1, mixing, adding ethylenediamine with the mass of 0.1-0.2 times of that of the microsphere mixture, stirring for reaction, filtering, washing, and drying in vacuum to obtain modified microspheres;
(4) mixing an additive and the modified microspheres in a mass ratio of 1: 3-1: and 5, mixing, adding water with the mass 5-8 times that of the additive, stirring and mixing to obtain a mixed blank, introducing carbon dioxide into the mixed blank at the speed of 10-20 mL/min at the temperature of 40-45 ℃, standing, and performing rotary evaporation and concentration to obtain the concrete air entraining agent.
The polyethylene glycol derivative in the step (1) is any one of polyethylene glycol-p-toluenesulfonate or polyethylene glycol salicylate.
The initiator in the step (2) is any one of potassium persulfate, sodium persulfate or ammonium persulfate.
The surfactant in the step (2) is any one of tween-80, span-80 or sodium dodecyl benzene sulfonate.
The invention has the beneficial effects that:
(1) the modified microspheres are added during the preparation of the concrete air entraining agent, firstly, the microspheres are hollow structures and can be used as air holes to exist in the concrete after being added into a product, so that the porosity of the concrete is increased, and further, the air entraining effect of the product is improved;
(2) the additive is added when the concrete air entraining agent is prepared, on one hand, the additive contains a substance with a vesicle structure, and the substance can be used as micropores in a product after being added into the product, so that the air entraining effect of the product is improved, and on the other hand, the substance with the vesicle structure in the additive has the carbon dioxide adsorption capacity, and can adsorb carbon dioxide released by the modified microspheres after being added into the product, so that the vesicle structure is enlarged, and the number of through holes in concrete is reduced while the air entraining effect of the product is improved.
Detailed Description
Mixing (N-amidino) dodecyl acrylamide and polyethylene glycol derivatives in a mass ratio of 4: 1-5: 1, mixing the mixture in a beaker, adding p-dichlorobenzene with the mass of the polyethylene glycol derivative being 0.1-0.2 time, ferrocene with the mass of the polyethylene glycol derivative being 0.08-0.12 time and tetrahydrofuran with the mass of the polyethylene glycol derivative being 10-15 times into the beaker, stirring and mixing for 1-2 hours at the temperature of 45-55 ℃ and the rotation speed of 250-350 r/min to obtain an additive blank, and carrying out rotary evaporation and concentration on the additive blank for 30-40 minutes at the temperature of 60-70 ℃, the rotation speed of 120-150 r/min and the pressure of 500-600 kPa to obtain the additive; mixing styrene and a sodium hydroxide solution with the mass fraction of 5-8% according to the volume ratio of 1: 1-1: 2, mixing, stirring and mixing for 20-30 min under the conditions that the temperature is 28-35 ℃ and the rotating speed is 280-350 r/min, standing for 40-60 min at room temperature, removing lower layer liquid to obtain upper layer liquid, washing the upper layer liquid with deionized water until the washing liquid is neutral to obtain pretreated styrene, and mixing the pretreated styrene and glycidyl methacrylate according to the mass ratio of 1.0: 1.5-1.0: 1.8, stirring and mixing for 20-40 min under the conditions that the temperature is 30-35 ℃ and the rotating speed is 250-350 r/min to obtain a styrene mixture, and mixing an initiator and a surfactant according to a mass ratio of 1: 18-1: 20, adding water 90-120 times the mass of potassium persulfate into a flask, stirring and mixing at the temperature of 45-55 ℃ and the rotation speed of 700-1000 r/min to obtain a mixed solution, dripping a styrene mixture 0.3-0.5 times the mass of the mixed solution into the mixed solution at the speed of 5-12 mL/min, stirring and mixing at the temperature of 50-60 ℃ and the rotation speed of 600-800 r/min for 10-11 h, cooling to room temperature, discharging to obtain a blank material solution, mixing the blank material solution with an ethanol solution with the mass fraction of 45-65% according to the mass ratio of 1: 3-1: 5, mixing, performing centrifugal separation for 10-15 min under the condition that the rotating speed is 1200-2000 r/min to obtain a pretreated blank, and mixing the pretreated blank with an ethanol solution with the mass fraction of 45-65% according to the mass ratio of 1: 5-1: 6, mixing, carrying out ultrasonic dispersion for 10-15 min under the condition that the frequency is 45-55 kHz, and filtering to obtain pretreated microspheres; grinding the pretreated microspheres and sieving the ground microspheres with a 100-mesh sieve to obtain microsphere powder, and mixing the microsphere powder and water according to a mass ratio of 1: 10-1: 15, performing ultrasonic oscillation for 10-15 min under the condition that the frequency is 40-60 kHz to obtain a microsphere mixture, and mixing the microsphere mixture and water according to the mass ratio of 1: 1-2: 1, mixing an erlenmeyer flask, adding ethylenediamine with the mass of 0.1-0.2 times of that of a microsphere mixture into the erlenmeyer flask, stirring and reacting for 10-12 hours at the temperature of 90-95 ℃ and the rotating speed of 200-350 r/min, filtering to obtain a filter cake, washing the filter cake for 3-5 times with water, and performing vacuum drying for 1-3 hours at the temperature of 40-55 ℃ to obtain modified microspheres; mixing an additive and the modified microspheres in a mass ratio of 1: 3-1: 5, mixing the mixture in a reaction kettle, adding water with the mass 5-8 times of that of the additive into the reaction kettle, stirring and mixing the mixture for 30-45 min at the temperature of 40-50 ℃ to obtain a mixed blank, introducing carbon dioxide into the mixed blank at the speed of 10-20 mL/min at the temperature of 40-45 ℃, continuously introducing the carbon dioxide for 2-3 min, standing the mixture for 30-40 min at the temperature of 40-45 ℃, introducing nitrogen into the mixed blank at the speed of 5-8 mL/min, continuously introducing the nitrogen for 5-8 min, and then carrying out rotary evaporation and concentration on the mixed blank for 2-5 h at the temperature of 40-45 ℃, the rotation speed of 120-200 r/min and the pressure of 450-550 kPa to obtain the concrete air entraining agent. The polyethylene glycol derivative is any one of polyethylene glycol-p-toluenesulfonate or polyethylene glycol salicylate. The initiator is any one of potassium persulfate, sodium persulfate or ammonium persulfate. The surfactant is any one of tween-80, span-80 or sodium dodecyl benzene sulfonate.
Example 1
Mixing (N-amidino) dodecyl acrylamide and polyethylene glycol derivatives in a mass ratio of 5: 1, mixing the mixture in a beaker, adding p-dichlorobenzene with the mass of the polyethylene glycol derivative being 0.2 time, ferrocene with the mass of the polyethylene glycol derivative being 0.12 time and tetrahydrofuran with the mass of the polyethylene glycol derivative being 15 times into the beaker, stirring and mixing for 2 hours at the temperature of 55 ℃ and the rotating speed of 350r/min to obtain an additive blank, and carrying out rotary evaporation and concentration on the additive blank for 40 minutes at the temperature of 70 ℃, the rotating speed of 150r/min and the pressure of 600kPa to obtain the additive; mixing styrene and 8% by mass of sodium hydroxide solution according to the volume ratio of 1: 2, mixing, stirring and mixing for 30min under the conditions that the temperature is 35 ℃ and the rotating speed is 350r/min, standing for 60min under the condition of room temperature, removing lower layer liquid to obtain upper layer liquid, washing the upper layer liquid with deionized water until the washing liquid is neutral to obtain pretreated styrene, and mixing the pretreated styrene and glycidyl methacrylate according to the mass ratio of 1.0: 1.8, stirring and mixing for 40min under the conditions that the temperature is 35 ℃ and the rotating speed is 350r/min to obtain a styrene mixture, and mixing an initiator and a surfactant according to the mass ratio of 1: 20, mixing the mixture in a flask, adding water 120 times the mass of potassium persulfate into the flask, stirring and mixing the mixture at the temperature of 455 ℃ and the rotation speed of 1000r/min to obtain a mixed solution, dripping a styrene mixture 0.5 times the mass of the mixed solution into the mixed solution at the speed of 12mL/min, stirring and mixing the mixed solution at the temperature of 60 ℃ and the rotation speed of 800r/min for 11 hours, cooling the mixed solution to room temperature, discharging the mixed solution to obtain a blank material liquid, mixing the blank material liquid with an ethanol solution with the mass fraction of 65% according to the mass ratio of 1: 5, mixing, carrying out centrifugal separation for 15min under the condition that the rotating speed is 2000r/min to obtain a pretreatment blank, and mixing the pretreatment blank with 65% ethanol solution according to the mass ratio of 1: 6, mixing, carrying out ultrasonic dispersion for 15min under the condition of 55kHz frequency, and filtering to obtain pretreated microspheres; grinding the pretreated microspheres and sieving the ground microspheres with a 100-mesh sieve to obtain microsphere powder, and mixing the microsphere powder and water according to a mass ratio of 1: 15, mixing, carrying out ultrasonic oscillation for 15min under the condition that the frequency is 60kHz to obtain a microsphere mixture, and mixing the microsphere mixture and water according to the mass ratio of 2: 1, mixing a conical flask, adding ethylenediamine with the mass of 0.2 time of that of a microsphere mixture into the conical flask, stirring and reacting for 12 hours at the temperature of 95 ℃ and the rotation speed of 350r/min, filtering to obtain a filter cake, washing the filter cake for 5 times with water, and drying in vacuum for 3 hours at the temperature of 55 ℃ to obtain modified microspheres; mixing an additive and the modified microspheres in a mass ratio of 1: 5, mixing the mixture in a reaction kettle, adding water with the mass 8 times of that of the additive into the reaction kettle, stirring and mixing the mixture for 45min at the temperature of 50 ℃ to obtain a mixed blank, introducing carbon dioxide into the mixed blank at the rate of 20mL/min at the temperature of 45 ℃, continuously introducing the carbon dioxide for 3min, standing the mixture for 40min at the temperature of 45 ℃, introducing nitrogen into the mixed blank at the rate of 8mL/min, continuously introducing the nitrogen for 8min, and carrying out rotary evaporation and concentration on the mixed blank for 5h at the temperature of 45 ℃, the rotating speed of 200r/min and the pressure of 550kPa to obtain the concrete air entraining agent. The polyethylene glycol derivative is polyethylene glycol-p-toluenesulfonate. The initiator is potassium persulfate. The surfactant is tween-80.
Example 2
Mixing styrene and 8% by mass of sodium hydroxide solution according to the volume ratio of 1: 2, mixing, stirring and mixing for 30min under the conditions that the temperature is 35 ℃ and the rotating speed is 350r/min, standing for 60min under the condition of room temperature, removing lower layer liquid to obtain upper layer liquid, washing the upper layer liquid with deionized water until the washing liquid is neutral to obtain pretreated styrene, and mixing the pretreated styrene and glycidyl methacrylate according to the mass ratio of 1.0: 1.8, stirring and mixing for 40min under the conditions that the temperature is 35 ℃ and the rotating speed is 350r/min to obtain a styrene mixture, and mixing an initiator and a surfactant according to the mass ratio of 1: 20, mixing the mixture in a flask, adding water 120 times the mass of potassium persulfate into the flask, stirring and mixing the mixture at the temperature of 455 ℃ and the rotation speed of 1000r/min to obtain a mixed solution, dripping a styrene mixture 0.5 times the mass of the mixed solution into the mixed solution at the speed of 12mL/min, stirring and mixing the mixed solution at the temperature of 60 ℃ and the rotation speed of 800r/min for 11 hours, cooling the mixed solution to room temperature, discharging the mixed solution to obtain a blank material liquid, mixing the blank material liquid with an ethanol solution with the mass fraction of 65% according to the mass ratio of 1: 5, mixing, carrying out centrifugal separation for 15min under the condition that the rotating speed is 2000r/min to obtain a pretreatment blank, and mixing the pretreatment blank with 65% ethanol solution according to the mass ratio of 1: 6, mixing, carrying out ultrasonic dispersion for 15min under the condition of 55kHz frequency, and filtering to obtain pretreated microspheres; grinding the pretreated microspheres and sieving the ground microspheres with a 100-mesh sieve to obtain microsphere powder, and mixing the microsphere powder and water according to a mass ratio of 1: 15, mixing, carrying out ultrasonic oscillation for 15min under the condition that the frequency is 60kHz to obtain a microsphere mixture, and mixing the microsphere mixture and water according to the mass ratio of 2: 1, mixing a conical flask, adding ethylenediamine with the mass of 0.2 time of that of a microsphere mixture into the conical flask, stirring and reacting for 12 hours at the temperature of 95 ℃ and the rotation speed of 350r/min, filtering to obtain a filter cake, washing the filter cake for 5 times with water, and drying in vacuum for 3 hours at the temperature of 55 ℃ to obtain modified microspheres; mixing the modified microspheres with water according to a mass ratio of 1: 1.6, mixing the mixture in a reaction kettle, stirring and mixing the mixture for 45min at the temperature of 50 ℃ to obtain a mixed blank, introducing carbon dioxide into the mixed blank at the rate of 20mL/min at the temperature of 45 ℃, continuously introducing the carbon dioxide for 3min, standing the mixture for 40min at the temperature of 45 ℃, then introducing nitrogen into the mixed blank at the rate of 8mL/min, continuously introducing the nitrogen for 8min, and carrying out rotary evaporation and concentration on the mixed blank for 5h at the temperature of 45 ℃, the rotating speed of 200r/min and the pressure of 550kPa to obtain the concrete air entraining agent. The initiator is potassium persulfate. The surfactant is tween-80.
Example 3
Mixing (N-amidino) dodecyl acrylamide and polyethylene glycol derivatives in a mass ratio of 5: 1, mixing the mixture in a beaker, adding p-dichlorobenzene with the mass of the polyethylene glycol derivative being 0.2 time, ferrocene with the mass of the polyethylene glycol derivative being 0.12 time and tetrahydrofuran with the mass of the polyethylene glycol derivative being 15 times into the beaker, stirring and mixing for 2 hours at the temperature of 55 ℃ and the rotating speed of 350r/min to obtain an additive blank, and carrying out rotary evaporation and concentration on the additive blank for 40 minutes at the temperature of 70 ℃, the rotating speed of 150r/min and the pressure of 600kPa to obtain the additive; mixing styrene and 8% by mass of sodium hydroxide solution according to the volume ratio of 1: 2, mixing, stirring and mixing for 30min under the conditions that the temperature is 35 ℃ and the rotating speed is 350r/min, standing for 60min under the condition of room temperature, removing lower layer liquid to obtain upper layer liquid, washing the upper layer liquid with deionized water until the washing liquid is neutral to obtain pretreated styrene, and mixing the pretreated styrene and glycidyl methacrylate according to the mass ratio of 1.0: 1.8, stirring and mixing for 40min under the conditions that the temperature is 35 ℃ and the rotating speed is 350r/min to obtain a styrene mixture, and mixing an initiator and a surfactant according to the mass ratio of 1: 20, mixing the mixture in a flask, adding water 120 times the mass of potassium persulfate into the flask, stirring and mixing the mixture at the temperature of 455 ℃ and the rotation speed of 1000r/min to obtain a mixed solution, dripping a styrene mixture 0.5 times the mass of the mixed solution into the mixed solution at the speed of 12mL/min, stirring and mixing the mixed solution at the temperature of 60 ℃ and the rotation speed of 800r/min for 11 hours, cooling the mixed solution to room temperature, discharging the mixed solution to obtain a blank material liquid, mixing the blank material liquid with an ethanol solution with the mass fraction of 65% according to the mass ratio of 1: 5, mixing, carrying out centrifugal separation for 15min under the condition that the rotating speed is 2000r/min to obtain a pretreatment blank, and mixing the pretreatment blank with 65% ethanol solution according to the mass ratio of 1: 6, mixing, carrying out ultrasonic dispersion for 15min under the condition of 55kHz frequency, and filtering to obtain pretreated microspheres; grinding the pretreated microspheres and sieving the ground microspheres with a 100-mesh sieve to obtain microsphere powder; mixing an additive and microsphere powder according to a mass ratio of 1: 5, mixing the mixture in a reaction kettle, adding water with the mass 8 times of that of the additive into the reaction kettle, stirring and mixing the mixture for 45min at the temperature of 50 ℃ to obtain a mixed blank, introducing carbon dioxide into the mixed blank at the rate of 20mL/min at the temperature of 45 ℃, continuously introducing the carbon dioxide for 3min, standing the mixture for 40min at the temperature of 45 ℃, introducing nitrogen into the mixed blank at the rate of 8mL/min, continuously introducing the nitrogen for 8min, and carrying out rotary evaporation and concentration on the mixed blank for 5h at the temperature of 45 ℃, the rotating speed of 200r/min and the pressure of 550kPa to obtain the concrete air entraining agent. The polyethylene glycol derivative is polyethylene glycol-p-toluenesulfonate. The initiator is potassium persulfate. The surfactant is tween-80.
Comparative example: a concrete air entraining agent produced by Guangdong chemical industry Co.
The concrete air entraining agents obtained in the examples 1 to 3 and the comparative products are subjected to performance detection, and the specific detection method is as follows:
concrete strength and gas content are measured according to relevant regulations of national standard GB8076 concrete admixture, and the gas bubble structure and parameters of the corresponding concrete test piece are measured by using a gas bubble parameter measuring instrument, and the experimental result is shown in Table 1. The bending and fixing amount in the examples and the comparative examples in the table is different because if the same amount is used, the initial air entraining amount is different greatly, and the data of air content stability and strength influence are not easy to compare, so the application example adjusts the amount of doping to make the initial air entraining amount of each air entraining agent approximate, so that the subsequent air content stability, strength influence and bubble parameter results can be compared.
Specific detection results are shown in table 1:
TABLE 1 concrete air entraining agent Performance test results
The detection results in table 1 show that the concrete air entraining agent prepared by the technical scheme of the invention has the characteristics of excellent air entraining effect and small number of through holes, and has wide prospects in the development of the polymer material technology industry.
Claims (4)
1. The preparation method of the concrete air entraining agent is characterized by comprising the following specific preparation steps:
(1) mixing (N-amidino) dodecyl acrylamide and polyethylene glycol derivatives in a mass ratio of 4: 1-5: 1, mixing, adding p-dichlorobenzene accounting for 0.1-0.2 times of the mass of the polyethylene glycol derivative, ferrocene accounting for 0.08-0.12 times of the mass of the polyethylene glycol derivative and tetrahydrofuran accounting for 10-15 times of the mass of the polyethylene glycol derivative, stirring and mixing, and performing rotary evaporation and concentration to obtain an additive;
(2) mixing styrene and sodium hydroxide solution according to the volume ratio of 1: 1-1: 2, mixing, standing for layering, removing lower layer liquid to obtain upper layer liquid, washing the upper layer liquid with deionized water until the washing liquid is neutral to obtain pretreated styrene, and mixing the pretreated styrene and glycidyl methacrylate according to a mass ratio of 1.0: 1.5-1.0: 1.8, obtaining a styrene mixture, and mixing an initiator and a surfactant according to a mass ratio of 1: 18-1: 20, adding water 90-120 times the mass of potassium persulfate, stirring and mixing to obtain a mixed solution, dripping a styrene mixture 0.3-0.5 times the mass of the mixed solution into the mixed solution, stirring and mixing to obtain a blank material solution, and mixing the blank material solution and an ethanol solution according to the mass ratio of 1: 3-1: 5, mixing, performing centrifugal separation to obtain a pretreatment blank, and mixing the pretreatment blank with an ethanol solution according to a mass ratio of 1: 5-1: 6, mixing, ultrasonically dispersing and filtering to obtain pretreated microspheres;
(3) grinding and sieving the pretreated microspheres to obtain microsphere powder, and mixing the microsphere powder with water according to a mass ratio of 1: 10-1: 15, mixing, performing ultrasonic oscillation to obtain a microsphere mixture, and mixing the microsphere mixture and water according to a mass ratio of 1: 1-2: 1, mixing, adding ethylenediamine with the mass of 0.1-0.2 times of that of the microsphere mixture, stirring for reaction, filtering, washing, and drying in vacuum to obtain modified microspheres;
(4) mixing an additive and the modified microspheres in a mass ratio of 1: 3-1: and 5, mixing, adding water with the mass 5-8 times that of the additive, stirring and mixing to obtain a mixed blank, introducing carbon dioxide into the mixed blank at the speed of 10-20 mL/min at the temperature of 40-45 ℃, standing, and performing rotary evaporation and concentration to obtain the concrete air entraining agent.
2. The preparation method of the concrete air entraining agent according to the claim 1 is characterized in that: the polyethylene glycol derivative in the step (1) is any one of polyethylene glycol-p-toluenesulfonate or polyethylene glycol salicylate.
3. The preparation method of the concrete air entraining agent according to the claim 1 is characterized in that: the initiator in the step (2) is any one of potassium persulfate, sodium persulfate or ammonium persulfate.
4. The preparation method of the concrete air entraining agent according to the claim 1 is characterized in that: the surfactant in the step (2) is any one of tween-80, span-80 or sodium dodecyl benzene sulfonate.
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