CN109279809B - Modified air entraining agent and preparation method thereof - Google Patents
Modified air entraining agent and preparation method thereof Download PDFInfo
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- CN109279809B CN109279809B CN201811171081.6A CN201811171081A CN109279809B CN 109279809 B CN109279809 B CN 109279809B CN 201811171081 A CN201811171081 A CN 201811171081A CN 109279809 B CN109279809 B CN 109279809B
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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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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
Abstract
The invention relates to the technical field of air entraining agents, in particular to a modified air entraining agent and a preparation method thereof, wherein the modified air entraining agent comprises the following components in parts by weight: 50-60 parts of allyl fatty alcohol-polyoxyethylene ether, 5-9 parts of sodium laureth sulfate, 15-20 parts of sulfamic acid, 0.6-1 part of urea peroxide, 1-4 parts of an antifreezing component, 0.2-0.6 part of catechol, 0.7-1.3 parts of hydroxypropyl methyl fiber, 0.1-0.4 part of starch ether and 66-70 parts of water; the air entraining agent effectively solves the problem of poor adaptability with polycarboxylic acid water reducing agents and cement, has the advantages of simple process, quick reaction, good bubble and bubble stabilizing effect and good bubble compactness and bubble stabilizing time, can introduce fine and uniform stable bubbles into concrete, effectively improves the strength and frost resistance of the concrete when used in combination with the water reducing agents, and reduces the slump loss of the concrete.
Description
Technical Field
The invention relates to the technical field of air entraining agents, in particular to a modified air entraining agent and a preparation method thereof.
Background
The air entraining agent is the most economical and effective material which can obviously improve the workability of concrete and the internal pore structure of hardened concrete and improve the frost resistance of the concrete, and is an additive which can reduce the reaction risk of the alkali aggregate of the concrete and greatly improve the comprehensive durability of the concrete such as impermeability, chemical corrosion resistance and the like. Currently, the types of concrete air entraining agents commonly used are: 1) the rosin has the characteristics of simple preparation, low price, good foamability, large bubbles and the like; 2) the alkyl benzene sulfonate has the characteristics of good foamability, large bubbles, poor stability and the like; 3) saponins have the characteristics of good water solubility, easy deliquescence, good bubble structure and the like; 4) fatty acid and salts thereof have the characteristics of poor foamability, small bubbles and the like; however, when the polycarboxylic acid water reducer is mixed with the rosin thermopolymer or the saponin concrete air entraining agent, the two are often incompatible, and the air entraining agent floats on the surface of the solution in a layered manner or precipitates at the bottom of the solution in a flocculent manner, so that the research on the air entraining agent with excellent performance and good adaptability to the polycarboxylic acid water reducer and the cement is very important.
Disclosure of Invention
In order to solve the technical problems, the invention provides a modified air entraining agent and a preparation method thereof.
The method is realized according to the following technical scheme:
a modified air entraining agent comprises the following components in parts by weight: 50-60 parts of allyl fatty alcohol-polyoxyethylene ether, 5-9 parts of sodium laureth sulfate, 15-20 parts of sulfamic acid, 0.6-1 part of urea peroxide, 1-4 parts of an antifreezing component, 0.2-0.6 part of catechol, 0.7-1.3 parts of hydroxypropyl methyl fiber, 0.1-0.4 part of starch ether and 66-70 parts of water.
The temperature of the water is 45-50 ℃.
The antifreezing component is one or a composition of more than two of calcium nitrate, calcium formate, calcium acetate and calcium thiocyanate.
The preparation method of the modified air entraining agent comprises the following steps:
s1, placing allyl fatty alcohol-polyoxyethylene ether, sulfamic acid and urea peroxide in a titanium alloy reactor, stirring uniformly, raising the temperature to 100 ℃ in stages, adding catechol, stirring uniformly, and carrying out heat preservation treatment for 1-1.5 hours;
s2, cooling the product obtained in the step S1 to 82-87 ℃, adding hydroxypropyl methyl cellulose and starch ether, uniformly stirring, and carrying out heat preservation treatment for 20-30 min;
s3, cooling the product obtained in the step S2 to 62-67 ℃, adding an antifreezing agent, uniformly stirring, and carrying out heat preservation treatment for 10-15 min.
S4, adding water and sodium laureth sulfate into the product obtained in the step S3, and uniformly mixing to obtain the modified air entraining agent.
The step-by-step temperature rise is divided into three stages, wherein the temperature rises to 80 ℃ in the first stage and 90 ℃ in the second stage.
The temperature is raised to 80 ℃ at the speed of 0.2-0.5 ℃/min, and then the temperature is preserved for 10 min.
The two-stage heating is carried out at the speed of 0.8-1.2 ℃/min to 90 ℃, and then the heat preservation treatment is carried out for 20 min.
And in the third stage, the temperature is raised to 100 ℃ at the speed of 0.2-0.5 ℃/min, and then the heat preservation treatment is carried out for 8 min.
Compared with the prior art, the invention has the beneficial effects that:
the air entraining agent effectively solves the problem of poor adaptability with polycarboxylic acid water reducing agents and cement, has the advantages of simple process, quick reaction, good bubble and bubble stabilizing effect and good bubble compactness and bubble stabilizing time, can introduce fine and uniform stable bubbles into concrete, effectively improves the strength and frost resistance of the concrete when used in combination with the water reducing agents, and reduces the slump loss of the concrete.
The invention adopts catechol to promote the reaction of allyl fatty alcohol-polyoxyethylene ether, sulfamic acid and urea peroxide, shortens the reaction time, adopts hydroxypropyl methyl fiber and starch ether to further improve the viscosity and elasticity of the bubble wall, and further improves the bubble stability; the sodium laureth sulfate is adopted, so that the reactivity of the air entraining agent is further improved, and the adaptability and the solubility of the air entraining agent are further improved.
Detailed Description
The following is a detailed description of the embodiments of the present invention, but the present invention is not limited to these embodiments, and any modifications or substitutions in the basic spirit of the embodiments are included in the scope of the present invention as claimed in the claims.
Example 1
A modified air entraining agent comprising: 60g of allyl fatty alcohol-polyoxyethylene ether, 9g of sodium laureth sulfate, 20g of sulfamic acid, 1g of urea peroxide, 4g of an antifreezing component, 0.6g of catechol, 1.3g of hydroxypropyl methyl fiber and 0.4g of starch ether, and 70g of water with the temperature of 50 ℃;
the antifreezing component is a composition of calcium nitrate, calcium formate, calcium acetate and calcium thiocyanate;
the preparation method of the modified air entraining agent comprises the following steps:
s1, placing allyl fatty alcohol-polyoxyethylene ether, sulfamic acid and urea peroxide in a titanium alloy reactor, uniformly stirring, heating to 100 ℃ in three stages, adding catechol, uniformly stirring, and performing heat preservation treatment for 1.5 hours;
s2, cooling the product obtained in the step S1 to 87 ℃, adding hydroxypropyl methyl cellulose and starch ether, uniformly stirring, and carrying out heat preservation treatment for 30 min;
s3, cooling the product obtained in the step S2 to 67 ℃, adding an antifreezing agent, uniformly stirring, and carrying out heat preservation treatment for 15 min.
S4, adding water and sodium laureth sulfate into the product obtained in the step S3, and uniformly mixing to obtain a modified air entraining agent;
the temperature is raised to 80 ℃ at the speed of 0.5 ℃/min in the first stage, and then the heat preservation treatment is carried out for 10 min;
the two-stage heating is carried out, namely heating to 90 ℃ at the speed of 1.2 ℃/min, and then carrying out heat preservation treatment for 20 min;
and in the third stage, the temperature is raised to 100 ℃ at the speed of 0.5 ℃/min, and then the heat preservation treatment is carried out for 8 min.
Example 2
A modified air entraining agent comprising: 50g of allyl fatty alcohol-polyoxyethylene ether, 5g of sodium laureth sulfate, 15g of sulfamic acid, 0.6g of urea peroxide, 1-4g of an antifreezing component, 0.2g of catechol, 0.7g of hydroxypropyl methyl fiber, 0.1g of starch ether and 66g of water with the temperature of 45 ℃;
the antifreezing component is calcium formate;
the preparation method of the modified air entraining agent comprises the following steps:
s1, placing allyl fatty alcohol-polyoxyethylene ether, sulfamic acid and urea peroxide in a titanium alloy reactor, uniformly stirring, heating to 100 ℃ in three stages, adding catechol, uniformly stirring, and performing heat preservation treatment for 1 h;
s2, cooling the product obtained in the step S1 to 82 ℃, adding hydroxypropyl methyl cellulose and starch ether, uniformly stirring, and carrying out heat preservation treatment for 20 min;
s3, cooling the product obtained in the step S2 to 62 ℃, adding an antifreezing agent, uniformly stirring, and carrying out heat preservation treatment for 10 min.
S4, adding water and sodium laureth sulfate into the product obtained in the step S3, and uniformly mixing to obtain a modified air entraining agent;
the temperature is raised to 80 ℃ at the speed of 0.2 ℃/min in the first stage, and then the heat preservation treatment is carried out for 10 min;
the two-stage heating is carried out, namely the temperature is raised to 90 ℃ at the speed of 0.8 ℃/min, and then the heat preservation treatment is carried out for 20 min;
and in the third stage, the temperature is raised to 100 ℃ at the speed of 0.2 ℃/min, and then the heat preservation treatment is carried out for 8 min.
Example 3
A modified air entraining agent comprising: 55g of allyl fatty alcohol-polyoxyethylene ether, 7g of sodium laureth sulfate, 18g of sulfamic acid, 0.8g of urea peroxide, 1-4g of an antifreezing component, 0.4g of catechol, 1g of hydroxypropyl methyl fiber, 0.2g of starch ether and 68g of water with the temperature of 50 ℃;
the antifreezing component is a composition of calcium nitrate and calcium formate;
the preparation method of the modified air entraining agent comprises the following steps:
s1, placing allyl fatty alcohol-polyoxyethylene ether, sulfamic acid and urea peroxide in a titanium alloy reactor, uniformly stirring, heating to 100 ℃ in three stages, adding catechol, uniformly stirring, and performing heat preservation treatment for 1.2 hours;
s2, cooling the product obtained in the step S1 to 85 ℃, adding hydroxypropyl methyl cellulose and starch ether, uniformly stirring, and carrying out heat preservation treatment for 25 min;
s3, cooling the product obtained in the step S2 to 65 ℃, adding an anti-freezing agent, uniformly stirring, and carrying out heat preservation treatment for 12 min.
S4, adding water and sodium laureth sulfate into the product obtained in the step S3, and uniformly mixing to obtain a modified air entraining agent;
the temperature is raised to 80 ℃ at the speed of 0.4 ℃/min in the first stage, and then the heat preservation treatment is carried out for 10 min;
the two-stage heating is carried out, namely the temperature is raised to 90 ℃ at the speed of 1 ℃/min, and then the heat preservation treatment is carried out for 20 min;
and in the third stage, the temperature is raised to 100 ℃ at the speed of 0.3 ℃/min, and then the heat preservation treatment is carried out for 8 min.
Comparative example 1
Preparing an air entraining agent: putting 50g of fatty alcohol-polyoxyethylene ether, 18g of sulfamic acid and 0.5g of urea into a flask, continuously stirring, gradually heating to 100 ℃, and keeping the temperature constant for 4 hours; and cooling to 70 ℃, adding 370g of hot water for dilution, cooling to 40 ℃, adding 10g of modified silicone polyether microemulsion, and fully and uniformly stirring to obtain the air entraining agent.
Comparative example 2
Adding 250g of water and 25g of sodium hydroxide into a 1000 ml reaction kettle, heating to 90 ℃, slowly adding 250g of rosin powder, keeping the temperature at 90 ℃ for reaction for 2-3h, adding 25gOP-10 emulsifier, adjusting the solid content by water to 35%, and controlling the pH value to be 8.5-9.5 to obtain the air entraining agent.
Test example 1
The air entraining agents prepared in examples 1 to 3 and the air entraining agents prepared in comparative examples 1 and 2 were prepared as 5% aqueous solutions, and the stability thereof is shown in table 1:
TABLE 1
Test example 2
The air entraining agents prepared in examples 1 to 3 and the air entraining agents prepared in comparative examples 1 to 2 were subjected to tests on air content and slump with a polycarboxylic acid water reducing agent and portland cement, and the cement was selected as portland cement with a bonding amount of 0.08% by mass of the cement, and the results are shown in table 2:
TABLE 2
| Slump (cm) | Gas content (%) | |
| Example 1 | 19.8 | 3.5 |
| Example 2 | 19.3 | 3.6 |
| Example 3 | 20.5 | 3.4 |
| Comparative example 1 | 12.3 | 5.5 |
| Comparative example 2 | 18.5 | 3.4 |
Claims (7)
1. The modified air entraining agent is characterized by comprising the following components in parts by weight: 50-60 parts of allyl fatty alcohol-polyoxyethylene ether, 5-9 parts of sodium laureth sulfate, 15-20 parts of sulfamic acid, 0.6-1 part of urea peroxide, 1-4 parts of an antifreezing component, 0.2-0.6 part of catechol, 0.7-1.3 parts of hydroxypropyl methyl cellulose, 0.1-0.4 part of starch ether and 66-70 parts of water;
the preparation method of the modified air entraining agent comprises the following steps:
s1, placing allyl fatty alcohol-polyoxyethylene ether, sulfamic acid and urea peroxide in a titanium alloy reactor, stirring uniformly, raising the temperature to 100 ℃ in stages, adding catechol, stirring uniformly, and carrying out heat preservation treatment for 1-1.5 hours;
s2, cooling the product obtained in the step S1 to 82-87 ℃, adding hydroxypropyl methyl cellulose and starch ether, uniformly stirring, and carrying out heat preservation treatment for 20-30 min;
s3, cooling the product obtained in the step S2 to 62-67 ℃, adding an antifreezing component, uniformly stirring, and carrying out heat preservation treatment for 10-15 min;
s4, adding water and sodium laureth sulfate into the product obtained in the step S3, and uniformly mixing to obtain the modified air entraining agent.
2. The modified air entraining agent of claim 1 wherein the water is at a temperature of from 45 ℃ to 50 ℃.
3. The modified air entraining agent of claim 1 wherein the antifreeze component is one or more of calcium nitrate, calcium formate, calcium acetate and calcium thiocyanate.
4. The modified air entraining agent according to claim 1 wherein the stepwise temperature increase is divided into three stages, the first stage temperature increase to 80 ℃ and the second stage temperature increase to 90 ℃.
5. The modified air entraining agent according to claim 4, wherein the temperature is raised to 80 ℃ in the first stage at a rate of 0.2-0.5 ℃/min and then the temperature is maintained for 10 min.
6. The modified air entraining agent according to claim 4, wherein the temperature rise in the second stage is carried out at a rate of 0.8-1.2 ℃/min to 90 ℃, and then the temperature is maintained for 20 min.
7. The modified air entraining agent according to claim 4, wherein the temperature is raised to 100 ℃ at a rate of 0.2-0.5 ℃/min in the third stage, and then the temperature is maintained for 8 min.
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| CN111217970B (en) * | 2020-02-25 | 2022-06-17 | 陕西科技大学 | Modified starch concrete air entraining agent and preparation method thereof |
| CN115947563A (en) * | 2022-10-27 | 2023-04-11 | 贵州大学 | Polyether air entraining agent and preparation method and application thereof |
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| CA2081299C (en) * | 1991-10-25 | 2003-07-29 | Arpad Savoly | Foaming agent composition and process |
| CN102276290A (en) * | 2011-07-18 | 2011-12-14 | 马清浩 | Concrete foaming agent and composite additive containing same |
| CN104540804A (en) * | 2011-11-10 | 2015-04-22 | 罗地亚经营管理公司 | Novel method to manufacture surface active compounds such as sulfate betaine |
| CN103937466A (en) * | 2014-03-14 | 2014-07-23 | 长江大学 | Foaming agent used for oilfield development |
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