CN110615638A - Low-temperature-resistant liquid alkali-free setting accelerator and preparation method thereof - Google Patents
Low-temperature-resistant liquid alkali-free setting accelerator and preparation method thereof Download PDFInfo
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- CN110615638A CN110615638A CN201910979194.7A CN201910979194A CN110615638A CN 110615638 A CN110615638 A CN 110615638A CN 201910979194 A CN201910979194 A CN 201910979194A CN 110615638 A CN110615638 A CN 110615638A
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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
- C04B2103/10—Accelerators; Activators
- C04B2103/12—Set accelerators
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Organic Chemistry (AREA)
- Curing Cements, Concrete, And Artificial Stone (AREA)
Abstract
The invention provides a low-temperature-resistant liquid alkali-free accelerator and a preparation method thereof. The accelerator comprises the following components in percentage by mass: 40-50% of aluminum sulfate, 5-10% of alcohol amine, 0.01-0.05% of stabilizer, 4-6% of reinforcing agent, 1-2% of modified nano material, 1-2% of pH regulator and 29.95-48.99% of water. The invention can effectively solve the defect that the conventional alkali-free accelerator is easy to freeze at low temperature, and obviously improves the stability, the mechanical property and the durability of the product.
Description
Technical Field
The application relates to the technical field of concrete admixtures, in particular to a low-temperature-resistant liquid alkali-free accelerator and a preparation method thereof.
Background
The accelerating agent is an additive which is added into concrete and can make the concrete quickly set and harden. The accelerating agent can be divided into powder and liquid according to the form, and can be divided into alkali and alkali-free according to the characteristics. After the cement is mixed, the accelerating agent can promote the cement to be hydrated and coagulated quickly, and form enough strength in a short time, so as to achieve the purpose of quickly coagulating the concrete in rush repairs or roadways, and the accelerating agent is an indispensable additive in a sprayed concrete construction method.
With the current increasing concern of people on environmental friendliness and concrete durability, the alkali-free accelerator gradually becomes a mainstream product by virtue of the advantages of no alkali, no chlorine, no pungent smell, good cohesiveness, low resilience, high later strength storage rate, high impermeability grade and the like.
Because the aluminum salt which is the main component in the accelerator system is in a supersaturated state (the adding proportion is 50-70%), the homogeneous state is completely maintained by virtue of the stable component and the solubilizing component, and therefore, the accelerator system can rapidly destabilize and crystallize under the condition of low temperature (below 5 ℃), and the coagulation accelerating effect is seriously influenced. In addition, the hydration promoting effect of the conventional accelerating agent at low temperature is obviously reduced, and the technical requirements of accelerating setting and early strength cannot be met.
Because the main synthetic raw materials of the liquid alkali-free setting accelerator of various manufacturers are basically consistent at present, the selection of an efficient antifreezing component without side effect becomes the key point for solving the technical problem.
Chinese patent CN107298540A discloses a method for preparing an anti-freezing alkali-free accelerator, which comprises the steps of uniformly mixing soluble starch, N-dimethylglycine and trimethylglycine to prepare an anti-freezing solution, and then uniformly mixing the anti-freezing solution and the prepared alkali-free accelerator to obtain the anti-freezing alkali-free accelerator.
However, the method for preparing the anti-freeze alkali-free accelerator has the following disadvantages: the antifreeze component-soluble starch adopted by the method is adsorbed on the surface of cement particles, can generate a certain retarding effect, is not beneficial to the rapid hydration of cement, and can cause the problem of poor adaptability when meeting part of cement. In addition, the whole process needs to be synthesized by two methods, namely, after the alkali-free accelerator and the antifreeze are respectively synthesized, the alkali-free accelerator and the antifreeze are mixed to obtain a final product, and the production efficiency is low.
Chinese patent CN108516720A discloses an anti-freezing alkali-free liquid accelerator and a preparation method thereof, wherein the accelerator is prepared from water-soluble aluminum salt, polyaluminum salt, alkaline earth nitrate and/or carbonate, alkaline earth fluoride salt, alcamines organic matters and water, and the alkaline earth nitrate is a main anti-freezing component.
However, the freezing-resistant alkali-free liquid accelerator and the preparation method thereof have the disadvantages that: the alkali-earth nitrate is used as the anti-freezing component, although the anti-freezing property of the product is improved to a certain extent, the alkali metal ions are introduced, the alkali content of the product is improved, and the core technical idea that the alkali-free accelerator is low in alkali content and high in durability is not met.
Chinese patent CN109678388A discloses an anti-freezing alkali-free liquid accelerator, which is prepared from 30-50 parts of aluminum sulfate; 3-10 parts of aluminum hydroxide; 10-18 parts of hydrofluoric acid; 8-20 parts of magnesium salt; 2-7 parts of alcohol amine; 0.5-4 parts of a stabilizer; 5-13 parts of an antifreezing component; 10-15 parts of water.
However, the antifreeze alkali-free liquid accelerator has the following disadvantages: methanol is used as an anti-freezing component, although the freezing point of a system can be effectively reduced, the anti-freezing agent does not have any help effect on strength increase and coagulation time, and in addition, the methanol has stronger volatility and is easy to stimulate eyes and skin of contact personnel.
A core master batch for a liquid alkali-free accelerator and a preparation method thereof in Chinese patent CN109748533A comprise the following components in parts by weight: 30-50 parts of water, 10-15 parts of quick-setting component, 15-20 parts of early strength component, 5-10 parts of stabilizer, 5-8 parts of defoaming agent, 0-2 parts of pH value regulator, 8-10 parts of anti-freezing component and 2-5 parts of thickening component.
However, the core master batch for liquid alkali-free setting accelerator and the preparation method thereof have disadvantages in that: one or more of sodium sulfate, magnesium sulfate and urea are used as anti-freezing components, and the sodium sulfate and the magnesium sulfate are used as alkali metal sulfate, so that the anti-freezing concrete has no anti-freezing property, is easy to crystallize and separate out at low temperature, improves the alkali content of the product and reduces the durability of the concrete. Although urea can lower the freezing point, the country has strict requirements on the release limit of ammonia, and volatile gas generated by urea can cause harm to constructors.
Furthermore, the above-mentioned several prior art techniques have a common disadvantage: namely, the introduced materials are all components with single anti-freezing performance and can not improve the main component Al of the accelerator3+The solubility of the ions may increase the ratio of solute in the solution system, which may increase the solution saturation of the accelerator system and decrease the stability.
Disclosure of Invention
In view of the above, the invention provides a low-temperature resistant liquid alkali-free accelerator and a preparation method thereof, so that the defect that the conventional alkali-free accelerator is easy to freeze at low temperature can be effectively overcome, and the product stability, the concrete mechanical property and the durability can be remarkably improved.
The technical scheme of the invention is realized as follows:
the low-temperature-resistant liquid alkali-free setting accelerator comprises the following components in percentage by mass:
40-50% of aluminum sulfate, 5-10% of alcohol amine, 0.01-0.05% of stabilizer, 4-6% of reinforcing agent, 1-2% of modified nano material, 1-2% of pH regulator and 29.95-48.99% of water.
Preferably, the alcohol amine is one or more of diethanolamine, triethanolamine or N-methylethanolamine.
Preferably, the stabilizer is one or more of hydroxymethyl cellulose, hydroxyethyl cellulose or methyl hydroxyethyl cellulose.
Preferably, the reinforcing agent is one or more of magnesium sulfate, magnesium fluosilicate or magnesium silicate.
Preferably, the modified nano material is a nano material with cement hydration activity and micro aggregate filling effect.
Preferably, the modified nano material is one or more of nano silicon dioxide or nano aluminum oxide.
Preferably, the pH regulator is one or more of hydrofluoric acid, lactic acid, or oxalic acid.
The invention also provides a preparation method of the low-temperature-resistant liquid alkali-free accelerator, which comprises the following steps:
A. mixing aluminum sulfate, alcohol amine, a stabilizer and water, and heating to 60-80 ℃;
B. sequentially adding a reinforcing agent and a modified nano material and controlling the temperature to be unchanged;
C. preserving heat for 0.5-3.5 hours, and then cooling to below 30 ℃;
D. adding a pH regulator, and stirring uniformly to finish the reaction.
Preferably, the method comprises:
mixing 50 g of aluminum sulfate, 10g of alcohol amine, 0.05g of stabilizer and 29.95g of water, and heating to 80 ℃;
sequentially adding 4g of reinforcing agent and 1g of modified nano material, and controlling the temperature to be unchanged;
preserving heat for 3.5 hours, and then cooling to below 30 ℃;
adding 1g of pH regulator, and stirring uniformly to finish the reaction.
Preferably, the method comprises:
mixing 40g of aluminum sulfate, 5g of alcohol amine, 0.01g of stabilizer and 45.99g of water, and heating to 60 ℃;
sequentially adding 6g of reinforcing agent and 2g of modified nano material, and controlling the temperature to be unchanged;
keeping the temperature for 2.5 hours, and then cooling to below 30 DEG C
Adding 1g of pH regulator, and stirring uniformly to finish the reaction.
As can be seen from the above, in the low temperature resistant liquid alkali-free accelerator and the preparation method thereof, the modified nano material is introduced as the novel antifreeze enhancement component, so that the defect that the conventional alkali-free accelerator is easy to freeze at low temperature can be effectively overcome, and the product stability, the concrete mechanical property and the durability can be remarkably improved. In addition, the anti-freezing component used in the low-temperature resistant liquid alkali-free accelerator is green and pollution-free, has no harm to human bodies, and has a remarkable improvement effect on the durability of concrete. In addition, the preparation method of the low-temperature resistant liquid alkali-free accelerator provided by the invention is a one-step synthesis process, is simple and feasible, and has high production efficiency.
Drawings
FIG. 1 is a schematic flow chart of a method for preparing a low-temperature resistant liquid alkali-free setting accelerator according to an embodiment of the present invention.
Detailed Description
In order to make the technical scheme and advantages of the invention more apparent, the invention is further described in detail with reference to the accompanying drawings and specific embodiments.
The low-temperature-resistant liquid alkali-free accelerator in the embodiment of the invention comprises the following components in percentage by mass: 40-50% of aluminum sulfate, 5-10% of alcohol amine, 0.01-0.05% of stabilizer, 4-6% of reinforcing agent, 1-2% of modified nano material, 1-2% of pH regulator and 29.95-48.99% of water.
In addition, as an example, in a preferred embodiment of the present invention, the alcohol amine is one or more of diethanolamine, triethanolamine or N-methylethanolamine.
In addition, as an example, in a preferred embodiment of the present invention, the stabilizer is one or more of hydroxymethyl cellulose, hydroxyethyl cellulose or methyl hydroxyethyl cellulose.
In addition, as an example, in a preferred embodiment of the present invention, the reinforcing agent is one or more of magnesium sulfate, magnesium fluorosilicate, or magnesium silicate.
In addition, as an example, in a preferred embodiment of the present invention, the modified nanomaterial is a nanomaterial having cement hydration activity and a micro-aggregate filling effect.
In addition, as an example, in a preferred embodiment of the present invention, the modified nanomaterial is one or more of nano silica or nano alumina.
In addition, as an example, in a preferred embodiment of the present invention, the modified nano material has a size range of 1 to 100 nanometers (nm).
In addition, as an example, in a preferred embodiment of the present invention, the pH adjusting agent is one or more of hydrofluoric acid, lactic acid, or oxalic acid.
In addition, the technical scheme of the invention also provides a preparation method of the low-temperature-resistant liquid alkali-free accelerator.
FIG. 1 is a schematic flow chart of a method for preparing a low-temperature resistant liquid alkali-free setting accelerator according to an embodiment of the present invention. As shown in fig. 1, the method for preparing the low temperature resistant liquid alkali-free setting accelerator in the embodiment of the present invention includes the following steps:
step 101, mixing aluminum sulfate, alcohol amine, a stabilizer and water, and heating to 60-80 ℃.
And 102, sequentially adding a reinforcing agent and a modified nano material, and controlling the temperature to be unchanged.
And 103, preserving heat for 0.5-3.5 hours (h), and then cooling to below 30 ℃.
And step 104, adding a pH regulator, uniformly stirring, and finishing the reaction.
The low-temperature resistant liquid alkali-free setting accelerator can be prepared through the steps 101-104.
In order to better understand the invention, the following examples are given for further illustration of the invention, but the invention is not limited to the scope of the examples.
The first embodiment is as follows:
in the first embodiment, the preparation method of the low temperature resistant liquid alkali-free setting accelerator comprises the following steps:
step 11, 50 grams (g) of aluminum sulfate, 10g of alcohol amine, 0.05g of stabilizer and 29.95g of water are mixed and heated to 80 ℃.
And step 12, sequentially adding 4g of reinforcing agent and 1g of modified nano material, and controlling the temperature to be unchanged.
And step 13, preserving the heat for 3.5 hours, and then cooling to below 30 ℃.
And step 14, adding 1g of pH regulator, and stirring uniformly to finish the reaction.
The low-temperature resistant liquid alkali-free setting accelerator can be prepared through the steps 11-14.
The second embodiment is as follows:
in the second embodiment, the preparation method of the low temperature resistant liquid alkali-free setting accelerator comprises the following steps:
step 21, mixing 40g of aluminum sulfate, 5g of alcohol amine, 0.01g of stabilizer and 45.99g of water, and heating to 60 ℃.
And step 22, sequentially adding 6g of reinforcing agent and 2g of modified nano material, and controlling the temperature to be unchanged.
And step 23, preserving the heat for 2.5 hours, and then cooling to below 30 ℃.
And step 24, adding 1g of pH regulator, and stirring uniformly to finish the reaction.
The low-temperature resistant liquid alkali-free setting accelerator can be prepared through the steps 21-24.
The low-temperature-resistant alkali-free accelerator provided by the technical scheme of the invention can obviously reduce the freezing point of an alkali-free accelerator solution, so that the accelerator is prevented from freezing or destabilizing and crystallizing; in addition, the modified nano material is introduced into the low-temperature resistant alkali-free accelerator, so that the cement hydration reaction process can be remarkably promoted, the interface binding power and the system compactness among the phases in mortar and concrete can be improved, and the structural mechanical property and the durability can be improved through the small-size filling effect and the higher hydration activity.
The following table shows the performance comparison of the inventive sample with two conventional liquid alkali-free setting accelerators on the market:
TABLE 1 comparison of the Properties of the inventive samples with other samples on the market
As can be seen from the data shown in the table above: the samples of the present invention (i.e., the samples of the above-mentioned low-temperature resistant alkali-free setting accelerator) were much longer in the stable period under a low-temperature environment than the samples of the other two prior art products. In addition, the low-temperature resistant alkali-free accelerator has obvious advantages in early and later strength.
In summary, in the technical scheme of the invention, because the modified nano material is introduced into the low temperature resistant liquid alkali-free accelerator as a novel antifreeze enhancing component, the modified nano material has the following characteristics:
(1) the water-based anti-freezing agent can be uniformly dispersed in a liquid accelerator to form a cross-linked network structure, and the freezing point of a system is effectively reduced, so that the anti-freezing property of a product is improved.
(2) The micro surface of the accelerator has a large amount of unsaturated residual bonds and hydroxyl groups in different bonding states, and the unsaturated residual bonds and the hydroxyl groups can be combined with Al which is greatly existed in an alkali-free accelerator3+Ions form coordinate bonds and phase transformation improves Al3+The solubility of the ions further improves the stability of the system and inhibits the instability crystallization.
(3) The size range of the concrete filling material is 1-100nm, the concrete filling material has a small size filling effect, and the compactness of a concrete system can be improved. In addition, it can effectively react with Ca (OH) generated in the cement hydration process2The crystal generates secondary reaction to generate C-S-H gel which is filled in the cement stone gap, the bonding interface of cement hardened slurry and aggregate is improved, the mechanical property of concrete is enhanced, and the durability is improved.
Therefore, the low-temperature resistant liquid alkali-free accelerator provided by the invention can effectively overcome the defect that the conventional alkali-free accelerator is easy to freeze at low temperature, and can also obviously improve the stability, the mechanical property and the durability of a product. In addition, the anti-freezing component used in the low-temperature resistant liquid alkali-free accelerator is green and pollution-free, has no harm to human bodies, and has a remarkable improvement effect on the durability of concrete.
In addition, the preparation method of the low-temperature resistant liquid alkali-free accelerator provided by the invention is a one-step synthesis process, is simple and feasible and has high production efficiency.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like made within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (10)
1. The low-temperature-resistant liquid alkali-free accelerator is characterized by comprising the following components in percentage by mass:
40-50% of aluminum sulfate, 5-10% of alcohol amine, 0.01-0.05% of stabilizer, 4-6% of reinforcing agent, 1-2% of modified nano material, 1-2% of pH regulator and 29.95-48.99% of water.
2. The accelerator according to claim 1, characterized in that:
the alcohol amine is one or more of diethanolamine, triethanolamine or N-methylethanolamine.
3. The accelerator according to claim 1, characterized in that:
the stabilizer is one or more of hydroxymethyl cellulose, hydroxyethyl cellulose or methyl hydroxyethyl cellulose.
4. The accelerator according to claim 1, characterized in that:
the reinforcing agent is one or more of magnesium sulfate, magnesium fluosilicate or magnesium silicate.
5. The accelerator according to claim 1, characterized in that:
the modified nano material is a nano material with cement hydration activity and micro aggregate filling effect.
6. The accelerator according to claim 1 or 5, characterized in that:
the modified nano material is one or more of nano silicon dioxide or nano aluminum oxide.
7. The accelerator according to claim 1, characterized in that:
the pH regulator is one or more of hydrofluoric acid, lactic acid or oxalic acid.
8. A method for preparing the low temperature resistant liquid alkali-free accelerator according to claims 1 to 7, which comprises the following steps:
A. mixing aluminum sulfate, alcohol amine, a stabilizer and water, and heating to 60-80 ℃;
B. sequentially adding a reinforcing agent and a modified nano material and controlling the temperature to be unchanged;
C. preserving heat for 0.5-3.5 hours, and then cooling to below 30 ℃;
D. adding a pH regulator, and stirring uniformly to finish the reaction.
9. The method of claim 8, wherein the method comprises:
mixing 50 g of aluminum sulfate, 10g of alcohol amine, 0.05g of stabilizer and 29.95g of water, and heating to 80 ℃;
sequentially adding 4g of reinforcing agent and 1g of modified nano material, and controlling the temperature to be unchanged;
preserving heat for 3.5 hours, and then cooling to below 30 ℃;
adding 1g of pH regulator, and stirring uniformly to finish the reaction.
10. The method of claim 8, wherein the method comprises:
mixing 40g of aluminum sulfate, 5g of alcohol amine, 0.01g of stabilizer and 45.99g of water, and heating to 60 ℃;
sequentially adding 6g of reinforcing agent and 2g of modified nano material, and controlling the temperature to be unchanged;
keeping the temperature for 2.5 hours, and then cooling to below 30 DEG C
Adding 1g of pH regulator, and stirring uniformly to finish the reaction.
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Cited By (5)
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| CN111454013A (en) * | 2020-04-08 | 2020-07-28 | 贵州天威建材科技有限责任公司 | Stabilizer for liquid alkali-free accelerator and preparation method thereof |
| CN111847964A (en) * | 2020-08-06 | 2020-10-30 | 贵州中兴南友建材有限公司 | High-adaptability green environment-friendly alkali-free liquid accelerator and preparation method thereof |
| CN112723787A (en) * | 2020-12-30 | 2021-04-30 | 山西佳维新材料股份有限公司 | Fluorine-free liquid accelerator and preparation method and application thereof |
| CN113860787A (en) * | 2021-02-01 | 2021-12-31 | 中国铁道科学研究院集团有限公司铁道建筑研究所 | Double-component alkali-free accelerator suitable for plateau cold regions and use method thereof |
| CN114455881A (en) * | 2022-04-13 | 2022-05-10 | 天津冶建特种材料有限公司 | Non-aqueous liquid alkali-free accelerator and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113860787A (en) * | 2021-02-01 | 2021-12-31 | 中国铁道科学研究院集团有限公司铁道建筑研究所 | Double-component alkali-free accelerator suitable for plateau cold regions and use method thereof |
| CN113860787B (en) * | 2021-02-01 | 2022-06-28 | 中国铁道科学研究院集团有限公司铁道建筑研究所 | Double-component alkali-free accelerator suitable for plateau cold regions and use method thereof |
| CN114455881A (en) * | 2022-04-13 | 2022-05-10 | 天津冶建特种材料有限公司 | Non-aqueous liquid alkali-free accelerator and preparation method thereof |
| CN114455881B (en) * | 2022-04-13 | 2022-06-21 | 天津冶建特种材料有限公司 | Non-aqueous liquid alkali-free accelerator and preparation method thereof |
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Application publication date: 20191227 |