CN110510906B - Alkali-free liquid accelerator and preparation method thereof - Google Patents
Alkali-free liquid accelerator and preparation method thereof Download PDFInfo
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- CN110510906B CN110510906B CN201910942774.9A CN201910942774A CN110510906B CN 110510906 B CN110510906 B CN 110510906B CN 201910942774 A CN201910942774 A CN 201910942774A CN 110510906 B CN110510906 B CN 110510906B
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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 relates to an alkali-free liquid accelerator which is prepared from polyaluminium sulfate, an alcohol amine substance, a complexing agent, an accelerator and water, and has the technical effect of quick setting on cement-based building materials.
Description
Technical Field
The invention relates to the technical field of cement-based material additives, in particular to an alkali-free liquid accelerator and a preparation method thereof, which are suitable for spraying concrete constant-speed-setting cement-based materials.
Background
The sprayed concrete is a concrete which is formed by conveying a concrete mixture prepared according to a certain proportion through a pipeline by using compressed air and spraying the concrete mixture to the surface of a rock wall or other structures at a high speed through a spraying machine, and then condensing and hardening, and is widely applied to the completion of quick support in projects such as mining, civil engineering and the like, and the quality of the sprayed concrete depends on the quality of an accelerator to a great extent.
At present, alkaline powder accelerators are commonly used in China, and although the accelerators have good accelerating effect and low price, the accelerators have the problems of high alkali content, serious corrosion to eyes and skin of constructors, large loss of later strength, dust pollution and the like. In recent years, with the development of wet shotcrete technology, wet shotcrete liquid setting accelerators have come into play. However, most of these accelerators are strongly alkaline, and similarly, they have problems of large strength loss at the later stage, high corrosiveness, poor durability, high spray resilience, and the like. The alkali-free liquid accelerator has been used more and more in recent years, and particularly, in developed countries such as japan and europe, there is almost no alkali-free liquid accelerator, and in China, the alkali-free liquid accelerator has been used more and more. In recent years, the use amount of liquid setting accelerators and market share in China are rapidly increased, a series of problems caused by high alkali content of the traditional alkaline setting accelerator are solved by gradually replacing the alkali-free setting accelerator of powder setting accelerators, and the alkali-free setting accelerator has the advantages of safety, environmental protection, no corrosion, good durability, good mechanical property, low injection resilience and the like. Therefore, the research and development of the novel high-efficiency accelerating agent are always the key points of concrete spraying scientific research, and are concerned by concrete researchers at home and abroad. In the prior art, an alkali-free liquid accelerator is researched, and patent document CN109896771 mixes a solution A and a solution B in proportion to prepare the accelerator, wherein the raw material components of the solution A comprise 45-60% of aluminum sulfate octadecahydrate, 0.05-1% of sodium fluoride, 2-5% of inorganic accelerating agent, 2-4% of organic early strength agent and 35-50% of water, the raw material for preparing the solution B comprises 45-55% of aluminum sulfate octadecahydrate, 8-15% of sodium metaaluminate, 2-4% of organic early strength agent, 3-6% of tackifier and 25-40% of water, but the components are more and the practical application is difficult, and patent document CN 110981047 utilizes 40-50% of polyaluminum sulfate, 5-10% of metakaolin, 5-15% of nano silica sol, 3-6% of alcohol amine, 1-4% of organic acid, 0.01-0.05% of thickener and 0.01-0.05% of dispersant, the balance of water is used for preparing the accelerator, the patent document CN105271867 is used for preparing polyaluminium sulfate, and the accelerator is prepared by utilizing 45-55% of the polyaluminium sulfate, 0-5% of inorganic acid, 0-2% of stabilizer, 0-2% of organic early strength agent and 0-2% of organic tackifier. Although the alkali-free liquid accelerator recorded in the prior art has the advantages of quick setting, wide cement adaptability and the like, the alkali-free liquid accelerator still has the defects of high mixing amount and poor quick setting effect on cement with high mixing amount of mixed materials.
The accelerator industry in China enters a new development stage, relevant specifications and standards are provided, and the use experience and scientific research achievements of large-scale projects under construction in China provide a better research and application platform for the development of accelerators. On the other hand, with the construction of a large number of infrastructure works, higher demands are made on the performance of shotcrete, and high-performance shotcrete having excellent workability, good adhesion, low resilience, and a small dust amount is in the direction of development. Under the condition, novel sprayed concrete accelerators are continuously developed, and the novel accelerators such as low-alkali and alkali-free accelerators, liquid accelerators and organic polymer composite accelerators are applied to sprayed concrete, so that the technical process level of the sprayed concrete is greatly improved. In conclusion, the research on the novel sprayed concrete accelerator has higher social and economic benefits.
Disclosure of Invention
In order to overcome the problems in the prior art, the invention provides the alkali-free liquid accelerator which has the technical effect of quick setting on cement-based building materials.
Specifically, the alkali-free liquid accelerator comprises polymeric aluminum sulfate, an alcohol amine substance, a complexing agent, an accelerator and water.
Preferably, the alkali-free liquid accelerator comprises, by mass, 35-50 parts of polyaluminium sulfate, 2-8 parts of alcohol amine substances, 5-15 parts of complexing agents, 1-5 parts of accelerating agents and a proper amount of water.
More preferably, the alkali-free liquid accelerator comprises, by mass, 40 parts of polyaluminium sulfate, 5 parts of alcohol amine substances, 15 parts of complexing agents, 3 parts of accelerators and 80 parts of water.
The invention adopts polyaluminium sulfate as a main component, can greatly shorten the cement setting time, and has the following reaction principle:
Al2(SO4)3the following chemical reactions can occur when the cement paste is added:
Al2(SO4)3+3Ca(OH)2+6H2O→2Al(OH)3+3CaSO4·2H2O (1)
C3A+3CaSO4·2H2O+26H2O→3CaO·A12O3·3CaSO4·32H2O (2)
Al2(SO4)3+6Ca(OH)2+26H2O→3CaO·Al2O3·3CaSO4·32H2O (3)
2Al(OH)3+3Ca(OH)2+3CaSO4+26H2O→3CaO·Al2O3·3CaSO4·32H2O (4)
SO4 2-with Ca2+The reaction generates secondary gypsum which has higher activity than the original gypsum in the cement and is easier to react with C3A reacts to generate ettringite, namely reaction formulas (1) and (2). Al (Al)2(SO4)3With Ca (OH) in the liquid phase2Can directly react to generate ettringite without C3The participation of A, namely the reaction formula (3), the ettringite is formed in the original water filling space of the cement paste, which is different from C3A is the position where hydration generates ettringite. Al (OH) formed by the reaction3Generally do not exist stably and will react with Ca (OH)2The reaction produces ettringite, i.e. reaction formula (4). A13+Can also accelerate the coagulation of C-S-H gel particles and C3And (4) hydrating the S. Consumption of Ca (OH) by Each reaction2Promote C3And (4) hydrating the S. More ettringite is cross-linked to form a network to form a skeleton of the cement paste, and meanwhile, hydrated calcium silicate gel is filled in the skeleton to promote the coagulation of the cement paste.
Preferably, the alcohol amine substance is one or more of ethanolamine, diethanolamine and triethanolamine, can promote cement hydration, is an organic early strength agent variety, and can provide early strength of concrete.
Preferably, the complexing agent is selected from organic acid, more preferably one or more of citric acid, lactic acid and tartaric acid, the organic acid can be complexed with polyaluminium sulfate to improve Al in the accelerator3+And SO4 2-The content of the complexing agent is higher than that of the solid content of the quick-setting admixture, and meanwhile, the product stability of the quick-setting admixture can be enhanced by the complexing agent, and the higher the content of the complexing agent is, the better the product stability of the quick-setting admixture is.
Preferably, the coagulant is polyaluminium chloride modified cationic polyacrylamide, and specifically, the polyaluminium chloride modified cationic polyacrylamide is prepared by the following steps: preparing 10-35% of polyaluminium chloride solution A and 0.1-0.5% of cationic polyacrylamide solution B, and mixing the solution A and the solution B according to the mass percentageUniformly mixing the mixture in a volume ratio of 1:1-2 to obtain a mixed solution C, adding an ammonium persulfate solution into the mixed solution C, mixing, slowly dropwise adding a sodium bisulfite solution, reacting at the temperature of 40-60 ℃ for 90-120min, and then carrying out centrifugal separation. The polyaluminium chloride is hydrolyzed to generate amphoteric aluminium hydroxide which is dissolved under acidic condition to form a large amount of stable aluminium ions Al3+Amphoteric aluminium hydroxide can be dissolved under alkaline condition to form aluminium hydroxide colloid, and the cationic polyacrylamide has thickening and stabilizing properties, and its charged group can promote setting of cement paste. The invention modifies the cationic polyacrylamide by adopting polyaluminium chloride, utilizes the cationic polyacrylamide to stabilize aluminum ions, improves the stability and the dispersibility of aluminum groups, avoids the interference of other ions in the liquid accelerator on the activity of the aluminum groups, can improve the solubility of the cationic polyacrylamide by utilizing charged aluminum groups, can be stably dissolved in the alkali-free liquid accelerator, enables the aluminum groups to form aluminum hydroxide colloid in a strong alkaline environment when being added into a cement environment, enables high-concentration active aluminum ions to participate in the cement hydration reaction as well, promotes the generation of ettringite, disperses the cationic polyacrylamide as a positive charge group around the aluminum groups, is rapidly combined with negative charge hydration products of cement hydration to form a spatial network structure, promotes the rapid coagulation of cement paste, and can realize 'physical-chemical' double promotion by utilizing the cationic polyacrylamide modified by the polyaluminium chloride as an accelerant, the cement-based material solidification is realized together, and the influence of the high-doping-amount mixed material on the cement-based material solidification time can be effectively avoided.
Preferably, the water is selected from deionized water.
The invention also relates to a preparation method of the alkali-free liquid accelerator, which specifically comprises the following preparation steps:
1) weighing raw materials of each component, adding water into a reaction kettle, and heating to 60-80 ℃;
2) adding the weighed complexing agent into a reaction kettle, and stirring until the complexing agent is completely dissolved;
3) adding polyaluminium sulfate for three times, and continuously stirring until the polyaluminium sulfate is completely dissolved;
4) adding the alcohol amine substance into a reaction kettle, stirring until the alcohol amine substance is completely dissolved, adding the coagulant into the reaction kettle after 30min, continuously stirring until the alcohol amine substance is completely dissolved, keeping the temperature for 30-60min, and naturally cooling to room temperature to obtain the alcohol amine compound.
Preferably, the adding time of the alcohol amine substance in the step 4) is 20-40min, the temperature is 70-80 ℃, the adding time of the coagulant is 30-60min, and the temperature is 70-80 ℃.
The invention adopts polyaluminium sulfate as a main component and an organic acid complexing agent as an auxiliary component, and can greatly improve Al in the accelerator3+And SO4 2-Content of (C), accelerated cement C3A and C3The hydration of S improves the depolymerization of the active components of the cement and the mixed material, the alcamines can also improve the early performance of the cement-based material and improve the cohesiveness when the sprayed concrete is constructed, the polyaluminium chloride modified cationic polyacrylamide is used as a coagulant, the unique physical-chemical double promotion effect is utilized to realize the rapid solidification of the cement-based material, and the influence of the high-dosage mixed material on the setting time of the cement-based material can be effectively avoided.
Detailed Description
The present invention will be described in detail with reference to examples.
Method for measuring setting time the test method is carried out according to GB/T35159-2017 accelerator for shotcrete. The specific method for measuring the coagulation time is as follows: the weighed water (140g minus the amount of water in the liquid accelerator) and 400 g of cement were put into a stirring pan, and the stirrer was started and stopped at low speed for 30 seconds. And sequentially adding the weighed liquid accelerating agent into a 50 ml syringe, stirring at a low speed for 5s, and stirring at a high speed for 15 s. Immediately placing into a round mold, tamping with a knife, slightly vibrating for several times, scraping off excessive paste, and smoothing the surface. The total operating time should not exceed 50s from the addition of the liquid accelerator.
Example 1
The alkali-free liquid accelerator comprises, by mass, 35 parts of polyaluminium sulfate, 4 parts of triethanolamine, 5 parts of tartaric acid, 2 parts of polyaluminium chloride modified cationic polyacrylamide and 80 parts of water. And (3) testing results: P.O 42.5 cement is used as a cementing material, an alkali-free liquid accelerator is added in an amount of 2%, the initial setting time of a clean slurry is 175s, and the final setting time is 430 s.
Example 2
The alkali-free liquid accelerator comprises, by mass, 38 parts of polyaluminium sulfate, 3 parts of diethanolamine, 8 parts of citric acid, 3 parts of polyaluminium chloride modified cationic polyacrylamide and 80 parts of water. And (3) testing results: P.O 42.5 cement is used as a cementing material, an alkali-free liquid accelerator is added in an amount of 2%, the initial setting time of a clear slurry is 160s, and the final setting time is 425 s.
Example 3
The alkali-free liquid accelerator comprises, by mass, 40 parts of polyaluminium sulfate, 5 parts of triethanolamine, 15 parts of citric acid, 3 parts of polyaluminium chloride modified cationic polyacrylamide and 80 parts of water. And (3) testing results: P.O 42.5 cement is used as a cementing material, an alkali-free liquid accelerator is added in an amount of 2%, the initial setting time of a clear slurry is 115s, and the final setting time is 320 s.
Example 4
The alkali-free liquid accelerator comprises, by mass, 38 parts of polyaluminium sulfate, 4 parts of diethanolamine, 13 parts of lactic acid, 4 parts of polyaluminium chloride modified cationic polyacrylamide and 80 parts of water. And (3) testing results: P.O 42.5 cement is used as a cementing material, an alkali-free liquid accelerator is added with 2 percent, the initial setting time of a clear slurry is 128s, and the final setting time is 361 s.
Example 5
The alkali-free liquid accelerator comprises 45 parts of polyaluminium sulfate, 8 parts of triethanolamine, 12 parts of citric acid, 1 part of polyaluminium chloride modified cationic polyacrylamide and 80 parts of water by mass. And (3) testing results: P.O 42.5 cement is used as a cementing material, an alkali-free liquid accelerator is added in an amount of 2%, the initial setting time of a clear slurry is 125s, and the final setting time is 345 s.
Example 6
The alkali-free liquid accelerator comprises, by mass, 40 parts of polyaluminium sulfate, 5 parts of triethanolamine, 15 parts of citric acid, 3 parts of polyaluminium chloride modified cationic polyacrylamide and 80 parts of water. And (3) testing results: P.O 42.5 cement is adopted: and (2) class II fly ash: the mass ratio of S95-grade mineral powder is 2:1:1, the mineral powder is used as a cementing material, the addition amount of an alkali-free liquid accelerator is 2%, the initial setting time of a net slurry is 122S, and the final setting time is 339S.
Comparative example 1
The alkali-free liquid accelerator comprises, by mass, 40 parts of polyaluminium sulfate, 5 parts of triethanolamine, 15 parts of citric acid and 80 parts of water. And (3) testing results: P.O 42.5 cement is used as a cementing material, an alkali-free liquid accelerator is added in an amount of 4%, the initial setting time of the clear slurry is 355s, and the final setting time is 760 s.
Comparative example 2
The alkali-free liquid accelerator comprises, by mass, 40 parts of polyaluminium sulfate, 5 parts of triethanolamine, 15 parts of citric acid, 1 part of polyaluminium chloride, 2 parts of cationic polyacrylamide and 80 parts of water. And (3) testing results: P.O 42.5 cement is used as a cementing material, the addition amount of an alkali-free liquid accelerator is 3 percent, the initial setting time of a clear slurry is 304s, and the final setting time is 659 s.
Comparative example 3
The alkali-free liquid accelerator comprises, by mass, 40 parts of polyaluminium sulfate, 5 parts of triethanolamine, 15 parts of citric acid and 80 parts of water. And (3) testing results: P.O 42.5 cement is adopted: and (2) class II fly ash: the mass ratio of S95-grade mineral powder is 2:1:1, the mineral powder is used as a cementing material, the addition amount of the alkali-free liquid accelerator is 4%, the initial setting time of the clear slurry is 516S, and the final setting time is 873S.
Finally, it should be noted that: the above embodiments are only used to illustrate the technical solution of the present invention, and not to limit the same; while the invention has been described in detail and with reference to the foregoing embodiments, it will be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; and the modifications or the substitutions do not make the essence of the corresponding technical solutions depart from the scope of the technical solutions of the embodiments of the present invention.
Claims (7)
1. An alkali-free liquid accelerator is characterized in that raw materials comprise 35-50 parts of polyaluminium sulfate, 2-8 parts of alcohol amine substances, 5-15 parts of complexing agents, 1-5 parts of accelerating agents and a proper amount of water, wherein the accelerating agents are polyaluminium chloride modified cationic polyacrylamide, and the preparation steps of the polyaluminium chloride modified cationic polyacrylamide are as follows: preparing a polyaluminum chloride solution A with the mass fraction of 10-35% and a cationic polyacrylamide solution B with the mass fraction of 0.1-0.5%, uniformly mixing the solution A and the solution B according to the volume ratio of 1:1-2 to obtain a mixed solution C, adding an ammonium persulfate solution into the mixed solution C, mixing, slowly dropwise adding a sodium bisulfite solution, reacting at the temperature of 40-60 ℃ for 90-120min, and performing centrifugal separation.
2. The alkali-free liquid accelerator according to claim 1, wherein the raw materials comprise 40 parts of polyaluminium sulfate, 5 parts of alcohol amine substances, 15 parts of complexing agents, 3 parts of coagulants and 80 parts of water.
3. The alkali-free liquid accelerator according to any one of claims 1 to 2, wherein the alcohol amine substance is one or more of ethanolamine, diethanolamine and triethanolamine.
4. The alkali-free liquid accelerator according to any one of claims 1 to 2, wherein the complexing agent is one or more selected from citric acid, lactic acid and tartaric acid.
5. The alkali-free liquid accelerator according to any one of claims 1 to 2, wherein the water is selected from deionized water.
6. The method for preparing an alkali-free liquid accelerator as claimed in any one of claims 1 to 5, comprising the steps of: 1) weighing raw materials of each component, adding water into a reaction kettle, and heating to 60-80 ℃; 2) adding the weighed complexing agent into a reaction kettle, and stirring until the complexing agent is completely dissolved; 3) adding polyaluminium sulfate for three times, and continuously stirring until the polyaluminium sulfate is completely dissolved; 4) adding the alcohol amine substance into a reaction kettle, stirring until the alcohol amine substance is completely dissolved, adding the coagulant into the reaction kettle after 30min, continuously stirring until the alcohol amine substance is completely dissolved, keeping the temperature for 30-60min, and naturally cooling to room temperature to obtain the alcohol amine compound.
7. The method for preparing the alkali-free liquid accelerator according to claim 6, wherein the adding time of the alcohol amine substance in the step 4) is 20-40min, the temperature is 70-80 ℃, the adding time of the accelerator is 30-60min, and the temperature is 70-80 ℃.
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| CN110963741A (en) * | 2019-12-27 | 2020-04-07 | 芜湖弘马新材料有限公司 | Early-strength powdery alkali-free liquid accelerator core master batch and preparation method and application thereof |
| CN111662036A (en) * | 2020-05-18 | 2020-09-15 | 山西佳维新材料股份有限公司 | Low-alkali accelerator and preparation method and application thereof |
| CN113354326A (en) * | 2021-06-30 | 2021-09-07 | 河南砼道中人新材料技术有限公司 | Green environment-friendly liquid accelerator and preparation method thereof |
| CN114014582B (en) * | 2021-11-08 | 2022-09-06 | 北京市建筑工程研究院有限责任公司 | Chlorine-free, fluorine-free and alkali-free liquid accelerator and preparation method and application thereof |
| CN114835425A (en) * | 2022-03-23 | 2022-08-02 | 中铁第一勘察设计院集团有限公司 | Liquid alkali-free accelerator and preparation method thereof |
| CN114671644B (en) * | 2022-03-24 | 2023-06-23 | 江苏奥莱特新材料股份有限公司 | High-early-strength low-resilience high-performance sprayed concrete and preparation method thereof |
| CN115819006B (en) * | 2022-11-25 | 2023-10-31 | 中建材中岩科技有限公司 | Method for preparing alkali-free liquid accelerator by using suspension |
| CN115893899B (en) * | 2022-12-19 | 2024-01-19 | 安徽中铁工程材料科技有限公司 | Antifreezing alkali-free liquid accelerator and preparation method and application thereof |
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