CN111960713A - High-performance alkali-free liquid accelerator and preparation method thereof - Google Patents

High-performance alkali-free liquid accelerator and preparation method thereof Download PDF

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CN111960713A
CN111960713A CN202010847776.2A CN202010847776A CN111960713A CN 111960713 A CN111960713 A CN 111960713A CN 202010847776 A CN202010847776 A CN 202010847776A CN 111960713 A CN111960713 A CN 111960713A
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alkali
free liquid
accelerator
liquid accelerator
aluminum
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CN111960713B (en
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王伟
周婷婷
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Hunan Jiameilesu New Material Co ltd
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Hunan Jiameilesu New Material Co ltd
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    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B40/00Processes, in general, for influencing or modifying the properties of mortars, concrete or artificial stone compositions, e.g. their setting or hardening ability
    • C04B40/0028Aspects relating to the mixing step of the mortar preparation
    • C04B40/0039Premixtures of ingredients
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B28/00Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements
    • C04B28/18Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements containing mixtures of the silica-lime type
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2103/00Function or property of ingredients for mortars, concrete or artificial stone
    • C04B2103/10Accelerators; Activators
    • C04B2103/12Set accelerators
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2111/00Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
    • C04B2111/34Non-shrinking or non-cracking materials
    • C04B2111/343Crack resistant materials

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Materials Engineering (AREA)
  • Structural Engineering (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Inorganic Chemistry (AREA)
  • Curing Cements, Concrete, And Artificial Stone (AREA)

Abstract

The invention discloses a high-performance alkali-free liquid accelerator and a preparation method thereof, and the high-performance alkali-free liquid accelerator comprises the following components: 30-45% of active aluminum hydroxide, 3-15% of fluorine-aluminum complex, 0.5-8% of early strength coagulation accelerating component, 2-8% of alcohol amine substance, 5-15% of nano silica sol, 0.5-2% of dispersing agent and water. The high-performance alkali-free liquid accelerator disclosed by the invention has the advantages that the adverse effects on the later-stage mechanical strength and the durability of concrete are weakened while a good accelerating effect is realized, the expansion cracking of the concrete can be effectively inhibited, the early-stage strength is improved, the cement adaptability is improved, and the using amount is low. The preparation method is simple to operate and mild in condition.

Description

High-performance alkali-free liquid accelerator and preparation method thereof
Technical Field
The invention belongs to the field of technology, and particularly relates to a high-performance alkali-free liquid accelerator and a preparation method thereof.
Background
With the development of wet-mixed shotcrete technology in recent years, the engineering application range of shotcrete is continuously expanded, and the shotcrete is commonly used for coal mine roadways, railway tunnels, rush repair and reinforcement, highway slopes and the like. The accelerator is an additive for quickly setting and hardening cement cementing materials, and is a key material for preparing shotcrete. The setting and hardening time of concrete slurry can be obviously shortened, the resilience is reduced, the thickness of a primary sprayed layer is increased, the time interval between two times of spraying is shortened, and the early strength of sprayed concrete is improved so as to provide payment resistance in time; initial setting time, final setting time, 1d strength, 28d strength retention rate and the like are important indicators of interest in shotcrete.
The accelerating agent is mainly divided into powdery, alkaline liquid accelerating agent and alkali-free liquid accelerating agent. The powdery accelerator has the defects of large working dust, large rebound quantity, uneven dispersion and the like in the use process. The alkali liquid accelerator improves the defects of the powdery accelerator, and the alkali accelerator is easier to disperse uniformly, so that the performance of each part of the concrete is uniformly distributed. However, the early strength loss of concrete caused by the high alkalinity is large, the corrosivity is strong, the problems that the concrete reacts with alkaline aggregate for a long time and the body of a constructor is damaged are serious, and the development of the alkaline accelerating agent is limited. The alkali-free accelerator solves the problems well, and has the advantages of no corrosion, high later strength retention rate, safety, no pollution and the like.
At present, aluminum-containing components in the alkali-free liquid accelerator are mainly aluminum sulfate and amorphous aluminum hydroxide, the ionic active aluminum ions in the product are few due to limited solubility of the aluminum sulfate, and the alkali-free accelerator product is easy to generate poor stability phenomena such as crystallization and delamination due to the concentration of high-concentration inorganic salt and the hydrolysis of aluminum phase ions, and has low early strength during use and higher rebound rate due to poor cohesiveness of concrete. Meanwhile, researches show that the alkali-free accelerator taking aluminum sulfate as a system can cause the over-high content of sulfate in the sprayed concrete, so that the hydrated C-S-H gel is subjected to decalcification reaction, the gaps of the sprayed concrete are further enlarged to form internal defects, and volume expansion cracking is generated under the action of the corrosion of external sulfate radicals. Further research shows that the concreting caused by the low-alkali setting accelerator mainly comprising aluminate has the problems of large loss of later mechanical property and durability and the like.
CN105174790A discloses an alkali-free liquid cement accelerator and its use method, which uses aluminum sulfate as main component and aluminum trifluoride to supplement aluminum content, and prepares an alkali-free liquid accelerator which does not consider the problem of aluminum fluoride solubility because aluminum fluoride is insoluble in water. CN110128044A discloses a method for preparing alkali-free liquid accelerator, which takes aluminum sulfate, waste liquid from phosphate fertilizer production containing fluorine silicic acid, aluminum hydroxide, sodium silicate and water as raw materials to prepare accelerator containing SiO2Mixing and stirring the mother liquor of the aluminum fluoride particles, sodium silicate and aluminum sulfate solution uniformly to prepare the alkali-free liquid accelerator. According to the method, two products, namely aluminum fluoride and silicon dioxide crystals, are generated simultaneously, and silicon dioxide is attached to the surface of aluminum hydroxide, so that the synthesis reaction efficiency of the mother liquor is greatly reduced, and the performance of the accelerating agent is greatly influenced. The two technical schemes not only have respective problems, but also do not solve the problems that the early strength of the low-alkali accelerator mainly comprising aluminum salt is not enough, the loss of mechanical property and durability is large in the later period, and the sprayed concrete expands and cracks due to sulfate radical corrosion.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a high-performance alkali-free liquid accelerator which can realize a good accelerating effect and simultaneously weaken adverse effects on the later mechanical strength and durability of concrete.
The technical scheme adopted by the invention for solving the technical problems is as follows:
a high-performance alkali-free liquid accelerator comprises the following components in percentage by weight:
activated aluminum hydroxide: 30 to 45 percent of
Fluorine aluminum complex: 3 to 15 percent of
Early strength coagulation-promoting component: 0.5 to 8 percent
Alcamines substance: 2 to 8 percent of
Nano silica sol: 5 to 15 percent of
Dispersing agent: 0.5 to 2 percent
Water: and (4) the balance.
The alkali-free liquid accelerator is doped with a certain content of nano silica sol as a structure stabilizer and a pH regulator, wherein the silica sol can be mixed with a hydration product Ca (OH) of portland cement2The reaction is carried out while consuming Ca (OH)2Simultaneously generates C-S-H gel with higher strength, improves the mechanical property and durability of the cement-based material, and simultaneously SiO in the silica sol2Contains a large amount of hydroxyl, can adjust the pH value of the accelerator and improve the product stability of the accelerator.
Preferably, the activated aluminum hydroxide is prepared by the following method: reacting ammonia water and aluminum nitrate crystals in a constant-temperature water bath, simultaneously dropwise adding disodium ethylene diamine tetraacetate, filtering, and obtaining a precipitate, namely active aluminum hydroxide, wherein the mass percentages of the raw materials are as follows: 13-20% of ammonia water, 63-70% of aluminum nitrate and 3-10% of disodium ethylene diamine tetraacetate.
Preferably, in the nano silica sol, the particle size of nano silicon is 800-1000 nm, and the solid content is 40%; preferably, the nano silica sol is prepared by using simple substance silicon through a one-step dissolving method, wherein the one-step dissolving method is characterized in that inorganic or organic alkali is used as a catalyst, and the simple substance silicon and pure water are adopted for reaction.
Preferably, the early strength accelerating component is calcium fluoride, calcium formate, magnesium carbonate or magnesium sulfate.
Preferably, the alcohol amine is one or more of diethanolamine, triethanolamine, triisopropanolamine and diethanolisopropanolamine.
Preferably, the dispersant is any one of hydrous magnesium silicate, polyethylene glycol and polyacrylamide.
The invention also provides a preparation method of the high-performance alkali-free liquid accelerator, which comprises the following steps:
(1) preparation of the fluorine aluminum complex: adding bottom water and hydrofluoric acid into a reaction kettle, starting a stirring device, controlling the temperature of the reaction kettle to be 50-60 ℃, adding aluminum hydroxide, and reacting for 2-4 hours under heat preservation to generate a fluorine-aluminum complex.
(2) Adding active aluminum hydroxide into the fluorine-aluminum complex prepared in the step (1), then sequentially dropwise adding the early strength coagulation promoting component and the alcohol amine substance, and after dropwise adding, carrying out heat preservation reaction for 1-2 hours at the temperature of 50-60 ℃; and then cooling to 40 ℃, adding a dispersing agent, carrying out heat preservation reaction for 30-60min, and then cooling to room temperature to obtain the accelerator base solution.
(3) And (3) uniformly mixing the nano silica sol and the accelerator base liquid prepared in the step (2), dispersing at a high speed of 5000-.
The sprayed concrete comprises the alkali-free liquid accelerator, and accounts for 4-6 wt% of the mass of the concrete cementing material.
Compared with the prior art, the invention has the beneficial effects that:
(1) the invention adopts the active aluminum hydroxide to replace the main component aluminum sulfate in the conventional alkali-free accelerator, can effectively inhibit the expansion cracking of concrete, improve the early strength and the cement adaptability, and simultaneously has low dosage;
(2) the pH regulator of the nano silica sol accelerator is utilized, the dosage of alkaline substance pH regulators used in conventional low-alkali or alkali-free accelerators due to strong acidity can be reduced (generally, sodium silicate, a small amount of liquid alkali or ammonia water is mainly used for regulating the pH value of the alkali-free or alkali-free accelerators, the later strength of concrete can be obviously reduced, and the durability of the concrete is also damaged), the nano silica sol is used as the pH regulator of the accelerator, the sodium silicate, the liquid alkali or the ammonia water and the like are not added completely, the low-alkali accelerator can be upgraded into the alkali-free accelerator, the requirements of the accelerator on the alkali-free accelerator in national standards are met (the content of equivalent Na2O is calculated to be less than or equal to 1 percent), and the later strength of the concrete is kept;
(3) the preparation method of the invention adds the active component of the nano silica sol, utilizes the strong permeability, the volcanic ash effect and the filling effect of the nano silica sol to react with calcium hydroxide in a concrete base layer to generate calcium silicate, accelerates the generation of C-S-H gel and enhances the quick setting effect of the alkali-free quick setting agent; meanwhile, the adaptability of the accelerator can be improved, and the development of early strength is promoted.
(4) The prepared alkali-free accelerator has good long-term stability, the 28d layering rate is less than or equal to 1.0%, and the storage stability at normal temperature is more than or equal to 9 months;
(5) the alkali-free liquid accelerator prepared by the preparation method has the advantages of high early strength, high retention rate of later strength and low injection resilience rate, and can be widely applied to supporting, leaking stoppage, repairing and the like of tunnels, highways, railways, mines and subways.
Detailed Description
The present invention will be further described with reference to the following examples.
In order to make the technical problems, technical solutions and advantageous effects solved by the present invention more apparent, the present invention is further described in detail below with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Example 1
The embodiment comprises the following steps:
(1) preparation of activated aluminum hydroxide: 1125g of aluminum nitrate nonahydrate aqueous solution is used as bottom water and placed in a constant temperature water bath with the temperature of 40 ℃ for reaction, meanwhile 1140g of ammonia water (20 percent) and 40g of ethylene diamine tetraacetic acid disodium aqueous solution are respectively dripped, and the precipitate is filtered, namely the active aluminum hydroxide.
(2) The preparation of the fluorine aluminum complex comprises the steps of adding 150.00g of 40% hydrofluoric acid and bottom water into a reaction kettle, starting a stirring device, controlling the temperature of the reaction kettle to be 55 ℃, adding 78.00g of aluminum hydroxide twice, and carrying out heat preservation reaction for 2 hours to generate the fluorine aluminum complex.
(3) Preparing an accelerating agent: 240.00g of active aluminum hydroxide, 40.00g of calcium fluoride and 25.00g of triethanolamine are sequentially added into the fluorine-aluminum complex reaction kettle obtained in the step (2) while stirring, the temperature is reduced to 45 ℃, and the reaction is carried out for 2.5 hours under the condition of heat preservation; after cooling to 30 ℃, 5.00g of polyacrylamide is added, and the temperature is kept for 30min and then the mixture is cooled to room temperature.
(4) And (3) uniformly mixing 60.00g of 40% concentration nano silica sol and the accelerator base liquid prepared in the step (3), dispersing at a high speed of 5000r/min for 70min, and adjusting the pH value to 3.0 to obtain the high-performance alkali-free liquid accelerator.
In the high-performance alkali-free liquid accelerator prepared in the embodiment, the components in percentage by weight are as follows: 25% of active aluminum hydroxide, 8.4% of fluorine aluminum complex, 4.2% of calcium fluoride, 2.6% of triethanolamine, 6.3% of nano silica sol, 0.5% of polyacrylamide and the balance of water.
Example 2
The embodiment comprises the following steps:
(1) preparation of activated aluminum hydroxide: 1125g of aluminum nitrate nonahydrate aqueous solution is used as bottom water and placed in a constant temperature water bath with the temperature of 40 ℃ for reaction, meanwhile 1140g of ammonia water (20%) and 45g of ethylene diamine tetraacetic acid disodium aqueous solution are respectively dripped, and the precipitate is filtered, namely the active aluminum hydroxide.
(2) The preparation of the fluorine aluminum complex comprises the steps of adding 175.00g of 40% hydrofluoric acid and bottom water into a reaction kettle, starting a stirring device, controlling the temperature of the reaction kettle to be 60 ℃, adding 78.00g of aluminum hydroxide twice, and carrying out heat preservation reaction for 3 hours to generate the fluorine aluminum complex.
(3) Preparing an accelerating agent: adding 230.00g of active aluminum hydroxide, 40.00g of magnesium carbonate and 30.00g of triisopropanolamine into the fluorine-aluminum complex reaction kettle obtained in the step (2) while stirring in sequence, cooling to 40 ℃, and carrying out heat preservation reaction for 2.5 hours; after cooling to 30 ℃, 10.00g of polyethylene glycol is added, and the temperature is kept for 30min and then the mixture is cooled to room temperature.
(4) And (3) uniformly mixing 70.00g of 40% concentration nano silica sol and the accelerator base solution prepared in the step (3), dispersing at a high speed of 6000r/min for 60min, and adjusting the pH value to 3.0 to obtain the high-performance alkali-free liquid accelerator.
In the high-performance alkali-free liquid accelerator prepared in the embodiment, the components in percentage by weight are as follows: 23% of active aluminum hydroxide, 8.2% of fluorine aluminum complex, 4.0% of magnesium carbonate, 3.0% of triisopropanolamine, 7.0% of nano silica sol, 1.0% of polyethylene glycol and the balance of water.
Example 3
The embodiment comprises the following steps:
(1) preparation of activated aluminum hydroxide: 1140g of aqueous solution of aluminum nitrate nonahydrate is taken as bottom water and placed in a constant temperature water bath with the temperature of 40 ℃ for reaction, 1140g of ammonia water (20 percent) and 50g of aqueous solution of ethylene diamine tetraacetic acid are respectively dripped at the same time, and the precipitate is filtered, namely the active aluminum hydroxide.
(2) The preparation of the fluorine aluminum complex comprises the steps of adding 150.00g of 40% hydrofluoric acid and bottom water into a reaction kettle, starting a stirring device, controlling the temperature of the reaction kettle to be 60 ℃, adding 75.00g of aluminum hydroxide twice, and carrying out heat preservation reaction for 2.5 hours to generate the fluorine aluminum complex.
(3) Preparing an accelerating agent: adding 235.00g of active aluminum hydroxide, 35.00g of magnesium sulfate and 30.00g of diethanol amine into the fluorine-aluminum complex reaction kettle obtained in the step (2) while stirring in sequence, cooling to 45 ℃, and keeping the temperature for reaction for 2 hours; after cooling to 35 ℃, 15.00g of water and magnesium silicate are added, the temperature is kept for 30min, and then the mixture is cooled to room temperature.
(4) And (3) uniformly mixing 65.00g of 40% concentration nano silica sol and the accelerator base solution prepared in the step (3), dispersing at a high speed of 7000r/min for 80min, and adjusting the pH value to 3.0 to obtain the high-performance alkali-free liquid accelerator.
In the high-performance alkali-free liquid accelerator prepared in the embodiment, the components in percentage by weight are as follows: 24 percent of active aluminum hydroxide, 8.0 percent of fluorine-aluminum complex, 3.6 percent of magnesium sulfate, 3.0 percent of diethanol amine, 6.6 percent of nano silica sol, 1.5 percent of water and magnesium silicate, and the balance of water.
Example 4
The embodiment comprises the following steps:
(1) preparation of activated aluminum hydroxide: 1140g of aqueous solution of aluminum nitrate nonahydrate is taken as bottom water and placed in a constant temperature water bath at 40 ℃ for reaction, 1140g of ammonia water (20%) and 55g of disodium ethylene diamine tetraacetate aqueous solution are respectively dripped at the same time, and the precipitate is filtered, namely the active aluminum hydroxide.
(2) The preparation of the fluorine aluminum complex comprises the steps of adding 163.00g of 40% hydrofluoric acid and bottom water into a reaction kettle, starting a stirring device, controlling the temperature of the reaction kettle to be 55 ℃, adding 80.00g of aluminum hydroxide twice, and carrying out heat preservation reaction for 3 hours to generate the fluorine aluminum complex.
(3) Preparing an accelerating agent: 240.00g of active aluminum hydroxide, 35.00g of calcium formate and 35.00g of diethanol monoisopropanolamine are sequentially added into the aluminum fluoride complex reaction kettle obtained in the step (2) while stirring, the temperature is reduced to 40 ℃, and the reaction is carried out for 2.5 hours under the condition of heat preservation; after cooling to 30 ℃, 10.00g of polyethylene glycol is added, and the temperature is kept for 30min and then the mixture is cooled to room temperature.
(4) And (3) uniformly mixing 75.00g of 40% concentration nano silica sol and the accelerator base solution prepared in the step (3), dispersing at a high speed of 8000r/min for 80min, and adjusting the pH value to 3.0 to obtain the high-performance alkali-free liquid accelerator.
In the high-performance alkali-free liquid accelerator prepared in the embodiment, the components in percentage by weight are as follows: 25% of active aluminum hydroxide, 8.7% of fluorine aluminum complex, 3.6% of calcium formate, 3.6% of diethanol monoisopropanolamine, 7.8% of nano silica sol, 1.0% of polyethylene glycol and the balance of water.
Example 5
The embodiment comprises the following steps:
(1) preparation of activated aluminum hydroxide: 1140g of aqueous solution of aluminum nitrate nonahydrate is taken as bottom water and placed in a constant temperature water bath with the temperature of 40 ℃ for reaction, 1140g of ammonia water (20 percent) and 60g of aqueous solution of ethylene diamine tetraacetic acid are respectively dripped simultaneously, and the precipitate is filtered, namely the active aluminum hydroxide.
(2) The preparation of the fluorine aluminum complex comprises the steps of adding 150.00g of 40% hydrofluoric acid and bottom water into a reaction kettle, starting a stirring device, controlling the temperature of the reaction kettle to be 60 ℃, adding 78.00g of aluminum hydroxide twice, and carrying out heat preservation reaction for 3.5 hours to generate the fluorine aluminum complex.
(3) Preparing an accelerating agent: 245.00g of active aluminum hydroxide, 35.00g of calcium fluoride and 30.00g of triethanolamine are sequentially added into the fluorine-aluminum complex reaction kettle obtained in the step (2) while stirring, the temperature is reduced to 45 ℃, and the reaction is carried out for 2 hours under the condition of heat preservation; after the temperature is reduced to 35 ℃, 7.00g of polyacrylamide is added, the temperature is kept for 30min, and then the mixture is cooled to the room temperature.
(4) And (3) uniformly mixing 70.00g of 40% concentration nano silica sol and the accelerator base solution prepared in the step (3), dispersing at a high speed of 7000r/min for 70min, and adjusting the pH value to 3.0 to obtain the high-performance alkali-free liquid accelerator.
In the high-performance alkali-free liquid accelerator prepared in the embodiment, the components in percentage by weight are as follows: 26% of active aluminum hydroxide, 8.5% of fluorine aluminum complex, 3.7% of calcium fluoride, 3.2% of triethanolamine, 7.4% of nano silica sol, 0.7% of polyacrylamide and the balance of water.
Comparative example 1
The embodiment comprises the following steps:
(1) the preparation of the fluorine aluminum complex comprises the steps of adding 150.00g of 40% hydrofluoric acid and bottom water into a reaction kettle, starting a stirring device, controlling the temperature of the reaction kettle to be 60 ℃, adding 78.00g of aluminum hydroxide twice, and carrying out heat preservation reaction for 3.5 hours to generate the fluorine aluminum complex.
(2) Preparing an accelerating agent: 245.00g of aluminum sulfate, 35.00g of calcium fluoride and 30.00g of triethanolamine are sequentially added into the fluorine-aluminum complex reaction kettle obtained in the step (2) while stirring, the temperature is reduced to 45 ℃, and the reaction is carried out for 2 hours under the condition of heat preservation; after the temperature is reduced to 35 ℃, 7.00g of polyacrylamide is added, the temperature is kept for 30min, and then the mixture is cooled to the room temperature.
And adjusting the pH value to 3.0 to obtain the high-performance alkali-free liquid accelerator.
In the high-performance alkali-free liquid accelerator prepared in the embodiment, the components in percentage by weight are as follows: 26% of aluminum sulfate, 8.5% of fluorine-aluminum complex, 3.7% of calcium fluoride, 3.2% of triethanolamine, 7.4% of nano silica sol, 0.7% of polyacrylamide and the balance of water.
The liquid alkali-free accelerators obtained in examples 1 to 5 and comparative example 1 were tested according to the following relevant standards:
GB T8077-2012 test method for homogeneity of concrete admixture
Accelerating agent for GBT 35159 and 2017 shotcrete
The alkali-free liquid accelerator prepared in the embodiment 1-5 and the comparative example 1 are subjected to a control test, and a compressive strength test is carried out; and carrying out initial and final setting time test on the liquid alkali-free accelerator according to the standard' GBT 35159-:
setting time test materials used: 400g of cement, 140g of water (containing water in the liquid alkali-free setting accelerator), and 6 percent of the doping amount of the liquid alkali-free setting accelerator, namely 24g of cement.
Materials used for compressive strength test: 900g of cement, 450g of water (containing water of the alkali-free liquid accelerator) and 1350g of standard sand.
The accelerator is added into the cement paste according to 4-6% of the weight of cement, and the water consumption comprises the water contained in the liquid accelerator. Using comparative example 1 as a control, the setting time of the cement paste, the mortar strength and the stability were tested. The test results are shown in tables 1 and 2.
TABLE 1 Cement paste setting time test results
Figure 794659DEST_PATH_IMAGE001
TABLE 2 Cement mortar Strength testing and stability
Figure 242958DEST_PATH_IMAGE002
As can be seen from tables 1 and 2, the initial setting time and the final setting time of the high-strength stable liquid accelerator are shorter than those of the high-strength stable liquid accelerator in comparison with the comparative example 1, and the high-strength stable liquid accelerator has higher retention rate of 1d compressive strength, 28d compressive strength and 90d compressive strength and better stability.
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 present invention, so that any modifications, equivalents and improvements made by the present invention as described in the specification are included in the scope of the present invention.

Claims (8)

1. The high-performance alkali-free liquid accelerator is characterized by comprising the following components in percentage by weight:
activated aluminum hydroxide: 30 to 45 percent;
fluorine aluminum complex: 3 to 15 percent;
early strength coagulation-promoting component: 0.5 to 8 percent;
alcamines substance: 2 to 8 percent;
nano silica sol: 5 to 15 percent;
dispersing agent: 0.5-2%;
water: and (4) the balance.
2. The high-performance alkali-free liquid accelerator according to claim 1, wherein the activated aluminum hydroxide is prepared by the following method: reacting ammonia water and aluminum nitrate crystals in a constant-temperature water bath, simultaneously dropwise adding disodium ethylene diamine tetraacetate, filtering, and obtaining a precipitate, namely active aluminum hydroxide, wherein the mass percentages of the raw materials are as follows: 13-20% of ammonia water, 63-70% of aluminum nitrate and 3-10% of disodium ethylene diamine tetraacetate.
3. The high-performance alkali-free liquid accelerator as claimed in claim 1 or 2, wherein in the nano silica sol, the nano silica has a particle size of 800-1000 nm and a solid content of 40%; preferably, the nano silica sol is prepared by using simple substance silicon through a one-step dissolving method, wherein the one-step dissolving method is characterized in that inorganic or organic alkali is used as a catalyst, and the simple substance silicon and pure water are adopted for reaction.
4. The high-performance alkali-free liquid accelerator as claimed in any one of claims 1 to 3, wherein the early strength accelerating component is calcium fluoride, calcium formate, magnesium carbonate or magnesium sulfate.
5. The high-performance alkali-free liquid accelerator according to any one of claims 1 to 4, wherein the alcohol amine is one or more selected from the group consisting of diethanolamine, triethanolamine, triisopropanolamine and diethanolisopropanolamine.
6. The high-performance alkali-free liquid accelerator as claimed in any one of claims 1 to 5, wherein the dispersant is any one of hydrated magnesium silicate, polyethylene glycol and polyacrylamide.
7. The preparation method of the high-performance alkali-free liquid accelerator as claimed in any one of claims 1 to 4, which is characterized by comprising the following steps:
(1) preparation of the fluorine aluminum complex: adding bottom water and hydrofluoric acid into a reaction kettle, starting a stirring device, controlling the temperature of the reaction kettle to be 50-60 ℃, adding aluminum hydroxide, and reacting for 2-4 hours under heat preservation to generate a fluorine-aluminum complex;
(2) adding active aluminum hydroxide into the fluorine-aluminum complex prepared in the step (1), then sequentially dropwise adding the early strength coagulation promoting component and the alcohol amine substance, and after dropwise adding, carrying out heat preservation reaction for 1-2 hours at the temperature of 50-60 ℃; then cooling to 40 ℃, adding a dispersing agent, carrying out heat preservation reaction for 30-60min, and cooling to room temperature to obtain an accelerator base solution;
(3) and (3) uniformly mixing the nano silica sol and the accelerator base liquid prepared in the step (2), dispersing at a high speed of 5000-.
8. The sprayed concrete is characterized by comprising the alkali-free liquid accelerator, wherein the alkali-free liquid accelerator accounts for 4-6 wt% of the mass of a concrete cementing material.
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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112456853A (en) * 2020-12-16 2021-03-09 湖南加美乐素新材料股份有限公司 High-strength alkali-free liquid accelerator and preparation method thereof
CN112456849A (en) * 2020-12-21 2021-03-09 西安建筑科技大学 Alkali-free liquid accelerator prepared from fluorine-aluminum complex and preparation method thereof
CN112608056A (en) * 2020-11-27 2021-04-06 陕西科之杰新材料有限公司 Liquid accelerator and preparation method thereof
CN113087441A (en) * 2021-03-05 2021-07-09 山西佳维新材料股份有限公司 Fluoride-free liquid alkali-free accelerator and preparation method and application thereof
CN113200704A (en) * 2021-05-19 2021-08-03 湖南加美乐素新材料股份有限公司 Environment-friendly stable alkali-free liquid accelerator and preparation method and application thereof

Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101648785A (en) * 2009-09-14 2010-02-17 江苏博特新材料有限公司 Alkali-free liquid setting accelerator
CN102219425A (en) * 2011-04-15 2011-10-19 中铁隧道集团有限公司 Alkali-free liquid accelerating agent and preparation method thereof
EP2500329A1 (en) * 2011-03-17 2012-09-19 Industrias Quimicas del Ebro, S.A. A method for preparing a set accelerator, the product obtained and its use
CN104193211A (en) * 2014-08-18 2014-12-10 刘翠芬 Heating-free non-alkali liquid accelerator for jetting concrete and preparation method of heating-free non-alkali liquid accelerator
CN104446090A (en) * 2014-12-08 2015-03-25 江苏奥莱特新材料有限公司 Durable alkali-free liquid setting accelerator and preparation method thereof
CN108358497A (en) * 2018-05-10 2018-08-03 江苏地基工程有限公司 Novel foundation pit waterproof curtain added material alkali-free liquid accelerator and preparation method thereof
CN109824294A (en) * 2019-03-25 2019-05-31 科之杰新材料集团有限公司 A kind of high-strength stable type liquid accelerator and preparation method thereof

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101648785A (en) * 2009-09-14 2010-02-17 江苏博特新材料有限公司 Alkali-free liquid setting accelerator
EP2500329A1 (en) * 2011-03-17 2012-09-19 Industrias Quimicas del Ebro, S.A. A method for preparing a set accelerator, the product obtained and its use
CN102219425A (en) * 2011-04-15 2011-10-19 中铁隧道集团有限公司 Alkali-free liquid accelerating agent and preparation method thereof
CN104193211A (en) * 2014-08-18 2014-12-10 刘翠芬 Heating-free non-alkali liquid accelerator for jetting concrete and preparation method of heating-free non-alkali liquid accelerator
CN104446090A (en) * 2014-12-08 2015-03-25 江苏奥莱特新材料有限公司 Durable alkali-free liquid setting accelerator and preparation method thereof
CN108358497A (en) * 2018-05-10 2018-08-03 江苏地基工程有限公司 Novel foundation pit waterproof curtain added material alkali-free liquid accelerator and preparation method thereof
CN109824294A (en) * 2019-03-25 2019-05-31 科之杰新材料集团有限公司 A kind of high-strength stable type liquid accelerator and preparation method thereof

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
厉衡隆等: "《铝冶炼生产技术手册》", 31 July 2011, 北京:冶金工业出版社 *
古朝建等: "氟铝络合物制备无碱液体速凝剂及性能研究", 《新型建筑材料》 *

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112608056A (en) * 2020-11-27 2021-04-06 陕西科之杰新材料有限公司 Liquid accelerator and preparation method thereof
CN112456853A (en) * 2020-12-16 2021-03-09 湖南加美乐素新材料股份有限公司 High-strength alkali-free liquid accelerator and preparation method thereof
CN112456849A (en) * 2020-12-21 2021-03-09 西安建筑科技大学 Alkali-free liquid accelerator prepared from fluorine-aluminum complex and preparation method thereof
CN113087441A (en) * 2021-03-05 2021-07-09 山西佳维新材料股份有限公司 Fluoride-free liquid alkali-free accelerator and preparation method and application thereof
CN113200704A (en) * 2021-05-19 2021-08-03 湖南加美乐素新材料股份有限公司 Environment-friendly stable alkali-free liquid accelerator and preparation method and application thereof

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