CN112456849A - Alkali-free liquid accelerator prepared from fluorine-aluminum complex and preparation method thereof - Google Patents
Alkali-free liquid accelerator prepared from fluorine-aluminum complex and preparation method thereof Download PDFInfo
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- CN112456849A CN112456849A CN202011516791.5A CN202011516791A CN112456849A CN 112456849 A CN112456849 A CN 112456849A CN 202011516791 A CN202011516791 A CN 202011516791A CN 112456849 A CN112456849 A CN 112456849A
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- fluorine
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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)
- Silicon Compounds (AREA)
Abstract
The invention relates to the technical field of building material additives, in particular to an alkali-free liquid accelerator prepared by using a fluorine-aluminum complex and a preparation method thereof. The raw materials comprise mother liquor, fluorine-aluminum complex, alkaline silica sol and aluminum sulfate. Provides an alkali-free liquid accelerator prepared by using a fluorine aluminum complex and a preparation method thereof, and more Al is provided by compounding aluminum sulfate and the fluorine aluminum complex3+Aiming at the problems of great pollution, unsafe pollution and the like of hydrofluoric acid in the process of preparing the accelerator, the low-concentration hydrofluoric acid is adopted, and the aluminum hydroxide is dropwise added into the hydrofluoric acid solution step by step to prepare the fluorine-aluminum complex, so that the smoke is small in the preparation process, and the environmental pollution is small. The alkaline silica sol is added to improve the early strength of the accelerator, and the accelerator has excellent performance and high cost performance.
Description
Technical Field
The invention relates to the technical field of building material additives, in particular to an alkali-free liquid accelerator prepared by using a fluorine-aluminum complex and a preparation method thereof.
Background
The concrete spraying accelerator has the main functions of accelerating the solidification and hardening speed of the sprayed concrete, ensuring that the concrete reaches enough strength in a short time, reducing the rebound loss, preventing the sprayed concrete from falling off due to gravity, increasing the once spraying thickness, shortening the interval time between spraying layers and improving the productivity.
The accelerator comprises a powdery accelerator and a liquid accelerator, and the powdery accelerator is gradually eliminated due to large dust emission and large environmental pollution. At present, a large amount of liquid accelerators are used in construction, including alkaline liquid accelerators and alkali-free liquid accelerators, the alkaline liquid accelerators have the defects of strong corrosivity, large resilience amount during construction, large shrinkage of hardened concrete, large later strength loss, high content of potassium and sodium ions, deterioration of concrete durability and the like, and the alkali-free liquid accelerators have the advantages of low resilience amount, small shrinkage of hardened concrete, high later strength and the like.
For alkali-free liquid accelerators, aluminium sulphate is an excellent set accelerator component, F－Has super complexing Al3+Can increase Al in the solution3+Or the concentration of free aluminum, increases the stability of the aluminum sulfate. In addition, the reaction activity ratio of the fluorine-aluminum complex ions is Al3+Higher, the accelerator has accelerating effect under lower fluorine-aluminum complex ion mixing amount. However, hydrofluoric acid is a highly toxic and volatile liquid, great danger exists in the preparation process, and the early strength of the accelerating agent is low, so that the reduction of the consumption of the hydrofluoric acid in the accelerating agent is of great importance on the premise of ensuring the performance of the accelerating agent.
Disclosure of Invention
In order to solve the defects of the prior art, the invention aims to provide an alkali-free liquid accelerator prepared by using a fluorine-aluminum complex and a preparation method thereof, wherein aluminum sulfate and the fluorine-aluminum complex are compounded to provide more Al3+Aiming at the problems of great pollution, unsafe pollution and the like of hydrofluoric acid in the process of preparing the accelerator, the invention adopts low-concentration hydrofluoric acid and dropwise adds aluminum hydroxide into hydrofluoric acid solution step by step to prepare the fluorine-aluminum complex, and has small smoke and small environmental pollution in the preparation process. In addition, the alkaline silica sol is added to improve the early strength of the accelerator, and the accelerator has excellent performance and high cost performance.
In order to achieve the purpose, the invention provides the following technical scheme:
an alkali-free liquid accelerator prepared from a fluorine-aluminum complex comprises a mother liquor, the fluorine-aluminum complex, alkaline silica sol and aluminum sulfate.
The mother liquor comprises magnesium fluosilicate, ferrous sulfate, alcohol amine, urea and formic acid; the fluorine-aluminum complex is composed of hydrofluoric acid and aluminum hydroxide; the alkaline silica sol is a colloidal solution of silica.
In a further scheme, the alkali-free liquid accelerator prepared by using the fluorine aluminum complex comprises the following raw materials in percentage by mass: 25.0-35.0% of mother liquor; 1.5-2.5% of a fluorine-aluminum complex; 3.0-3.5% of alkaline silica sol; 40.0-50.0% of aluminum sulfate; the balance being water.
In a further scheme, the mother solution comprises the following raw materials in percentage by mass: 20.0 percent of magnesium fluosilicate; 12.0 percent of ferrous sulfate; 8.0 percent of alcohol amine; 4.0 percent of urea; 3.0 percent of formic acid and the balance of water.
The alcohol amine is one or a mixture of two of diethanolamine and triethanolamine.
In the alkaline silica sol, the particle size of the silicon dioxide is 8-15 nm, and the solid content is 30-31%.
The preparation process of the mother liquor comprises the following steps: under the conditions of normal temperature and normal pressure, adding formic acid into water for dissolving and stirring for 3-5 min, adding magnesium fluosilicate, stirring for 15-30 min until the formic acid is completely dissolved, adding urea, stirring for 3-5 min until the formic acid is completely dissolved, continuing adding alcohol amine, stirring for 10min, finally adding ferrous sulfate, and stirring until the formic acid is completely dissolved to obtain mother liquor.
The preparation method of the fluorine aluminum complex comprises the following steps: dropwise adding the aluminum hydroxide powder into a hydrofluoric acid solution with the mass percentage concentration of 30% step by step in a gradient manner, and stirring while adding until the aluminum hydroxide powder is completely dissolved to obtain the fluorine aluminum complex.
The preparation method of the fluorine aluminum complex, the quality of aluminium hydroxide is 10.0% -20.0% of the quality of hydrofluoric acid; the dropping gradient of the aluminum hydroxide powder is 3.0-5.0% of the mass of hydrofluoric acid based on the mass of the hydrofluoric acid.
The preparation method of the alkali-free liquid accelerator comprises the following steps:
and adding the mother liquor into water, stirring until the mother liquor is uniformly mixed, adding the fluorine-aluminum complex, stirring for 15-20 min, adding the alkaline silica sol, stirring for 5-10 min, and finally adding the aluminum sulfate, stirring until the aluminum sulfate is completely dissolved to obtain the alkali-free liquid accelerator.
Compared with the prior art, the invention has the following beneficial effects:
the alkali-free liquid accelerator prepared from the fluorine-aluminum complex adopts two accelerating components, namely aluminum sulfate and the fluorine-aluminum complex, greatly improves the accelerating effect of the alkali-free liquid accelerator, reduces the mixing amount of the alkali-free liquid accelerator, adopts a step-by-step dropping method for preparing the fluorine-aluminum complex, and has the advantages of small smoke and small environmental pollution in the preparation process. The alkaline silica sol is added as an early strength substance, so that the early strength of the sprayed concrete is improved. When the doping amount of the finally prepared alkali-free liquid accelerator is 6% of the mass of cement, the finally prepared alkali-free liquid accelerator can meet the requirements in the national standard accelerator for sprayed concrete (GB/T35159-2017), and the accelerator has the advantages of simple preparation of raw materials, simple production process and good economical efficiency.
Detailed Description
The present invention is further described with reference to the following embodiments, which are only preferred embodiments of the present invention and not intended to limit the present invention in other forms, and any person skilled in the art may change or modify the technical content disclosed above into equivalent embodiments with equivalent changes. Any simple modification, equivalent change and modification of the above embodiments according to the technical essence of the present invention are within the scope of the present invention, unless they depart from the technical spirit of the present invention.
Example 1
The alkali-free liquid accelerator prepared from the fluorine-aluminum complex comprises the following raw materials in percentage by mass: 25.0% of mother liquor; 1.5% of a fluorine aluminum complex; 3.0% of alkaline silica sol; 40.0 percent of aluminum sulfate; the balance being water.
The mother solution comprises the following raw materials in percentage by mass: 20.0 percent of magnesium fluosilicate; 12.0 percent of ferrous sulfate; 8.0 percent of alcohol amine; 4.0 percent of urea; 3.0% of formic acid and the balance of water; the preparation process of the mother solution comprises the following steps: under the conditions of normal temperature and normal pressure, adding formic acid into water to dissolve and stir for 3min, adding magnesium fluosilicate to stir for 15min until the formic acid is completely dissolved, adding urea to stir for 3min until the urea is completely dissolved, continuously adding alcohol amine to stir for 10min, and finally adding ferrous sulfate to stir until the ferrous sulfate is completely dissolved to obtain mother liquor.
The preparation method of the fluorine aluminum complex comprises the following steps: dropwise adding aluminum hydroxide powder into a hydrofluoric acid solution with the mass percentage concentration of 30% step by step in a gradient manner, and stirring while adding until the aluminum hydroxide powder is completely dissolved to obtain a fluorine aluminum complex; wherein the mass of the aluminum hydroxide is 10.0 percent of the mass of the hydrofluoric acid; the dropping gradient of the aluminum hydroxide powder is 3.0 percent of the mass of hydrofluoric acid based on the mass of the hydrofluoric acid.
The preparation method of the alkali-free liquid accelerator comprises the following steps:
and adding the mother liquor into water, stirring until the mother liquor is uniformly mixed, adding the fluorine-aluminum complex, stirring for 15min, adding the alkaline silica sol, stirring for 5min, and finally adding the aluminum sulfate, stirring until the aluminum sulfate is completely dissolved to obtain the alkali-free liquid accelerator.
Example 2
The alkali-free liquid accelerator prepared from the fluorine-aluminum complex comprises the following raw materials in percentage by mass: 35.0% of mother liquor; 2.5% of a fluorine aluminum complex; 3.5% of alkaline silica sol; 50.0 percent of aluminum sulfate; the balance being water.
The mother solution comprises the following raw materials in percentage by mass: 20.0 percent of magnesium fluosilicate; 12.0 percent of ferrous sulfate; 8.0 percent of alcohol amine; 4.0 percent of urea; 3.0% of formic acid and the balance of water; the preparation process of the mother solution comprises the following steps: under the conditions of normal temperature and normal pressure, adding formic acid into water to dissolve and stir for 5min, adding magnesium fluosilicate to stir for 30min until the magnesium fluosilicate is completely dissolved, adding urea to stir for 5min until the magnesium fluosilicate is completely dissolved, continuing adding alcohol amine to stir for 10min, and finally adding ferrous sulfate to stir until the magnesium fluosilicate is completely dissolved to obtain mother liquor.
The preparation method of the fluorine aluminum complex comprises the following steps: dropwise adding aluminum hydroxide powder into a hydrofluoric acid solution with the mass percentage concentration of 30% step by step in a gradient manner, and stirring while adding until the aluminum hydroxide powder is completely dissolved to obtain a fluorine aluminum complex; wherein the mass of the aluminum hydroxide is 20.0 percent of the mass of the hydrofluoric acid; the dropping gradient of the aluminum hydroxide powder is 4.0 percent of the mass of hydrofluoric acid based on the mass of the hydrofluoric acid.
The preparation method of the alkali-free liquid accelerator comprises the following steps:
and adding the mother liquor into water, stirring until the mother liquor is uniformly mixed, adding the fluorine-aluminum complex, stirring for 20min, adding the alkaline silica sol, stirring for 10min, and finally adding the aluminum sulfate, stirring until the aluminum sulfate is completely dissolved to obtain the alkali-free liquid accelerator.
Example 3
The alkali-free liquid accelerator prepared from the fluorine-aluminum complex comprises the following raw materials in percentage by mass: 30.0% of mother liquor; 2.0% of a fluorine aluminum complex; 3.0% of alkaline silica sol; 48.0 percent of aluminum sulfate; the balance being water.
The mother solution comprises the following raw materials in percentage by mass: 20.0 percent of magnesium fluosilicate; 12.0 percent of ferrous sulfate; 8.0 percent of alcohol amine; 4.0 percent of urea; 3.0% of formic acid and the balance of water; the preparation process of the mother solution comprises the following steps: under the conditions of normal temperature and normal pressure, adding formic acid into water for dissolving and stirring for 4min, adding magnesium fluosilicate, stirring for 20min until the formic acid is completely dissolved, adding urea, stirring for 4min until the urea is completely dissolved, continuously adding alcohol amine, stirring for 10min, and finally adding ferrous sulfate, stirring until the ferrous sulfate is completely dissolved, thus obtaining mother liquor.
The preparation method of the fluorine aluminum complex comprises the following steps: dropwise adding aluminum hydroxide powder into a hydrofluoric acid solution with the mass percentage concentration of 30% step by step in a gradient manner, and stirring while adding until the aluminum hydroxide powder is completely dissolved to obtain a fluorine aluminum complex; wherein the mass of the aluminum hydroxide is 15.0 percent of the mass of the hydrofluoric acid; the dropping gradient of the aluminum hydroxide powder is 5.0 percent of the mass of hydrofluoric acid based on the mass of the hydrofluoric acid.
The preparation method of the alkali-free liquid accelerator comprises the following steps:
and adding the mother liquor into water, stirring until the mother liquor is uniformly mixed, adding the fluorine-aluminum complex, stirring for 15min, adding the alkaline silica sol, stirring for 5min, and finally adding the aluminum sulfate, stirring until the aluminum sulfate is completely dissolved to obtain the alkali-free liquid accelerator.
The reaction phenomenon for preparing the fluorine aluminum complex according to the above example 1 is shown in table 1:
TABLE 1 reaction phenomena for the preparation of fluorine-aluminum complexes
| Amount of aluminum hydroxide/%) | Reaction time (min) | Reaction temperature (. degree.C.) | Amount of precipitate | Amount of flue gas |
| 10 | 5 | 62 | Chinese character shao (a Chinese character of 'shao') | Small |
| 15 | 10 | 68 | Is rarely used | Small |
| 20 | 20 | 64 | Is less | Small |
According to the embodiment 3, the prepared alkali-free liquid accelerator is an experiment product 1, an experiment product 2, an experiment product 3, an experiment product 4, an experiment product 5 and an experiment product 6, the other conditions are the same, and the variation amounts are the adding amount of aluminum hydroxide and the adding amount of a fluorine aluminum complex; wherein:
experiment 1: 15% of aluminum hydroxide and 1.5% of fluorine aluminum complex;
experiment 2: 15% of aluminum hydroxide and 2.0% of fluorine aluminum complex;
experiment 3: 15% of aluminum hydroxide and 2.5% of fluorine aluminum complex;
experiment 4: the adding amount of the aluminum hydroxide is 20 percent, and the adding amount of the fluorine aluminum complex is 1.5 percent;
experiment 5: the adding amount of the aluminum hydroxide is 20 percent, and the adding amount of the fluorine aluminum complex is 2.0 percent;
experiment 6: the adding amount of the aluminum hydroxide is 20 percent, and the adding amount of the fluorine aluminum complex is 2.5 percent;
the experimental product 1, the experimental product 2, the experimental product 3, the experimental product 4, the experimental product 5, the experimental product 6 and two alkali-free liquid accelerating agent samples sold in the market at present are compared, 6% of the weight of cement is respectively added into a cement paste or a cement mortar sample, the setting time and the compressive strength are tested according to the standard of accelerating agent for sprayed concrete (GB/T35159-2017), the performance test results are shown in the following table 2, the cement used in the experiment is sea snail cement, the adding amount of aluminum hydroxide is based on the adding amount of hydrofluoric acid, and the adding amount of a fluorine aluminum complex is based on the mass of the accelerating agent.
As can be seen from Table 2, compared with two kinds of alkali-free liquid setting accelerators sold in the market, the alkali-free liquid setting accelerator provided by the invention has shorter setting time and higher compressive strength, the setting time of cement paste can meet the requirements that the initial setting time is less than 5min and the final setting time is less than 12min under the condition of 6% of doping amount, the 1d compressive strength of mortar is more than 10MPa, the 28d compressive strength ratio is more than 100%, and the alkali-free liquid setting accelerator has good adaptability to various kinds of cement, and can meet the construction requirements of sprayed concrete.
In the specific embodiment of the present invention, the 30% hydrofluoric acid used was diluted with commercially available 40% hydrofluoric acid, and the remaining raw materials were commercially available.
The above description is only for the specific embodiments of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art can easily conceive of the changes or substitutions within the technical scope of the present invention, and all the changes or substitutions should be covered within the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the claims.
Claims (10)
1. An alkali-free liquid accelerator prepared from a fluorine-aluminum complex is characterized in that raw materials comprise mother liquor, the fluorine-aluminum complex, alkaline silica sol and aluminum sulfate.
2. The alkali-free liquid accelerator prepared using a fluoroaluminium complex as claimed in claim 1, wherein the mother liquor comprises magnesium silicofluoride, ferrous sulfate, alcohol amine, urea and formic acid; the fluorine-aluminum complex consists of hydrofluoric acid and aluminum hydroxide; the alkaline silica sol is a colloidal solution of silicon dioxide.
3. The alkali-free liquid accelerator prepared from the fluorine aluminum complex according to claim 1, which comprises the following raw materials in percentage by mass: 25.0-35.0% of mother liquor; 1.5-2.5% of a fluorine-aluminum complex; 3.0-3.5% of alkaline silica sol; 40.0-50.0% of aluminum sulfate; the balance being water.
4. The alkali-free liquid accelerator prepared from the fluorine aluminum complex according to any one of claims 1 to 3, wherein the mother liquor comprises the following raw materials in percentage by mass: 20.0 percent of magnesium fluosilicate; 12.0 percent of ferrous sulfate; 8.0 percent of alcohol amine; 4.0 percent of urea; 3.0 percent of formic acid and the balance of water.
5. The alkali-free liquid accelerator prepared from a fluorine aluminum complex according to claim 2 or 4, wherein the alcohol amine is one or a mixture of two of diethanolamine and triethanolamine.
6. The alkali-free liquid accelerator prepared from the fluoroaluminium complex as claimed in claim 1, wherein the alkali silica sol has a silica particle size of 8 to 15nm and a solid content of 30 to 31%.
7. The alkali-free liquid accelerator prepared from a fluoroaluminium complex according to any one of claims 1 to 4, wherein the mother liquor is prepared by: under the conditions of normal temperature and normal pressure, adding formic acid into water for dissolving and stirring for 3-5 min, adding magnesium fluosilicate, stirring for 15-30 min until the formic acid is completely dissolved, adding urea, stirring for 3-5 min until the formic acid is completely dissolved, continuing adding alcohol amine, stirring for 10min, finally adding ferrous sulfate, and stirring until the formic acid is completely dissolved to obtain mother liquor.
8. The alkali-free liquid accelerator prepared from a fluoroaluminium complex according to any one of claims 1 to 3, wherein the fluoroaluminium complex is prepared by: dropwise adding the aluminum hydroxide powder into a hydrofluoric acid solution with the mass percentage concentration of 30% step by step in a gradient manner, and stirring while adding until the aluminum hydroxide powder is completely dissolved to obtain the fluorine aluminum complex.
9. The method for producing a fluoroaluminium complex according to claim 8, wherein the mass of the aluminum hydroxide is 10.0% to 20.0% of the mass of the hydrofluoric acid; the dropping gradient of the aluminum hydroxide powder is 3.0-5.0% of the mass of hydrofluoric acid based on the mass of the hydrofluoric acid.
10. The alkali-free liquid accelerator prepared by using the fluorine aluminum complex according to any one of claims 1 to 9, wherein the preparation method of the alkali-free liquid accelerator comprises the steps of:
and adding the mother liquor into water, stirring until the mother liquor is uniformly mixed, adding the fluorine-aluminum complex, stirring for 15-20 min, adding the alkaline silica sol, stirring for 5-10 min, and finally adding the aluminum sulfate, stirring until the aluminum sulfate is completely dissolved to obtain the alkali-free liquid accelerator.
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| 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 |
| CN115073209A (en) * | 2022-07-21 | 2022-09-20 | 广州市克来斯特建材科技有限公司 | Scabbling agent and preparation method and application thereof |
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| CN113213877A (en) * | 2021-06-03 | 2021-08-06 | 厦门美益建材有限公司 | Low-temperature cement and preparation method 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 |
| CN115073209A (en) * | 2022-07-21 | 2022-09-20 | 广州市克来斯特建材科技有限公司 | Scabbling agent and preparation method and application thereof |
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