CN114105513A - Alkali-free accelerator and preparation method and application thereof - Google Patents
Alkali-free accelerator and preparation method and application thereof Download PDFInfo
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- CN114105513A CN114105513A CN202111388798.8A CN202111388798A CN114105513A CN 114105513 A CN114105513 A CN 114105513A CN 202111388798 A CN202111388798 A CN 202111388798A CN 114105513 A CN114105513 A CN 114105513A
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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
- C04B22/00—Use of inorganic materials as active ingredients for mortars, concrete or artificial stone, e.g. accelerators, shrinkage compensating agents
- C04B22/0006—Waste inorganic materials
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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
- C04B26/00—Compositions of mortars, concrete or artificial stone, containing only organic binders, e.g. polymer or resin concrete
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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
- C04B28/00—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements
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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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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/91—Use of waste materials as fillers for mortars or concrete
Abstract
The invention discloses an alkali-free accelerator, a preparation method and application thereof. The alkali-free accelerator is mainly prepared from a solution A, a solution B and a solution C according to the mass ratio of 1:1:0.005-0.02, wherein the solution A and the solution B divide a modified aluminum ash solution into two systems for reaction, and can inhibit Al3+Hydrolysis to Al (OH)3Precipitating to improve stability of alkali-free accelerator, and dispersing the solution C as polymer surface dispersant with good dispersing effectStability problems of alkali accelerators.
Description
Technical Field
The invention relates to the field of concrete admixtures, in particular to an alkali-free accelerator, a preparation method and application thereof, and especially relates to an alkali-free accelerator prepared from waste liquor and aluminum ash of a phosphoric acid plant, a preparation method and application thereof.
Background
The accelerator has been used as an indispensable additive in sprayed concrete for many years, has the function of accelerating the hydration hardening of cement, forms enough strength in a short time to meet the requirements of special construction, and is widely applied to projects such as tunnels, electric power pipelines, water conservancy culverts and the like. The alkali-free accelerator has the advantages of high strength retention rate, good durability, no corrosiveness and the like, so that the research is hot, but the alkali-free accelerator is still in the research stage at present, and the application of the alkali-free accelerator has various problems to be solved, such as large doping amount, high price, insufficient stability, poor adaptability to cement admixture and the like.
Phosphoric acid plants mainly produce phosphoric acid, sulfuric acid, ammonium phosphate, phosphate fertilizer, byproducts of aluminum fluoride, fluosilicic acid and the like, the phosphoric acid plants can generate a large amount of waste liquid in the production and operation processes, the pH of the untreated waste liquid is 2-3, the fluoride content can reach 400-2000mg/L, and the discharge of the waste liquid can cause water source pollution and ecological damage. The existing methods for purifying the waste liquid of the phosphoric acid plant comprise a chemical precipitation method, a coagulating precipitation method, an adsorption method and the like, and have complex process and high cost. Fluoride, sulfuric acid and hydrochloric acid contained in the phosphoric acid plant waste liquid are all required raw materials of the alkali-free accelerator, and the components are used for synthesizing the accelerator, so that waste recycling can be realized, and circular economy, energy conservation and emission reduction can be realized.
The secondary aluminum ash is one of the main byproducts in the industrial production of secondary aluminum, has very uneven components, mainly comprises aluminum oxide and simple substance aluminum, and the other components comprise magnesium, calcium, sodium and potassium metal chlorides and iron, silicon and magnesium oxides. Statistically, every 1t of aluminum is produced, 25-30kg of secondary aluminum ash is produced. At present, the secondary aluminum ash treatment is mainly performed by accumulation, the accumulation of the aluminum ash is not only a great waste of aluminum resources, but also heavy metal salts in the aluminum ash and the like can cause serious pollution to surrounding atmosphere, soil and underground water. Therefore, the efficient recycling of aluminum resources can be realized by further utilizing the aluminum and the compounds thereof in the secondary aluminum ash, and the method has important significance for the sustainable development of the society.
At present, the stability of the alkali-free setting accelerator is poor, the precipitation and delamination appear in the product, the industrial development of the alkali-free setting accelerator is severely limited, the problem is urgently solved in the whole industry, the stability of the alkali-free setting accelerator is mostly solved by introducing organic acid, an anti-settling agent, a suspending agent and the like at present, but the stabilizing effect is urgently required to be improved.
Disclosure of Invention
The invention aims to solve the technical problem of providing an alkali-free accelerator prepared from waste liquid and waste residues and a preparation method thereof.
The technical scheme adopted by the invention for solving the technical problems is as follows:
an alkali-free accelerator is mainly prepared from a solution A, a solution B and a solution C according to the mass ratio of 1:1:0.005-0.02, wherein the solution A comprises 40-65% of modified aluminum ash solution, 3-9% of fluoride and 20-40% of phosphoric acid plant waste liquid by mass percent; the solution B comprises 32-50% of phosphoric acid plant waste liquid, 35-50% of modified aluminum ash liquid and 10-18% of aluminum hydroxide; the solution C comprises 2-10% of methacrylic acid, 2-15% of sodium acrylate, 1-5% of glycerol, 0.1-0.8% of sodium dodecyl benzene sulfonate, 0.1-1% of fatty alcohol-polyoxyethylene ether, 0.001-0.02% of ferrous sulfate, 0.02-0.5% of hydrogen peroxide (10-15 vol.% of hydrogen peroxide solution), 0.05-1% of sodium hypophosphite and 70-86% of deionized water; the modified aluminum ash liquid comprises aluminum sulfate and magnesium sulfate, wherein the content of the aluminum sulfate is more than or equal to 52 percent, and the content of the magnesium sulfate is 14-16 percent; the phosphoric acid plant waste liquid comprises fluosilicic acid, aluminum fluoride, sulfuric acid and hydrochloric acid, wherein the content of the fluosilicic acid is more than or equal to 16.5 percent, the content of the aluminum fluoride is more than or equal to 6 percent, the content of the sulfuric acid is not more than 3.5 percent, and the content of the hydrochloric acid is not more than 2 percent.
Further, the preparation method of the modified aluminum ash solution comprises the following steps:
adding the secondary aluminum ash and water into a reaction kettle, mixing and stirring to obtain an aluminum ash mixed solution with the solid content of 60%, and then dropwise adding concentrated sulfuric acid with the mass of 10% of the aluminum ash into the mixed solutionAnd after the dripping is finished within 1h, continuing to react until the temperature is reduced to the room temperature, and filtering residues to obtain the modified aluminum ash solution. The aluminum ash is the surplus aluminum ash after secondary aluminum ash treatment, wherein the simple substance Al content is 33.8 percent, and the aluminum oxide Al is2O317.4% of Si, 7.1% of MgAl2O4The content of the other components is 15.3 percent, and the other components are magnesium, calcium, sodium and potassium metal chlorides and iron, silicon and magnesium oxides.
Further, the fluoride is sodium fluoride and potassium fluoride.
The preparation method of the alkali-free accelerator comprises the following steps:
(1) adding the modified aluminum ash solution, fluoride, phosphoric acid plant waste liquid and deionized water into a reaction kettle, heating to 90 ℃, reacting for 1-2h, and cooling to room temperature to obtain a solution A;
(2) putting the phosphoric acid plant waste liquid, the modified aluminum ash liquid and the aluminum hydroxide into a reaction kettle, heating to 80 ℃, stirring for reaction for 1.5-3h, and cooling to room temperature to obtain a solution B;
(3) adding methacrylic acid, sodium acrylate, glycerol, sodium dodecyl sulfate, fatty alcohol-polyoxyethylene ether, ferrous sulfate, hydrogen peroxide, sodium hypophosphite and deionized water into a reaction kettle, stirring for 10min, stopping stirring, and standing for reaction for 1.5h to obtain a solution C;
(4) and preparing the solution A, the solution B and the solution C according to the mass ratio to obtain the alkali-free accelerator.
Further, the modified aluminum ash solution is prepared by the following method:
and (3) putting the secondary aluminum ash and water into a reaction kettle, mixing and stirring to obtain a 60% solid-contained aluminum ash mixed solution, then dropwise adding concentrated sulfuric acid with the mass of 10% of the aluminum ash into the mixed solution, continuing to react until the temperature is reduced to room temperature within 1h, and filtering residues to obtain the modified aluminum ash solution.
The application of the alkali-free accelerator is characterized in that the mixing amount of the accelerator is 5-8% of the cementing material in actual use.
Further, the solution A, the solution B and the solution C are separately stored and mixed uniformly according to the mass ratio before use.
The invention has the beneficial effects that:
1. the alkali-free accelerator prepared from the waste liquid and the waste residues is prepared by using the waste liquid and the modified secondary aluminum ash liquid of a phosphoric acid production workshop of a phosphate factory as raw materials for synthesizing the alkali-free accelerator, the phosphoric acid, the sulfuric acid, the fluosilicic acid and the aluminum fluoride in the waste liquid are reasonably utilized, and 90% of aluminum oxide and aluminum simple substances in the secondary aluminum ash are converted into aluminum sulfate through water and concentrated sulfuric acid treatment, so that the purposes of recycling waste, recycling economy, energy conservation and emission reduction are realized, and the raw material cost of the alkali-free accelerator is greatly reduced.
2. The alkali-free accelerator prepared from the waste liquid and the waste residues consists of a liquid A, a liquid B and a liquid C, wherein the liquid A and the liquid B divide a modified aluminum ash liquid into two systems for reaction, so that Al can be inhibited3+Hydrolysis to Al (OH)3And the solution C is used as a polymer surface dispersant, has a good dispersing effect and can solve the stability problem of the alkali-free setting accelerator. The liquid A, the liquid B and the liquid C are stored independently as much as possible after production, and are mixed uniformly according to a proportion before use, and can be directly mixed and delivered from a factory if the quality guarantee period does not have special requirements. The mixing amount of the accelerator is 5-8% of that of the cementing material in actual use, and the accelerator can realize good accelerating effect under the condition of low mixing amount, and the later strength is hardly lost.
Detailed Description
The present invention is further illustrated by the following specific examples.
Example 1
The alkali-free accelerator prepared from waste liquid and waste residues comprises the following steps:
(1) adding 600g of secondary aluminum ash and 400g of water into a reaction kettle, mixing and stirring to obtain a 60% solid aluminum ash mixed solution, then dropwise adding 60g of concentrated sulfuric acid into the mixed solution, continuing to react until the temperature is reduced to room temperature within 1h, and filtering residues to obtain a modified aluminum ash solution.
(2) And (3) putting 40% of the modified aluminum ash solution, 3% of sodium fluoride and 40% of phosphoric acid plant waste liquid into a reaction kettle, heating to 90 ℃, reacting for 1h, and cooling to room temperature to obtain a solution A. 32% of phosphoric acid plant waste liquid, 50% of modified aluminum ash liquid and 18% of aluminum hydroxide are put into a reaction kettle, the temperature is increased to 80 ℃, the stirring reaction is carried out for 1.5h, and the temperature is reduced to room temperature to obtain solution B. Putting 2% of methacrylic acid, 15% of sodium acrylate, 1% of glycerol, 0.1% of sodium dodecyl sulfate, 1% of fatty alcohol-polyoxyethylene ether, 0.001% of ferrous sulfate, 0.02% of hydrogen peroxide, 0.05% of sodium hypophosphite and 80% of deionized water into a reaction kettle, stirring for 10min, stopping stirring, and standing for reaction for 1.5h to obtain a solution C. And uniformly mixing the solution A, the solution B and the solution C according to the mass ratio of 1:1:0.01 to obtain the alkali-free accelerator.
Example 2
The alkali-free accelerator prepared by using the waste liquid of the phosphoric acid plant comprises the following steps:
65% of the modified aluminum ash solution, 9% of sodium fluoride and 20% of phosphoric acid plant waste liquid which are described in the embodiment 1 are put into a reaction kettle, the temperature is increased to 90 ℃, the reaction is carried out for 1.5h, and the temperature is reduced to the room temperature, so that a solution A is obtained. 50% of phosphoric acid plant waste liquid, 35% of modified aluminum ash liquid and 10% of aluminum hydroxide are put into a reaction kettle, the temperature is increased to 80 ℃, the stirring reaction is carried out for 1.5h, and the temperature is reduced to room temperature to obtain solution B. Putting 2% of methacrylic acid, 10% of sodium acrylate, 3% of glycerol, 0.5% of sodium dodecyl sulfate, 0.5% of fatty alcohol-polyoxyethylene ether, 0.02% of ferrous sulfate, 0.5% of hydrogen peroxide, 1% of sodium hypophosphite and 82% of deionized water into a reaction kettle, stirring for 10min, stopping stirring, and standing for reacting for 1.5h to obtain a solution C. And uniformly mixing the solution A, the solution B and the solution C according to the mass ratio of 1:1:0.01 to obtain the alkali-free accelerator.
Example 3
The alkali-free accelerator prepared by using the waste liquid of the phosphoric acid plant comprises the following steps:
50% of the modified aluminum ash solution, 5% of sodium fluoride and 30% of phosphoric acid plant waste liquid which are described in the embodiment 1 are put into a reaction kettle, heated to 90 ℃ for reaction for 1.5h, and cooled to room temperature to obtain a solution A. And (3) putting 40% of the phosphoric acid plant waste liquid, 40% of the modified aluminum ash liquid and 14% of aluminum hydroxide into a reaction kettle, heating to 80 ℃, stirring for reaction for 1.5h, and cooling to room temperature to obtain a solution B. Adding 6% of methacrylic acid, 12% of sodium acrylate, 2% of glycerol, 0.3% of sodium dodecyl sulfate, 0.8% of fatty alcohol-polyoxyethylene ether, 0.01% of ferrous sulfate, 0.2% of hydrogen peroxide, 0.6% of sodium hypophosphite and 78% of deionized water into a reaction kettle, stirring for 10min, stopping stirring, and standing for reaction for 1.5h to obtain a solution C. And uniformly mixing the solution A, the solution B and the solution C according to the mass ratio of 1:1:0.02 to obtain the alkali-free accelerator.
Comparative example 1
On the basis of example 1, only step (1), i.e., synthesis of solution a, was completed.
Comparative example 2
On the basis of example 1, only step (2), i.e., synthesis of solution B, was completed.
Comparative example 3
And (3) completing the steps (1) and (2) on the basis of the embodiment 1, and uniformly mixing the solution A and the solution B according to the mass ratio of 1:1 to obtain the alkali-free accelerator.
The performance detection of the alkali-free accelerator is in accordance with the standard of GBT 35159 and 2017 accelerator for sprayed concrete.
Table 1 shows the performance data of the alkali-free accelerators of examples 1-3 and comparative examples 1-3, and Table 2 shows the stability data of the alkali-free accelerators of examples 1-3 and comparative examples 1-3.
Table 1: performance comparison data of alkali-free accelerator
Note: the cement for detection is P.O 42.5.5 Dong Jun cement, and the mixing amount of the accelerator is 5%.
As can be seen from the data in Table 1, the alkali-free accelerator prepared from the waste liquid and the waste residues can effectively shorten the cement setting time and meet the requirement on the strength of sprayed concrete. The liquid A and liquid B alone have a lower quick-setting effect than the mixed liquid.
TABLE 2 stability control of alkali-free accelerators
| Sample (I) | Standing for 1d | Standing for 7d | Standing for 1 month | Standing for 3 months |
| Example 1 | Clarification | Clarification | Clarification | Clarification |
| Comparative example 1 | Clarification | Clarification | Clarification | Clarification |
| Comparative example 2 | Clarification | Clarification | Clarification | Clarification |
| Comparative example 3 | Clarification | Clarification | The appearance of micro suspended particles | A large amount of suspended particles appear |
As can be seen from the data in Table 2, the alkali-free accelerator prepared from the waste liquid and the waste residues has better stability, and the mixed liquid of the liquid A and the liquid B can effectively shorten the cement setting time, but has poor stability. The mixed liquid of the liquid A, the liquid B and the liquid C can shorten the cement setting time and ensure the stability.
It is to be noted that ". gtoreq.or" > "of the components mentioned in the present invention does not include 100%, and likewise, 0 is not included in the". gtoreq.or "<".
Claims (6)
1. An alkali-free accelerator is characterized by being mainly prepared from a solution A, a solution B and a solution C according to a mass ratio of 1:1: 0.005-0.02; calculated by mass percent, the solution A comprises 40-65% of modified aluminum ash solution, 3-9% of fluoride and 20-40% of phosphoric acid plant waste liquid; the solution B comprises 32-50% of phosphoric acid plant waste liquid, 35-50% of modified aluminum ash liquid and 10-18% of aluminum hydroxide; the solution C comprises 2-10% of methacrylic acid, 2-15% of sodium acrylate, 1-5% of glycerol, 0.1-0.8% of sodium dodecyl benzene sulfonate, 0.1-1% of fatty alcohol-polyoxyethylene ether, 0.001-0.02% of ferrous sulfate, 0.02-0.5% of hydrogen peroxide, 0.05-1% of sodium hypophosphite and 70-86% of deionized water; the modified aluminum ash liquid comprises aluminum sulfate and magnesium sulfate, wherein the content of the aluminum sulfate is more than or equal to 52 percent, and the content of the magnesium sulfate is 14-16 percent; the phosphoric acid plant waste liquid comprises fluosilicic acid, aluminum fluoride, sulfuric acid and hydrochloric acid, wherein the content of the fluosilicic acid is more than or equal to 16.5 percent, the content of the aluminum fluoride is more than or equal to 6 percent, the content of the sulfuric acid is less than or equal to 3.5 percent, and the content of the hydrochloric acid is less than or equal to 2 percent.
2. The alkali-free accelerator according to claim 1, wherein the fluoride is sodium fluoride or potassium fluoride.
3. A method for preparing an alkali-free accelerator as set forth in claim 1 or 2, comprising the steps of:
(1) adding the modified aluminum ash solution, fluoride, phosphoric acid plant waste liquid and deionized water into a reaction kettle, heating to 90 ℃, reacting for 1-2h, and cooling to room temperature to obtain a solution A;
(2) putting the phosphoric acid plant waste liquid, the modified aluminum ash liquid and the aluminum hydroxide into a reaction kettle, heating to 80 ℃, stirring for reaction for 1.5-3h, and cooling to room temperature to obtain a solution B;
(3) adding methacrylic acid, sodium acrylate, glycerol, sodium dodecyl sulfate, fatty alcohol-polyoxyethylene ether, ferrous sulfate, hydrogen peroxide, sodium hypophosphite and deionized water into a reaction kettle, stirring for 10min, stopping stirring, and standing for reaction for 1.5h to obtain a solution C;
(4) and preparing the solution A, the solution B and the solution C according to the mass ratio to obtain the alkali-free accelerator.
4. The preparation method according to claim 3, wherein the modified aluminum ash solution is prepared by the following method:
and (3) putting the secondary aluminum ash and water into a reaction kettle, mixing and stirring to obtain a 60% solid-contained aluminum ash mixed solution, then dropwise adding concentrated sulfuric acid with the mass of 10% of the aluminum ash into the mixed solution, continuing to react until the temperature is reduced to room temperature within 1h, and filtering residues to obtain the modified aluminum ash solution.
5. The use of an alkali-free accelerator as claimed in claim 1 or 2, wherein the accelerator is used in an amount of 5-8% of the cementitious material.
6. The use of claim 5, wherein the solution A, the solution B and the solution C are stored separately and mixed in the mass ratio before use.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115572099A (en) * | 2022-10-25 | 2023-01-06 | 中铁十一局集团有限公司 | Normal-temperature preparation method of alkali-free liquid accelerator for quick-hardening early-strength sprayed concrete |
| CN115611545A (en) * | 2022-08-22 | 2023-01-17 | 贵州天威建材科技有限责任公司 | Method for preparing dry powder accelerator from fluorine and silicon residues |
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