CN110627524A - Preparation method of light high-strength water-resistant phosphogypsum slurry - Google Patents
Preparation method of light high-strength water-resistant phosphogypsum slurry Download PDFInfo
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- CN110627524A CN110627524A CN201911024642.4A CN201911024642A CN110627524A CN 110627524 A CN110627524 A CN 110627524A CN 201911024642 A CN201911024642 A CN 201911024642A CN 110627524 A CN110627524 A CN 110627524A
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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
- C04B28/14—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 containing calcium sulfate cements
- C04B28/142—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 containing calcium sulfate cements containing synthetic or waste calcium sulfate cements
- C04B28/143—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 containing calcium sulfate cements containing synthetic or waste calcium sulfate cements the synthetic calcium sulfate being phosphogypsum
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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
- C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
- C04B2111/40—Porous or lightweight materials
-
- 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
- C04B2201/00—Mortars, concrete or artificial stone characterised by specific physical values
- C04B2201/50—Mortars, concrete or artificial stone characterised by specific physical values for the mechanical strength
Abstract
The invention discloses a preparation method of light high-strength water-resistant phosphogypsum slurry, which comprises the steps of firstly, taking phosphorus semi-hydrated gypsum and a water reducing agent, and wet-grinding the phosphorus semi-hydrated gypsum and the water reducing agent to prepare slurry; adding a lauric acid/oleic acid mixed solution into the slurry, continuously wet-grinding, and freeze-drying to obtain modified nano phosphogypsum powder; mixing alumina sol and polyvinyl alcohol solution, adding oxidant, stirring under heating condition, freeze drying to obtain nanometer alumina aerogel, and ball milling to obtain nanometer alumina aerogel powder; and finally, mixing and stirring the phosphorus semi-hydrated gypsum powder, the modified nano phosphogypsum powder, the fumed silica, the nano alumina aerogel powder and the gypsum excitant to obtain the light high-strength water-resistant phosphogypsum slurry. The invention solves the defects of poor water resistance and low crack resistance of gypsum, improves the performance of the phosphorus semi-hydrated gypsum, solves the problems of land occupation, environmental pollution and resource waste caused by stacking solid wastes, makes the best use of the matters and has higher economic benefit and environmental benefit.
Description
Technical Field
The invention relates to the technical field of building materials, in particular to a preparation method of light high-strength water-resistant phosphogypsum slurry.
Background
Phosphogypsum is a solid waste in phosphate fertilizer industry, generally, 5-6 tons of phosphogypsum are generated every 1 ton of phosphoric acid, and 2.5-5 tons of phosphogypsum are discharged every 1 ton of diammonium phosphate. At present, the comprehensive utilization rate of the phosphogypsum is low both abroad and domestically, and the phosphogypsum is mainly treated by adopting a stockpiling mode. The accumulated discharge amount of the phosphogypsum in China is nearly hundred million tons, the discharge amount of the phosphogypsum is the largest one in gypsum waste residues, and the discharged phosphogypsum residues occupy a large amount of land to form a residue hill and seriously pollute the environment. Besides a very small amount of phosphogypsum is utilized to produce building materials, a large amount of solid waste residues occupy a large area of land, and harmful heavy metal chemical substances such as arsenic, cadmium, mercury and the like contained in the phosphogypsum have hundreds of years of influence on the environment. Phosphorus enters the water body, and the eutrophication is more serious than nitrogen. When the content of phosphorus exceeds the standard, blue algae in the water body can burst to generate eutrophication. And its fluorine content is relatively high and leakage of fluorine occurs.
As the phosphogypsum contains a small amount of soluble substances, compared with natural gypsum used as a cement retarder in the application of cement, the phosphogypsum has the defects of low strength, slow setting time and the like generally, the principle is that the water-soluble substances in the phosphogypsum and the phosphogypsum are dissolved together and enter into cement slurry, the cement slurry has strong alkalinity, impurities such as phosphate, fluoride and the like are neutralized, insoluble calcium phosphate and calcium fluoride are generated and deposited on the surface of cement particles, the penetration of moisture is hindered, and the hydration speed of the cement is delayed.
Theoretically, the phosphogypsum can replace natural gypsum after being treated, has extremely wide application range and is mainly used in the following fields:
firstly, ardealite is used as a cement retarder;
secondly, the phosphogypsum is used as a novel building material;
utilizing phosphogypsum to prepare sulfuric acid and co-produce cement;
fourthly, the phosphogypsum is used for mine filling;
fifthly, the phosphogypsum is used for foundation reinforcement.
However, the phosphogypsum contains trace phosphorus, fluorine and other impurities, and the common diseases of gypsum are as follows: the water resistance and the crack resistance are insufficient, the comprehensive utilization of the phosphogypsum is restricted, and the comprehensive utilization of the phosphogypsum can be popularized only after the phosphogypsum is modified. Therefore, the modification treatment of the phosphogypsum is the key of the comprehensive utilization of the phosphogypsum.
The method for modifying the phosphogypsum at home and abroad is multiple, and the common practice is to wash the phosphogypsum and add a proper amount of quicklime in the washing process to solidify the soluble impurities such as phosphorus, fluorine and the like in the phosphogypsum into insoluble substances.
Related patents for water-resistant modification of gypsum that have been published in recent years:
the invention discloses a water-resistant self-cleaning heat-preservation building gypsum powder and a preparation method thereof, wherein the application number of the invention is 201610184209.7; the phosphogypsum is creatively baked, crushed and blown to a boiling state, and sprayed with a mist hydrochloric acid solution; in the method, hydrogen is released due to the reaction, so that the building structure has certain uncontrollable property.
The chinese invention patent with application number 201080058369.8 discloses a method for manufacturing a water-resistant gypsum article; the method sonicates a water resistance additive in water to form an emulsion; combining the emulsion, the calcined gypsum, and gauging water to form a slurry; and shaping and setting the slurry to form the water-resistant gypsum article. The method has high requirements on the emulsion of the additive and has great dependence on the interaction between the emulsion and the gypsum.
The invention patent of China with application number 201110306025.0 discloses a waterproof caulking gypsum powder and a preparation method thereof, wherein the waterproof caulking gypsum powder comprises the following components in percentage by weight: 7500-8500 parts of beta gypsum, 1500-2500 parts of limestone, 1-10 parts of retarder, 100-200 parts of cellulose and 20-80 parts of organic silicon powder; in the method, beta gypsum and limestone are prepared into fine powder with the granularity less than or equal to 200 mu m; and adding the prepared fine powder and other components into a mixer in proportion, mixing for 5-10 min, and uniformly mixing. The method has high requirement on organic silicon powder, and has great dependence on the interaction with gypsum.
Disclosure of Invention
The invention aims to solve the problems of the impurities of the existing phosphogypsum and the common diseases of gypsum: the problems of poor water resistance, insufficient crack resistance and the like are solved, and the preparation method of the light high-strength water-resistant phosphogypsum slurry is provided; the method utilizes the industrial waste phosphogypsum as a base material, and enhances the water resistance of the phosphogypsum through modification, and compared with the traditional treatment method, the treatment method has the advantages of high efficiency and remarkable effect; in addition, the method gives full play to the potential value of the industrial waste phosphogypsum, saves chemical raw materials, provides a new utilization approach for the comprehensive utilization of the phosphogypsum, and has great economic and environmental benefits.
In order to achieve the purpose, the invention designs a preparation method of light high-strength water-resistant phosphogypsum slurry, which comprises the following steps:
step 1: taking 100 parts by weight of phosphorus semi-hydrated gypsum and 0.2-0.6 part by weight of a water reducing agent (admixture), and wet-grinding the phosphorus semi-hydrated gypsum and the water reducing agent for 2-4 hours according to the water-solid ratio of water to the phosphorus semi-hydrated gypsum of 1.0; preparing into slurry;
step 2: adding 8-16 parts by weight of lauric acid/oleic acid mixed solution into 100 parts by weight of slurry, continuously wet-grinding for 1-2 hours, standing, and freeze-drying to obtain modified nano phosphogypsum powder;
and step 3: mixing 100 parts by weight of alumina sol and 10-20 parts by weight of polyvinyl alcohol solution, adding 6-8 parts by weight of oxidant, continuously stirring under heating conditions, freezing and molding at low temperature, preparing nano alumina aerogel by freeze drying, and performing ball milling to obtain nano alumina aerogel powder;
and 4, step 4: mixing and stirring 100-150 parts by weight of phosphorus semi-hydrated gypsum powder, 2-6 parts by weight of modified nano phosphogypsum powder, 6-8 parts by weight of fumed silica, 10-16 parts by weight of nano alumina aerogel powder, 4-6 parts by weight of gypsum excitant and 70-110 parts of water to obtain the light high-strength water-resistant phosphogypsum slurry.
Further, in the step 1), the water reducing agent is any one of a polycarboxylic acid-based high-performance water reducing agent, an HSB aliphatic high-efficiency water reducing agent and a naphthalene-based high-efficiency water reducing agent.
Furthermore, in the step 1), the slurry is an aqueous dispersion of phosphogypsum, and the average solid particle size of the slurry is 300-500 nm.
Still further, in the step 2), the weight ratio of lauric acid to oleic acid is 1: 1-1: 3.
Still further, in the step 3), the mass fraction of the polyvinyl alcohol solution is 0.5% -3%.
Still further, in the step 3), the oxidizing agent is any one of potassium persulfate, butyraldehyde, glyoxal and boric acid.
Further, in the step 3), the heating temperature is 40-60 ℃.
Still further, in the step 3), the freezing forming temperature is-60 to-30 ℃.
Furthermore, in the step 3), the average particle size of the nano alumina aerogel powder is 400-600 nm.
The invention has the beneficial effects that:
1) the invention solves the defects of poor water resistance and low crack resistance of gypsum, improves the performance of the phosphorus semi-hydrated gypsum, solves the problems of land occupation, environmental pollution and resource waste caused by stacking solid wastes, realizes the best use of the matters and has higher economic benefit and environmental benefit.
2) The nano effect is well utilized, so that the strength of the prepared gypsum slurry is obviously improved, the water resistance is also improved to a certain degree, and the softening coefficients of all cases in the implementation are more than 0.7
3) The material prepared by the invention has adjustable performance, stable structure and simple operation.
Detailed Description
The present invention is described in further detail below with reference to specific examples so as to be understood by those skilled in the art.
Example 1
The preparation method of the light high-strength water-resistant phosphogypsum slurry 1 comprises the following steps:
step 1: taking 100 parts by weight of phosphorus semi-hydrated gypsum and 0.2 part by weight of polycarboxylic acid high-performance water reducing agent, and wet-grinding the phosphorus semi-hydrated gypsum and the water reducing agent for 2-4 hours according to the water-solid ratio of water to the phosphorus semi-hydrated gypsum of 1.0; preparing into slurry; wherein the slurry is water dispersion of phosphogypsum, and the average solid particle size is 500 nm;
step 2: adding 10 parts by weight of lauric acid/oleic acid mixed solution into 100 parts by weight of slurry, continuously wet-milling for 1-2 hours, standing, and freeze-drying to obtain modified nano phosphogypsum powder; the weight ratio of lauric acid to oleic acid was 1: 1.
And step 3: mixing 100 parts by weight of alumina sol and 10 parts by weight of polyvinyl alcohol solution (the mass fraction is 0.5% -3%), adding 6 parts by weight of potassium sulfate, continuously stirring at the temperature of 40-60 ℃, freezing and forming at the temperature of-60-30 ℃, preparing nano alumina aerogel through freeze drying, and obtaining nano alumina aerogel powder with the average particle size of 600nm through ball milling;
and 4, step 4: mixing and stirring 100-150 parts by weight of phosphorus semi-hydrated gypsum powder, 2 parts by weight of modified nano phosphogypsum powder, 6 parts by weight of fumed silica, 10 parts by weight of nano alumina aerogel powder, 4 parts by weight of gypsum excitant and 70 parts by weight of water to obtain the light high-strength water-resistant phosphogypsum slurry 1.
Example 2
The preparation method of the light high-strength water-resistant phosphogypsum slurry 2 comprises the following steps:
step 1: taking 100 parts by weight of phosphorus semi-hydrated gypsum and 0.6 part by weight of HSB aliphatic high-efficiency water reducing agent, and wet-grinding the phosphorus semi-hydrated gypsum and the water reducing agent for 2-4 hours according to the water-solid ratio of water to the phosphorus semi-hydrated gypsum of 1.0; preparing into slurry; the slurry is an aqueous dispersion of phosphogypsum, the average particle size of the solid of which is 300 nm.
Step 2: adding 16 parts by weight of lauric acid/oleic acid mixed solution into 100 parts by weight of slurry, continuously wet-milling for 1-2 hours, standing, and freeze-drying to obtain modified nano phosphogypsum powder; the weight ratio of lauric acid to oleic acid was 1: 3.
And step 3: mixing 100 parts by weight of alumina sol and 20 parts by weight of polyvinyl alcohol solution (the mass fraction is 3%), adding 8 parts by weight of butyraldehyde, continuously stirring at the temperature of 40-60 ℃, freezing and molding at the temperature of-60-30 ℃, preparing nano alumina aerogel through freeze drying, and obtaining nano alumina aerogel powder with the average particle size of 400 through ball milling;
and 4, step 4: mixing and stirring 150 parts by weight of phosphorus hemihydrate gypsum powder, 6 parts by weight of modified nano phosphogypsum powder, 8 parts by weight of fumed silica, 16 parts by weight of nano alumina aerogel powder, 6 parts by weight of gypsum excitant and 110 parts by weight of water to obtain the light high-strength water-resistant phosphogypsum slurry 2.
Example 3
The preparation method of the light high-strength water-resistant phosphogypsum slurry 3 comprises the following steps:
step 1: taking 100 parts by weight of phosphorus semi-hydrated gypsum and 0.4 part by weight of naphthalene-based high-efficiency water reducing agent (admixture), and wet-grinding the phosphorus semi-hydrated gypsum and the water reducing agent for 2-4 hours according to the water-solid ratio of water to the phosphorus semi-hydrated gypsum of 1.0; preparing into slurry; the slurry is water dispersion of phosphogypsum, and the average solid particle size of the slurry is 300-500 nm.
Step 2: adding 12 parts by weight of lauric acid/oleic acid mixed solution into 100 parts by weight of slurry, continuously wet-milling for 1-2 hours, standing, and freeze-drying to obtain modified nano phosphogypsum powder; the weight ratio of lauric acid to oleic acid was 1: 2.
And step 3: mixing 100 parts by weight of alumina sol and 15 parts by weight of polyvinyl alcohol solution (the mass fraction is 1.75%), adding 7 parts by weight of glyoxal, continuously stirring at the temperature of 40-60 ℃, freezing and forming at the temperature of-60-30 ℃, preparing nano alumina aerogel through freeze drying, and obtaining nano alumina aerogel powder with the average particle size of 500nm through ball milling;
and 4, step 4: 125 parts by weight of phosphorus hemihydrate gypsum powder, 4 parts by weight of modified nano phosphogypsum powder, 7 parts by weight of fumed silica, 13 parts by weight of nano alumina aerogel powder, 5 parts by weight of gypsum excitant and 90 parts by weight of water are mixed and stirred to obtain the light high-strength water-resistant phosphogypsum slurry 3.
Example 4
The preparation method of the light high-strength water-resistant phosphogypsum slurry 4 comprises the following steps:
step 1: taking 100 parts by weight of phosphorus semi-hydrated gypsum and 0.6 part by weight of polycarboxylic acid high-performance water reducing agent, and wet-grinding the phosphorus semi-hydrated gypsum and the water reducing agent for 2-4 hours according to the water-solid ratio of water to the phosphorus semi-hydrated gypsum of 1.0; preparing into slurry; the slurry is an aqueous dispersion of phosphogypsum, the average particle size of the solid of which is 300 nm.
Step 2: adding 12 parts by weight of lauric acid/oleic acid mixed solution into 100 parts by weight of slurry, continuously wet-milling for 1-2 hours, standing, and freeze-drying to obtain modified nano phosphogypsum powder; the weight ratio of lauric acid to oleic acid was 1: 2.
And step 3: mixing 100 parts by weight of alumina sol and 15 parts by weight of polyvinyl alcohol solution (mass fraction is 2%), adding 7 parts by weight of boric acid, continuously stirring at the temperature of 40-60 ℃, freezing and forming at the temperature of-60-30 ℃, preparing the obtained nano alumina aerogel through freeze drying, and performing ball milling to obtain nano alumina aerogel powder with the average particle size of 400 nm;
and 4, step 4: 125 parts by weight of phosphorus hemihydrate gypsum powder, 4 parts by weight of modified nano phosphogypsum powder, 7 parts by weight of fumed silica, 10 parts by weight of nano alumina aerogel powder, 5 parts by weight of gypsum excitant and 90 parts by weight of water are mixed and stirred to obtain the light high-strength water-resistant phosphogypsum slurry 4.
Comparative example 1
Compared with example 4, no modified nano phosphogypsum powder is added to the final light high-strength water-resistant phosphogypsum slurry.
Comparative example 2
Compared to example 4, no nano alumina aerogel powder was added to the final lightweight high strength water resistant phosphogypsum slurry.
Comparative example 3
In comparison to example 4, no fumed silica was added to the final light weight, high strength, water resistant phosphogypsum slurry.
The performance test data of the phosphogypsum cementing material 1-4 prepared by the embodiment are shown in the table 1
TABLE 1
In all the above examples, the phosphogypsum slurry in example 2 has the best performance, the compressive strength of 3 days reaches 8.6MPa, the flexural strength of 3 days reaches 4.2MPa, the softening coefficient reaches 0.63, the water absorption rate of 2h is 18.2%, and the water absorption rate of 24h is 18.6%. However, in comparative examples 1 and 2, the nanomaterial was not added as compared to example 4, so that each performance in example 4 was better. In comparative example 3, the water resistance was greatly reduced in comparative example 3 because fumed silica was added in a smaller amount than in example 4.
Other parts not described in detail are prior art. Although the present invention has been described in detail with reference to the above embodiments, it is only a part of the embodiments of the present invention, not all of the embodiments, and other embodiments can be obtained without inventive step according to the embodiments, and the embodiments are within the scope of the present invention.
Claims (9)
1. A preparation method of light high-strength water-resistant phosphogypsum slurry is characterized by comprising the following steps: the method comprises the following steps:
step 1: taking 100 parts by weight of phosphorus semi-hydrated gypsum and 0.2-0.6 part by weight of a water reducing agent, and wet-grinding the phosphorus semi-hydrated gypsum and the water reducing agent for 2-4 hours according to the water-solid ratio of water to the phosphorus semi-hydrated gypsum of 1.0; preparing into slurry;
step 2: adding 8-16 parts by weight of lauric acid/oleic acid mixed solution into 100 parts by weight of slurry, continuously wet-grinding for 1-2 hours, standing, and freeze-drying to obtain modified nano phosphogypsum powder;
and step 3: mixing 100 parts by weight of alumina sol and 10-20 parts by weight of polyvinyl alcohol solution, adding 6-8 parts by weight of oxidant, continuously stirring under heating conditions, freezing and molding at low temperature, preparing nano alumina aerogel by freeze drying, and performing ball milling to obtain nano alumina aerogel powder;
and 4, step 4: mixing and stirring 100-150 parts by weight of phosphorus semi-hydrated gypsum powder, 2-6 parts by weight of modified nano phosphogypsum powder, 6-8 parts by weight of fumed silica, 10-16 parts by weight of nano alumina aerogel powder, 4-6 parts by weight of gypsum excitant and 70-110 parts of water to obtain the light high-strength water-resistant phosphogypsum slurry.
2. The preparation method of the light-weight, high-strength and water-resistant phosphogypsum slurry according to claim 1 is characterized in that: in the step 1), the water reducing agent is any one of a polycarboxylic acid high-performance water reducing agent, an HSB aliphatic high-efficiency water reducing agent and a naphthalene high-efficiency water reducing agent.
3. The preparation method of the light-weight, high-strength and water-resistant phosphogypsum slurry according to claim 1 is characterized in that: in the step 1), the slurry is water dispersion of phosphogypsum, and the average solid particle size of the slurry is 300-500 nm.
4. The preparation method of the light-weight, high-strength and water-resistant phosphogypsum slurry according to claim 1 is characterized in that: in the step 2), the weight ratio of lauric acid to oleic acid is 1: 1-1: 3.
5. The preparation method of the light-weight, high-strength and water-resistant phosphogypsum slurry according to claim 1 is characterized in that: in the step 3), the mass fraction of the polyvinyl alcohol solution is 0.5-3%.
6. The preparation method of the light-weight, high-strength and water-resistant phosphogypsum slurry according to claim 1 is characterized in that: in the step 3), the oxidant is any one of potassium persulfate, butyraldehyde, glyoxal and boric acid.
7. The preparation method of the light-weight, high-strength and water-resistant phosphogypsum slurry according to claim 1 is characterized in that: in the step 3), the heating temperature is 40-60 ℃.
8. The preparation method of the light-weight, high-strength and water-resistant phosphogypsum slurry according to claim 1 is characterized in that: in the step 3), the freezing and forming temperature is-60 to-30 ℃.
9. The preparation method of the light-weight, high-strength and water-resistant phosphogypsum slurry according to claim 1 is characterized in that: in the step 3), the average particle size of the nano alumina aerogel powder is 400-600 nm.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN116553849A (en) * | 2023-04-06 | 2023-08-08 | 湖北工业大学 | Method for preparing regenerated alpha high-strength gypsum by using waste gypsum |
| CN117049813A (en) * | 2023-10-12 | 2023-11-14 | 莱芜市兆信新材料股份有限公司 | Gypsum water reducer and preparation method and application thereof |
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| CN109851308A (en) * | 2019-04-04 | 2019-06-07 | 湖北合力久盛混凝土有限公司 | A kind of ardealite base cement concrete mortar and its preparation process |
| CN110105039A (en) * | 2019-05-20 | 2019-08-09 | 湖北工业大学 | The preparation method of anhydrous ardealite base assembled light partition wall batten |
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| RU2034805C1 (en) * | 1991-10-28 | 1995-05-10 | Сычева Людмила Ивановна | Raw mixture for lumped phosphogypsum producing |
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| CN116553849A (en) * | 2023-04-06 | 2023-08-08 | 湖北工业大学 | Method for preparing regenerated alpha high-strength gypsum by using waste gypsum |
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| CN117049813B (en) * | 2023-10-12 | 2023-12-26 | 莱芜市兆信新材料股份有限公司 | Gypsum water reducer and preparation method and application thereof |
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