CN111635209A - Calcination-free phosphogypsum brick and manufacturing method thereof - Google Patents
Calcination-free phosphogypsum brick and manufacturing method thereof Download PDFInfo
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- CN111635209A CN111635209A CN202010549251.0A CN202010549251A CN111635209A CN 111635209 A CN111635209 A CN 111635209A CN 202010549251 A CN202010549251 A CN 202010549251A CN 111635209 A CN111635209 A CN 111635209A
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- 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
- 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B28—WORKING CEMENT, CLAY, OR STONE
- B28B—SHAPING CLAY OR OTHER CERAMIC COMPOSITIONS; SHAPING SLAG; SHAPING MIXTURES CONTAINING CEMENTITIOUS MATERIAL, e.g. PLASTER
- B28B1/00—Producing shaped prefabricated articles from the material
- B28B1/14—Producing shaped prefabricated articles from the material by simple casting, the material being neither forcibly fed nor positively compacted
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B28—WORKING CEMENT, CLAY, OR STONE
- B28B—SHAPING CLAY OR OTHER CERAMIC COMPOSITIONS; SHAPING SLAG; SHAPING MIXTURES CONTAINING CEMENTITIOUS MATERIAL, e.g. PLASTER
- B28B11/00—Apparatus or processes for treating or working the shaped or preshaped articles
- B28B11/24—Apparatus or processes for treating or working the shaped or preshaped articles for curing, setting or hardening
- B28B11/245—Curing concrete articles
-
- 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
- C04B2111/00017—Aspects relating to the protection of the environment
-
- 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
- C04B2111/20—Resistance against chemical, physical or biological attack
-
- 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
- C04B2111/20—Resistance against chemical, physical or biological attack
- C04B2111/27—Water resistance, i.e. waterproof or water-repellent 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
- C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
- C04B2111/76—Use at unusual temperatures, e.g. sub-zero
-
- 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
- C04B2201/20—Mortars, concrete or artificial stone characterised by specific physical values for the density
-
- 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 calcination-free phosphogypsum brick and a manufacturing method thereof, belonging to the field of building materials. The formula comprises phosphogypsum, aggregate, cement and an alkaline activator. The preparation method comprises the steps of mixing the raw materials in proportion, stirring, crushing, extruding, forming and maintaining to finally obtain the finished product of the calcination-free phosphogypsum brick. The calcination-free phosphogypsum brick prepared by the invention has the advantages of compression resistance and fracture resistanceHigh strength, water resistance, frost resistance and durability. The main raw materials of the invention are phosphogypsum, aggregate and other bulk solid wastes which are activated and reasonably mixed into the phosphogypsum brick, thereby avoiding the complicated pretreatment processes of phosphogypsum, such as washing, drying, calcining and the like, and not generating and discharging CO2、NO2、SO2And greenhouse gases, waste water and secondary solid wastes. The invention greatly improves the utilization rate of the phosphogypsum, reduces the accumulation of the phosphogypsum, reduces the pollution rate of land and makes great contribution to environmental protection.
Description
Technical Field
The invention relates to the technical field of building materials, in particular to a calcination-free phosphogypsum brick and a manufacturing method thereof.
Background
The industrial by-product phosphogypsum is industrial solid waste generated in the process of producing phosphoric acid by a wet method, and about 4 to 5 tons of phosphogypsum are discharged when 1 ton of phosphoric acid is produced. Due to the limitation of technical level, the actual utilization rate of the phosphogypsum in China is only about 10 percent at present, and a large amount of phosphogypsum cannot be effectively treated actually.
The biggest difference between phosphogypsum and natural gypsum is that phosphogypsum contains certain impurities which affect the limited utilization of phosphogypsum to varying degrees. Pure phosphogypsum is pure white but is often dark grey due to impurities. The actual density of the phosphogypsum is 1.40-1.8 g/cm3The bulk density is 1.05 to 1.45g/cm3(ii) a Permeability coefficient of 10-3～10- 5cm/s, the horizontal permeability can be two orders of magnitude higher than the vertical permeability; contains radioactive elements such as Ra and Th, and has certain radioactivity; contains acid substances and has stronger acidity.
The disadvantages cause that the phosphogypsum is difficult to be utilized, the stacking of the phosphogypsum not only occupies a large amount of land and consumes a large amount of capital, but also can lead the soluble P in the phosphogypsum to be changed along with the passage of time2O5And fluorine and other impurities are leached out with rainwater to generate acidic wastewater, so that the pollution of soil, a water system and the atmosphere is caused, and serious ecological hazard is caused.
Therefore, a method for effectively utilizing phosphogypsum is urgently needed.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a calcination-free phosphogypsum brick which can effectively improve the utilization rate of phosphogypsum. The second purpose of the invention is to provide a manufacturing method of the calcination-free phosphogypsum brick.
In order to realize the first purpose of the invention, the invention is realized by the following technical scheme:
the calcination-free phosphogypsum brick comprises the following components in percentage by mass:
preferably, the aggregate comprises at least one of clay ceramsite, fly ash ceramsite, ceramic sand, scoria, coal slag, coal gangue, slag and/or melon and rice stone.
Preferably, the water content of the phosphogypsum is less than or equal to 27 percent.
Preferably, the particle size of the aggregate is less than or equal to 8 mm.
Preferably, the activity index of the alkali-activator is more than or equal to 60 percent.
Preferably, the content of insoluble substances in the cement is less than or equal to 1.5 percent, the loss on ignition is less than or equal to 5.0 percent, the content of magnesium oxide is less than or equal to 5.0 percent, the content of sulfur trioxide is less than or equal to 3.0 percent, and the specific surface area is more than or equal to 300m3The fineness is less than or equal to 80 mu m, the screen residue of the square-hole screen is less than or equal to 10 percent, the initial setting time is more than 45min, and the final setting time is less than 10 h.
In order to achieve the second purpose of the invention, the method is realized by the following technical scheme:
the method for manufacturing the calcination-free phosphogypsum brick comprises the following steps:
(1) weighing the raw materials in proportion;
(2) mixing and stirring phosphogypsum and aggregate to prepare a first mixture;
(3) adding cement and an alkaline activator into the first mixture and stirring to obtain a second mixture;
(4) placing the mixture II into a mold for molding, and conveying the mixture II into a curing room for curing for at least 24 hours;
(5) then transferring the brick out of a curing room, and curing for at least 24 hours at the temperature of more than or equal to 10 ℃ to obtain the finished product of the calcination-free phosphogypsum brick.
Preferably, the mixing in the step (2) is carried out until the material uniformity of the first mixed material is more than or equal to 95%.
Preferably, the stirring in the step (3) is carried out until the maximum particle size of the second mixture is less than or equal to 10 mm.
The calcination-free phosphogypsum brick prepared by the method has high compression strength and breaking strength, and good water resistance, frost resistance and durability. The main raw materials of the invention are phosphogypsum, aggregate and other bulk solid wastes which are activated and reasonably mixed into the phosphogypsum brick, so that the effect of advantage superposition can be achieved, the complicated pretreatment processes of phosphogypsum, such as washing, drying, calcining and the like, are avoided, and no CO emission is generated2、NO2、SO2And greenhouse gases, waste water and secondary solid wastes. The invention greatly improves the utilization rate of the phosphogypsum, reduces the accumulation of the phosphogypsum, reduces the pollution rate of land and makes great contribution to environmental protection.
Detailed Description
The following specific examples are provided to further illustrate the present invention so that those skilled in the art may better understand the invention and practice it, but the examples are not intended to limit the invention.
The aggregate contains active SiO2 and Al2O3, and can react with Ca (OH)2 to produce C-S-H gel and hydrated calcium sulfate, increase the bonding between the components in the PGS (phosphogypsum-based cementing material) solidified body and the fine aggregate, and improve the compactness of the phosphogypsum brick; the alkaline activator improves the alkalinity of a PGS system, neutralizes the acid of the phosphogypsum, promotes the hydration of the phosphogypsum system, shortens the setting time and improves the compactness, the strength and the water resistance of the PGS; under the excitation of sulfate, an exciting agent and cement, the aggregate generates a large amount of floccules to coat each component of the phosphogypsum brick to form a compact net structure, so that the compactness, the freezing resistance and the like of the phosphogypsum brick are improved, the mechanical property of the phosphogypsum brick is obviously improved, and various properties such as drying shrinkage, freezing and thawing, softening, corrosion resistance and the like are improved, so that the product performance is better.
Due to the fact that the content of harmful substances such as water-soluble phosphorus pentoxide and water-soluble chloride ions in the phosphogypsum is low in raw materials, through a series of neutralization reactions, the content of the water-soluble phosphorus pentoxide in a final product is 0 (which is not up to the detection limit) through test detection, and the content of the water-soluble chloride ions is only 0.006%, so that the use safety of the phosphogypsum brick is guaranteed. Reference can be made to the preparation and performance research of the calcination-free phosphogypsum brick, Huiyoxin, Wanjiandong, Huasu dong and the like
The raw materials were weighed out in the proportions given in table 1 below.
TABLE 1
| Unit: is based on | Example one | Example two |
| Phosphogypsum | 20 | 30 |
| Melon and rice stone | 69.8 | 57.8 |
| Cement | 10 | 12 |
| Alkali activator | 0.2 | 0.2 |
Wherein the phosphogypsum needs to have the water content less than or equal to 27 percent and no coarse blocks, and can meet the metering requirement.
The alkali activator needs to pass through a square hole sieve with 0.08mm, the residue is less than or equal to 5.0 percent, and the activity index is more than or equal to 62 percent.
The aggregate needs to be qualified in stability, the maximum particle size is less than or equal to 8mm, and the aggregate does not contain metal and wood materials. In the specific embodiment, the melon-rice stone is used as the aggregate, and other materials can be adopted
The cement needs less than or equal to 1.5 percent of insoluble substances in the cement, less than or equal to 5.0 percent of loss on ignition, less than or equal to 5.0 percent of magnesium oxide, less than or equal to 3.0 percent of sulfur trioxide, and the specific surface area is more than or equal to 300m3The fineness is less than or equal to 80 mu m, the screen residue of the square-hole screen is less than or equal to 10 percent, the initial setting time is more than 45min, and the final setting time is less than 10 h. The compressive strength at least satisfies: 3 d: 16.0, 28 d: 42.5; the flexural strength at least satisfies: 3 d: 3.5, 28 d: 6.5;
the manufacturing method comprises the following steps:
(1) weighing the raw materials according to the proportion in the table 1;
(2) adding the phosphogypsum and the aggregate into a stirrer for crushing and uniformly stirring to obtain a mixture I; the step requires the metering precision to be less than 1.0 percent and the material uniformity to be more than 95 percent; generally, a mixing and stirring time of >3min, a feed time of <30s, and a discharge time of <30s is required.
(3) Adding the cement and the alkaline activator into the second mixture and stirring uniformly again to obtain a second mixture; at the moment, the materials are in a block shape, a high-speed rotating forced dispersion machine is adopted to carry out homogenization and dispersion on the materials so as to realize the final uniform distribution of the materials, and the maximum particles of the dispersed materials are required to be less than or equal to 10 mm. Stirring time: 3min
(4) And placing the mixture II into a forming die on a block forming machine to obtain a forming rotor.
The block forming machine has the functions of automatically distributing dry powder to the supporting plate when supplying plates, distributing dry powder to the surface of the raw material in the die for the second time after completing automatic distribution, automatically forming, demoulding, feeding plates and stacking blanks.
(5) And transferring the formed product into a curing room for curing for at least 24 hours.
The curing room needs constant temperature and humidity, and the curing room is automatically stacked after curing and sent to a protection field for continuous natural curing.
(6) Moving the product to a curing room, and naturally curing for at least 24 hours at the temperature of more than or equal to 10 ℃ to obtain a finished product, wherein the curing is usually required for 10-15 days. The finished product has the appearance of lacking edges and falling corners obviously, and the size of the finished product meets the standard requirement and is a qualified product.
Measurement of the properties of the finished product:
the specification of the finished product of the above example is 238X45X1115mm, and the weight is 2.5 kg. Under the same environmental conditions, the strength grade is up to 12MPA, the compressive strength is 11, the flexural strength is up to 6.6, the water content is 5.6%, the water absorption is 7.1%, and the density is 1350kg/m3The water resistance coefficient is 15.6, the softening coefficient is 0.8, the carbonization coefficient is 0.96, and the rapid shrinkage value is 0.046%.
The test conditions and the standard thereof are recorded in GB-T23456-2009 phosphogypsum.
Claims (9)
1. The calcination-free phosphogypsum brick is characterized by comprising the following components in percentage by mass:
2. the calcination-free phosphogypsum brick according to claim 1, which is characterized in that: the aggregate comprises at least one of clay ceramsite, fly ash ceramsite, ceramic sand, scoria, coal slag, coal gangue, slag and/or melon and rice stone.
3. The calcination-free phosphogypsum brick according to claim 1, which is characterized in that: the water content of the phosphogypsum is less than or equal to 27 percent.
4. The calcination-free phosphogypsum brick according to claim 1, which is characterized in that: the particle size of the aggregate is less than or equal to 8 mm.
5. The calcination-free phosphogypsum brick according to claim 1, which is characterized in that: the activity index of the alkaline excitant is more than or equal to 60 percent.
6. The calcination-free phosphogypsum brick according to claim 1, which is characterized in that: the content of insoluble substances in the cement is less than or equal to 1.5 percent, and the loss on ignition isLess than or equal to 5.0 percent, less than or equal to 5.0 percent of magnesium oxide, less than or equal to 3.0 percent of sulfur trioxide, and the specific surface area is more than or equal to 300m3The fineness is less than or equal to 80 mu m, the screen residue of the square-hole screen is less than or equal to 10 percent, the initial setting time is more than 45min, and the final setting time is less than 10 h.
7. A method for making a calcination-free phosphogypsum brick as claimed in any one of claims 1 to 6, characterized by comprising the following steps:
(1) weighing the raw materials in proportion;
(2) mixing and stirring phosphogypsum and aggregate to prepare a first mixture;
(3) adding cement and an alkaline activator into the first mixture and stirring to obtain a second mixture;
(4) placing the mixture II into a mold for molding, and conveying the mixture II into a curing room for curing for at least 24 hours;
(5) then transferring the brick out of a curing room, and curing for at least 24 hours at the temperature of more than or equal to 10 ℃ to obtain the finished product of the calcination-free phosphogypsum brick.
8. The method for manufacturing the calcination-free phosphogypsum brick according to claim 7, is characterized in that: and (3) mixing and stirring in the step (2) until the material uniformity of the first mixture is more than or equal to 95%.
9. The method for manufacturing the calcination-free phosphogypsum brick according to claim 7, is characterized in that: and (4) stirring in the step (3) until the maximum particle size of the material of the mixture II is less than or equal to 10 mm.
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| CN202010549251.0A CN111635209A (en) | 2020-06-16 | 2020-06-16 | Calcination-free phosphogypsum brick and manufacturing method thereof |
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| CN202010549251.0A CN111635209A (en) | 2020-06-16 | 2020-06-16 | Calcination-free phosphogypsum brick and manufacturing method thereof |
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| CN114988832A (en) * | 2022-05-18 | 2022-09-02 | 中国地质大学（武汉） | Method for preparing daily flowerpot by utilizing regenerated gypsum and burnt waste ceramic sand |
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| CN114988832A (en) * | 2022-05-18 | 2022-09-02 | 中国地质大学（武汉） | Method for preparing daily flowerpot by utilizing regenerated gypsum and burnt waste ceramic sand |
| CN114988832B (en) * | 2022-05-18 | 2022-10-28 | 中国地质大学（武汉） | Method for preparing daily flowerpot by using regenerated gypsum and waste ceramic sand |
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Application publication date: 20200908 |