CN112939561B - Phosphogypsum-based light plastering gypsum and preparation method thereof - Google Patents
Phosphogypsum-based light plastering gypsum and preparation method thereof Download PDFInfo
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- CN112939561B CN112939561B CN202110349704.XA CN202110349704A CN112939561B CN 112939561 B CN112939561 B CN 112939561B CN 202110349704 A CN202110349704 A CN 202110349704A CN 112939561 B CN112939561 B CN 112939561B
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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
- C04B28/16—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 anhydrite, e.g. Keene's cement
- C04B28/165—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 anhydrite, e.g. Keene's cement containing synthetic anhydrite
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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
- C04B24/00—Use of organic materials as active ingredients for mortars, concrete or artificial stone, e.g. plasticisers
- C04B24/12—Nitrogen containing compounds organic derivatives of hydrazine
- C04B24/14—Peptides; Proteins; Derivatives thereof
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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
- C04B24/00—Use of organic materials as active ingredients for mortars, concrete or artificial stone, e.g. plasticisers
- C04B24/24—Macromolecular compounds
- C04B24/38—Polysaccharides or derivatives thereof
- C04B24/383—Cellulose or derivatives thereof
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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
- C04B2111/00474—Uses not provided for elsewhere in C04B2111/00
- C04B2111/00482—Coating or impregnation 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
- 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
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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
- 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 provides phosphogypsum-based light plastering gypsum and a preparation method thereof, wherein the plastering gypsum comprises the following raw materials in percentage by mass: calcined phosphogypsum and alum 30.1-70.5%, cement 4.5-15.5%, heavy calcium carbonate 14.5-45.5%, vitrified micro-beads 4.5-12.5%, cellulose 0.01-1.0%, coupling agent 0.1-2.0%, tackifier 0.01-1.0% and retarder 0.01-1.5%; the calcined phosphogypsum and the alum are prepared by mixing and calcining alunite raw ore and phosphogypsum. The hemihydrate-anhydrite mixed phase gypsum cementing material prepared by calcination can utilize the hydration characteristics of two gypsum phases, fully exert the advantages of the two gypsum phases, provide a new approach for large-scale utilization of phosphogypsum, and have better environmental and economic benefits.
Description
Technical Field
The invention relates to the field of building materials, in particular to a phosphogypsum-based light plastering gypsum product and a preparation method thereof.
Background
The phosphogypsum is solid waste discharged in the process of producing phosphate fertilizer and phosphoric acid, 4.5-5t of phosphogypsum is produced every 1t of phosphoric acid, and the main component of the phosphogypsum is CaSO4·2H2And O. The production of the phosphogypsum in China is greatly increased along with the annual increase of the yield of the high-concentration phosphorus compound fertilizer, the annual yield is over 7500 ten thousand tons at present, the utilization rate is only 40 percent, 4500-5000 ten thousand tons of newly-stockpiled phosphogypsum are newly added every year, the stockpiling pressure is increased year by year, and the current accumulated stockpiling amount of the phosphogypsum is about 6 hundred million tons. The phosphogypsum is generally grey white or grey black, contains residual organic phosphorus, inorganic phosphorus, fluoride, fluorine, potassium, sodium and other components and other inorganic substances, has more impurity types, and is difficult to be directly applied to producing gypsum building material products, and usually needs to be subjected to impurity removal pretreatment.
The method for removing impurities from phosphogypsum mainly comprises a chemical method, a physical method, a heat treatment method and the like. The heat treatment method is to treat phosphogypsum at high temperature to remove organic matters and eutectic phosphorus in the phosphogypsum, the phosphogypsum is calcined at high temperature to convert the eutectic phosphorus into pyrophosphate, and the organic matters and fluorine impurities are volatilized out through high-temperature treatment. Dihydrate gypsum CaSO as main component of phosphogypsum4·2H2O is also called gypsum, and there are 3 stages of discharging crystal water during heating: 105 ℃ and 180 ℃, 1 water molecule is firstly discharged, then half water molecules are immediately discharged and converted into calcined gypsum (CaSO)4·0.5H2O), also known as plaster of paris or hemihydrate, is an air-setting cementitious material having both alpha and beta forms, both rhombohedral crystals, but with different physical properties; 200 ℃ and 220 ℃, discharging the remaining half water molecules and converting the water molecules into type III anhydrite (CaSO)4·εH2O，0.06<ε<0.11); about 350 ℃ and is converted into anhydrous gypsum type II (CaSO)4) (ii) a 1120 ℃ and further converted into anhydrite I, the melting temperature of which is 1450 ℃.
Along with the rapid development of the building industry in China and the improvement of the environmental protection requirement, the plastering gypsum rapidly develops in China with excellent performances of good heat insulation, sound absorption, flame retardance and impact resistance, adjustable air humidity, low building load, high construction efficiency and the like, the dosage of the plastering gypsum is increased from 110 ten thousand tons to 450 ten thousand tons in 2015 in 2019, the use of the plastering gypsum in large quantity leads to the exhaustion of natural gypsum resources, and great challenge is brought to the sustainable development of the gypsum industry. The patent application with the publication number of CN108947439A discloses a light plastering gypsum and a manufacturing method thereof, the raw materials comprise phosphogypsum, glass beads, a PE gypsum retarder, cellulose H620 and starch ether, and the light plastering gypsum has the advantages of durability, large bonding force, difficult pulverization, no cracking, no hollowing and no powder falling; but the phosphogypsum is not further treated, contains soluble phosphorus and organic impurities and has low hydration rate. Patent publication No. CN101423351B discloses a plastering gypsum comprising 50-60% of uncalcined dihydrate gypsum, 40-50% of an air hardening gypsum binder (containing anhydrous gypsum) and/or a hydraulic hardening binder, and 0-0.3% of a functional additive; because the dihydrate gypsum exists in the raw materials, the subsequent hydration product is cemented with the existing dihydrate gypsum to form a new hardened body, thereby not only preserving the gypsum as a main body and the advantages thereof, but also solving the contradiction in the hydration hardening process. However, the dihydrate gypsum in the raw materials is industrial waste residues such as untreated desulfurized gypsum, phosphogypsum and the like, and the appearance and performance of products are affected by more impurities in the industrial waste residues, particularly, the phosphogypsum also contains some harmful impurities, and the direct use of the industrial waste residues can also generate adverse effects on the environment.
Based on the prior art, the phosphogypsum is used for preparing the plastering gypsum, so that the increasing phosphogypsum stockpiling pressure year by year can be effectively reduced, and the opportunity is provided for the continuous development of the gypsum industry.
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides phosphogypsum-based light plastering gypsum, soluble phosphorus and organic impurities can be effectively removed by calcining the phosphogypsum at a specific temperature, the hydration characteristics of two gypsum phases can be utilized by the semi-hydrated gypsum-anhydrous gypsum mixed phase gypsum cementing material prepared by calcining, and the activity of type AII anhydrous gypsum is excited by beta-semi-hydrated gypsum in the semi-hydrated gypsum-anhydrous gypsum-mixed phase gypsum cementing material, so that the advantages of the two gypsum phases are fully exerted.
The invention also provides a preparation method of the phosphogypsum-based light plastering gypsum.
In order to achieve the purpose, the invention adopts the following technical scheme:
the phosphogypsum-based light plastering gypsum comprises the following raw materials in percentage by mass: calcined phosphogypsum and alum 30.1-70.5%, cement 4.5-15.5%, heavy calcium carbonate 14.5-45.5%, vitrified micro-beads 4.5-12.5%, cellulose 0.05-1.0%, coupling agent 0.1-2.0%, tackifier 0.01-1.0% and retarder 0.01-0.05%; the calcined phosphogypsum and the alum are formed by mixing and calcining alunite raw ore and phosphogypsum; the coupling agent is used for modifying cellulose.
The gypsum phase system is complex and comprises 5 types and 7 varieties, wherein the bonding strength and the water resistance of type AII anhydrous gypsum are superior to those of common building beta-hemihydrate gypsum, but the type AII anhydrous gypsum is very slow in hydration hardening and needs to be added with an excitant to accelerate the hydration hardening rate, and the beta-hemihydrate gypsum is a gypsum phase which is faster in hydration, and the early hydration hardening of the beta-hemihydrate gypsum can reduce the calcium sulfate concentration in the system so as to promote the hydration of the anhydrous gypsum. Therefore, the invention calcines the phosphogypsum and the alum to obtain the semi-hydrated gypsum-anhydrous gypsum mixed phase gypsum cementing material which can fully exert the advantages of two gypsum phases and prepare a mixed phase gypsum product with excellent performance; in addition, the invention creatively discovers that the phosphogypsum and the alum are mutually promoted when being mixed and calcined, the activity of the phosphogypsum is improved, and the excitation effect of the alum on the phosphogypsum is more obvious. Meanwhile, the coupling agent is used for modifying the cellulose, so that the cellulose is more easily and uniformly distributed in the gypsum slurry, and the cellulose is wrapped on the surfaces of gypsum particles together under the action of the retarder, so that the gypsum slurry is more stable, the moisture in the slurry is not easy to lose, and the water is gradually released within a longer period of time, and the plastering gypsum has good water retention and workability. The plastering gypsum is also added with proper amount of water (added according to the water amount of standard consistency) in the preparation process.
More preferably, the raw materials comprise, by mass percent: 50-60% of calcined phosphogypsum and alum, 5-10% of cement, 20-35% of heavy calcium carbonate, 8-10% of vitrified micro bubbles, 0.2-0.25% of cellulose, 0.2-0.5% of coupling agent, 0.04-0.05% of tackifier and 0.01-0.05% of retarder. More preferably, the raw materials comprise, by mass percent: 55% of calcined phosphogypsum and alum, 6.2% of cement, 30% of heavy calcium carbonate, 8% of vitrified micro bubbles, 0.2% of cellulose, 0.5% of coupling agent, 0.05% of tackifier and 0.05% of retarder.
Preferably, in the calcined phosphogypsum and alum, the ratio of alunite to phosphogypsum is 1: 49-1: 199 mass ratio. More preferably, in the calcined phosphogypsum and alum, alunite and phosphogypsum are mixed according to the mass ratio of 1:50-1: 100. The invention discovers that in the process of calcining the phosphogypsum and the alum, the ratio of the alunite to the phosphogypsum influences the activity of the calcined phosphogypsum, the excitation effect of the alum on the phosphogypsum is improved along with the increase of the mixing amount of the alunite, and the setting time is obviously accelerated.
Preferably, the calcination temperature of the calcined phosphogypsum and the calcined alum is 550-680 ℃, and the temperature is kept for 1-2 h. More preferably, the calcination temperature of the calcined phosphogypsum and alum is 600 ℃ and the temperature is kept for 1 h. If the calcining temperature is lower, the amount of AIII type anhydrous gypsum and beta-hemihydrate gypsum in the phosphogypsum is relatively higher, the setting time is accelerated, the water retention rate is reduced, and meanwhile, the existence of more AIII type anhydrous gypsum can cause the performance of the gypsum to be unstable, thus leading to hidden danger of long-term durability burying of gypsum-based plastering gypsum. According to the invention, the semi-water-anhydrous phosphogypsum with a specific phase composition is obtained by calcining the phosphogypsum at a specific high temperature, so that water-soluble phosphorus, fluorine and organic matters can be effectively removed, the effect of removing impurities is achieved, the pretreatment process is omitted, and meanwhile, the whiteness of the phosphogypsum can be improved by calcining at a high temperature.
Preferably, the phase composition of the calcined phosphogypsum comprises 65-85% of beta-hemihydrate gypsum, 10-30% of beta-hemihydrate gypsum, less than 5% of AIII anhydrous gypsum and less than 2% of dihydrate gypsum by mass percentage.
Preferably, the coupling agent is one or two of silane coupling agent gamma-aminopropyl triethoxysilane and gamma- (2, 3-epoxypropoxy) propyl trimethoxysilane, and can effectively couple organic polymer material cellulose, tackifier, retarder, inorganic material gypsum, cement, heavy calcium carbonate and the like, so that the admixture can better play a role.
Preferably, the retarder is a bone collagen retarder which can effectively prolong the setting time of the gypsum and has small influence on the strength of the gypsum.
The invention also provides a preparation method of the phosphogypsum-based light plastering gypsum, which comprises the following steps:
s1, mixing the cellulose, the coupling agent and water according to a certain proportion, stirring and heating to 70-90 ℃ under the condition of 200-400 rpm, preserving heat for 15-45min, and then cooling to room temperature to obtain a solution a;
s2, adding the solution a into a low-alkali solution of a retarder, and stirring at the normal temperature at the rotating speed of 200-400 rpm for 10-30min to prepare a solution b; the pH value of the low alkali solution is 8-9;
and S3, adding the solution b and a tackifier into a proper amount of water to obtain a mixed solution, uniformly mixing the calcined phosphogypsum, alum, cement, heavy calcium carbonate and vitrified micro bubbles, adding the mixed solution into the mixed solution, standing for 1min according to a test method in the GBT28627-2012 plastering gypsum, and slowly stirring for 2min to obtain the light plastering gypsum.
In the preparation method, the cellulose and the coupling agent in the step S1 are added according to the mass percentage of the raw materials, and the preparation method specifically comprises the following steps: 0.05 to 1.0 percent of cellulose, 0.1 to 2.0 percent of coupling agent, and water is added to 100 weight percent for subsequent treatment; step S2, adding the retarder according to the mass percentage of the raw materials, specifically 0.01-0.05% of the retarder, adding water to 100 wt%, and then carrying out subsequent treatment; the appropriate amount of water is added according to the standard consistency water amount at step S3.
If the conventional preparation method is adopted, the raw materials are directly mixed and formed, the modification effect of the coupling agent on the cellulose cannot be exerted, and the effects of the water-retaining agent, the retarder, the tackifier and other additives are reduced, so that the performance is reduced. The invention provides the optimized preparation method of the phosphogypsum-based light plastering gypsum, which enables the gypsum slurry to be more stable, and also enables the moisture in the slurry to be slowly and gradually released, so that the plastering gypsum has good water retention and workability and excellent performance.
Preferably, the heat preservation time in the step S1 is 30 min.
Preferably, the stirring time in step S2 is 15 min.
Compared with the prior art, the invention has the beneficial effects that: the invention adopts calcined phosphogypsum, the phase composition of which is beta-hemihydrate gypsum, AIII type anhydrous gypsum and AIII type anhydrous gypsum, and the activity of AII type anhydrous gypsum can be excited by utilizing the beta-hemihydrate gypsum; in addition, the added cellulose and bone collagen retarders modified by the coupling agent are more easily and uniformly distributed in the gypsum slurry and wrapped on the surfaces of gypsum particles, so that the gypsum slurry is more stable, the moisture in the slurry is not easy to lose, and the retarder is gradually released within a longer period of time, so that the plastering gypsum has good water retention and workability, and the prepared plastering gypsum has the advantages of high bonding strength, low shrinkage rate, low hollowing, no cracking and weather resistance.
Detailed Description
The technical solutions of the present invention will be described clearly and completely with reference to the following embodiments of the present invention, and it should be understood that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Through a large number of experiments, the beneficial effects of the invention can be achieved by adopting the following preferred schemes in the examples:
the heavy calcium carbonate and the vitrified micro bubbles are sold in the market;
the cellulose can be hydroxypropyl methyl cellulose, and is sold in the market;
the coupling agent is one or two of silane coupling agent gamma-aminopropyl triethoxysilane and gamma- (2, 3-epoxypropoxy) propyl trimethoxysilane;
the tackifier can be a special tackifier for gypsum products, and is commercially available;
the retarder is a bone collagen retarder and is sold in the market.
The phosphogypsum-based light plastering gypsum provided in the embodiment comprises the following raw materials in percentage by mass: 50-60% of calcined phosphogypsum and alum, 5-10% of cement, 20-35% of heavy calcium carbonate, 8-10% of vitrified micro bubbles, 0.2-0.25% of cellulose, 0.2-0.5% of coupling agent, 0.04-0.05% of tackifier and 0.01-0.05% of retarder. The calcined phosphogypsum and alum are prepared by mixing and calcining raw alunite ore and phosphogypsum, and the preparation method comprises the following steps:
s1, mixing the cellulose, the coupling agent and water according to a certain proportion, stirring and heating to 70-90 ℃ under the condition of 200-400 rpm, preserving heat for 15-45min, and then cooling to room temperature to obtain a solution a;
s2, adding the solution a into a low-alkali solution of which the pH value is 8-9 of a retarder, and stirring at the normal temperature at the rotating speed of 200-400 rpm for 10-30min to prepare a solution b;
and S3, adding the solution b and a tackifier into a proper amount of water to obtain a mixed solution, uniformly mixing the calcined phosphogypsum, alum, cement, heavy calcium carbonate and vitrified micro bubbles, adding the mixed solution into the mixed solution, standing for 1min according to a test method in the GBT28627-2012 plastering gypsum, and slowly stirring for 2min to obtain the light plastering gypsum.
Example 1
The phosphogypsum-based light plastering gypsum comprises the following raw materials by weight: 550kg of calcined phosphogypsum and alum, 62kg of cement, 300kg of heavy calcium carbonate, 80kg of vitrified micro bubbles, 2kg of cellulose, 5kg of coupling agent, 0.5kg of tackifier and 0.5kg of retarder. Wherein, alunite: the mass ratio of the phosphogypsum is 1:100, the calcining condition is that the temperature is kept for 1h at 600 ℃, and the preparation process comprises the following steps:
(1) mixing the cellulose, the coupling agent and water according to the mass ratio of 2:5:93, stirring and heating to 70 ℃ under the condition of 200rpm, preserving heat for 30min, and then cooling to room temperature to obtain a solution a;
(2) adding the solution a into a low-alkali solution of 5 wt% of the bone collagen retarder, and stirring for 15min at the normal temperature at the rotating speed of 200rpm to prepare a solution b; the pH of the low alkali solution is 8;
(3) and adding the solution b and a tackifier into a proper amount of water, then uniformly mixing the calcined phosphogypsum, alum, cement, coarse whiting and vitrified micro bubbles, adding the mixture into the water, standing for 1min, and slowly stirring for 2min by using a mortar stirrer to prepare the light plastering gypsum.
Example 2
This example is substantially the same as example 1, except for the composition of the lightweight plastering gypsum: 550kg of calcined phosphogypsum and alum, 50kg of cement, 300kg of heavy calcium carbonate, 92kg of vitrified micro bubbles, 2.5kg of cellulose, 5kg of coupling agent, 0.4kg of tackifier and 0.1kg of retarder; mixing the cellulose, the coupling agent and the water in a mass ratio of 2.5:5:92.5 in the step S1; the low alkali solution in S2 contains 1 wt% of bone collagen retarder; the other preparation process of the plastering gypsum was the same as that of example 1.
Example 3
This example is substantially the same as example 1, except for the composition of the lightweight plastering gypsum: 500kg of calcined phosphogypsum and alum, 100kg of cement, 315kg of heavy calcium carbonate, 80kg of vitrified micro bubbles, 2kg of cellulose, 2kg of coupling agent, 0.5kg of tackifier and 0.5kg of retarder; mixing the cellulose, the coupling agent and water in a mass ratio of 2:2:96 in the step S1; the low alkali solution in S2 contains 5 wt% of bone collagen retarder; the other preparation process of the plastering gypsum was the same as that of example 1.
Example 4
This example is substantially the same as example 1, except for the composition of the lightweight plastering gypsum: 500kg of calcined phosphogypsum and alum, 95kg of cement, 300kg of heavy calcium carbonate, 100kg of vitrified micro bubbles, 2.2kg of cellulose, 2kg of coupling agent, 0.5kg of tackifier and 0.3kg of retarder; mixing the cellulose, the coupling agent and the water in a mass ratio of 2.2:2:95.8 in the step S1; the low alkali solution in S2 contains 3 wt% of bone collagen retarder; the other preparation process of the plastering gypsum was the same as that of example 1.
Example 5
This embodiment is substantially the same as embodiment 1 except that: alunite: the mass ratio of the phosphogypsum is 1:80, and the calcining condition is that the temperature is kept at 550 ℃ for 1 h.
Example 6
The phosphogypsum-based light plastering gypsum has the same raw material composition as that of the embodiment 1; wherein, alunite: the mass ratio of the phosphogypsum is 1:50, the calcining condition is 600 ℃, the temperature is kept for 1h, and the preparation process of the plastering gypsum is the same as that of the example 1.
Comparative example 1
The phosphogypsum-based light plastering gypsum has the same raw material composition as that of the embodiment 1; wherein, alunite: the mass ratio of the phosphogypsum is 1:100, the calcining temperature is 350 ℃, the temperature is kept for 1h, and the preparation process is the same as that of the example 1.
Comparative example 2
The phosphogypsum-based light plastering gypsum comprises the following raw materials by weight: 500kg of calcined phosphogypsum and alum, 62kg of cement, 350kg of heavy calcium carbonate, 80kg of vitrified micro bubbles, 2kg of cellulose, 5kg of coupling agent, 0.5kg of tackifier and 0.5kg of retarder; the calcination temperature is 600 ℃, the preparation process comprises the steps of directly mixing the raw materials, adding the mixture into water, standing for 1min, and slowly stirring for 2min by using a mortar stirrer to prepare the light plastering gypsum.
Comparative example 3
The phosphogypsum-based light plastering gypsum has the same raw material composition as that of the embodiment 1; wherein, alunite: the mass ratio of the phosphogypsum is 1:100, the phosphogypsum and the alum are respectively used as raw materials after being calcined, the calcining condition of the alunite is that the temperature is kept for 1h at 600 ℃, the calcining condition of the phosphogypsum is that the temperature is kept for 1h at 600 ℃, and other preparation processes are the same as the example 1.
Test example 1
The light plastering gypsum prepared in the examples 1 to 6 and the comparative examples 1 to 3 is subjected to performance test according to the test method in the plastering gypsum GBT28627-2012, and the results are shown in the table 1:
table 1 results of performance testing
Please analyze according to the detection result:
the test results of examples 1-4 show that, when the total dosage of phosphogypsum and cement is relatively high, the compressive strength and the flexural strength of the plastering gypsum are relatively high, while the volume density of the plastering gypsum is reduced when the dosage of the vitrified micro bubbles is high, but the strength is also reduced, and the bonding strength and the water retention rate of the plastering gypsum are effectively improved when the dosage of the cellulose and the coupling agent is increased, so that the most preferable light plastering gypsum in the application comprises 550kg of calcined phosphogypsum and alum, 62kg of cement, 300kg of heavy calcium carbonate, 80kg of vitrified micro bubbles, 2kg of cellulose, 5kg of coupling agent, 0.5kg of tackifier and 0.5kg of retarder.
From the test results of examples 1, 5 and 6 it can be seen that the higher the proportion of alum, the higher the activity of calcined phosphogypsum, the significantly faster the setting time, and the higher the excitation of alum on phosphogypsum with increasing amount of addition.
In the embodiment 1, when the calcining temperature is lower than that of the comparative example 1, the amounts of AIII type anhydrous gypsum and beta-hemihydrate gypsum in the phosphogypsum are relatively higher, the setting time is accelerated, the water retention rate is reduced, and meanwhile, the existence of more AIII type anhydrous gypsum can cause the unstable performance of the gypsum and hidden danger of long-term durability burying of gypsum-based plastering gypsum.
Combining the results of example 1 and comparative example 2, it was found that when the raw materials were directly mixed for molding, the coupling agent exerted less effect, and the effect of additives such as a water-retaining agent, a retarder, and a tackifier was reduced, resulting in a reduction in performance.
Combining the results of example 1 and comparative example 3, it can be seen that separate calcination of phosphogypsum and alum results in lower activity of phosphogypsum, and it is presumed that the mixed calcination of phosphogypsum and alum promotes each other, improves the activity of phosphogypsum, and has more obvious excitation effect of alum on phosphogypsum.
The foregoing embodiments are merely illustrative of the principles and utilities of the present invention and are intended to provide some examples of technical solutions and not to limit the same, it should be understood by those skilled in the art that the present invention is not limited to the foregoing embodiments, and that various changes and modifications in some or all of the technical features may be made without departing from the spirit and scope of the invention, but such changes and modifications are intended to be within the scope of the invention as claimed.
Claims (9)
1. The phosphogypsum-based light plastering gypsum is characterized by comprising the following raw materials in percentage by mass: calcined phosphogypsum and alum 30.1-70.5%, cement 4.5-15.5%, heavy calcium carbonate 14.5-45.5%, vitrified micro-beads 4.5-12.5%, cellulose 0.05-1.0%, coupling agent 0.1-2.0%, tackifier 0.01-1.0% and retarder 0.01-0.05%; the calcined phosphogypsum and the alum are formed by mixing and calcining alunite raw ore and phosphogypsum; the coupling agent is used for modifying cellulose;
the calcination temperature of the calcined phosphogypsum and the calcined alum is 550-680 ℃, and the temperature is kept for 1-2 h.
2. The phosphogypsum-based light plastering gypsum according to claim 1, is characterized by comprising the following raw materials in percentage by mass: 50-60% of calcined phosphogypsum and alum, 5-10% of cement, 20-35% of heavy calcium carbonate, 8-10% of vitrified micro bubbles, 0.2-0.25% of cellulose, 0.2-0.5% of coupling agent, 0.04-0.05% of tackifier and 0.01-0.05% of retarder.
3. The phosphogypsum-based light-weight plastering gypsum of claim 1, wherein in the calcined phosphogypsum and alum, the proportion of alunite and phosphogypsum is 1: 49-1: 199 mass ratio.
4. The phosphogypsum-based light weight plastering gypsum of claim 1, wherein the phase composition of the phosphogypsum after calcination comprises 65-85% of beta-hemihydrate gypsum, 10-30% of AIII type anhydrous gypsum, less than 5% of AIII type anhydrous gypsum and less than 2% of dihydrate gypsum by mass percent.
5. The phosphogypsum-based light-weight plastering gypsum of claim 1, wherein the coupling agent is one or two of a silane coupling agent gamma-aminopropyltriethoxysilane and gamma- (2, 3-epoxypropoxy) propyltrimethoxysilane.
6. The phosphogypsum-based light-weight plastering gypsum of claim 1, wherein the retarder is an ossein retarder.
7. The preparation method of the phosphogypsum-based light weight plastering gypsum as claimed in any one of claims 1 to 6, which is characterized by comprising the following steps:
s1, mixing the cellulose, the coupling agent and water according to a certain proportion, stirring and heating to 70-90 ℃ under the condition of 200-400 rpm, preserving heat for 15-45min, and then cooling to room temperature to obtain a solution a;
s2, adding the solution a into a low-alkali solution of a retarder, and stirring for 10-30min at a rotating speed of 200-400 rpm under a normal temperature condition to prepare a solution b; the pH value of the low alkali solution is 8-9;
and S3, adding the solution b and a tackifier into a proper amount of water to obtain a mixed solution, then uniformly mixing the calcined phosphogypsum, alum, cement, heavy calcium carbonate and vitrified micro bubbles, adding the mixture into the mixed solution, standing for 1min, and slowly stirring for 2min to obtain the light plastering gypsum.
8. The method for preparing phosphogypsum-based lightweight plastering gypsum according to claim 7, wherein the heat preservation time in step S1 is 30 min.
9. The method for preparing phosphogypsum-based lightweight plastering gypsum according to claim 7, wherein the stirring time in step S2 is 15 min.
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