CN111847956A - Phosphogypsum-based cement retarder and preparation method and application thereof - Google Patents
Phosphogypsum-based cement retarder and preparation method and application thereof Download PDFInfo
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- CN111847956A CN111847956A CN202010674315.XA CN202010674315A CN111847956A CN 111847956 A CN111847956 A CN 111847956A CN 202010674315 A CN202010674315 A CN 202010674315A CN 111847956 A CN111847956 A CN 111847956A
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B40/00—Processes, in general, for influencing or modifying the properties of mortars, concrete or artificial stone compositions, e.g. their setting or hardening ability
- C04B40/0028—Aspects relating to the mixing step of the mortar preparation
- C04B40/0039—Premixtures of ingredients
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2103/00—Function or property of ingredients for mortars, concrete or artificial stone
- C04B2103/20—Retarders
- C04B2103/22—Set retarders
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Abstract
The invention provides a phosphogypsum-based cement retarder and a preparation method and application thereof, wherein the phosphogypsum-based cement retarder is prepared by mixing 90-95% of phosphogypsum, 3-6% of slag powder or fly ash, 2-4% of calcareous quicklime powder or calcareous slaked lime powder or carbide slag powder, adding a proper amount of alkali activator, mixing and balling; the dosage of the alkali-activator is 6-15% of the dosage of the slag powder or the fly ash calculated by the mass of Na 2O. The invention can effectively adsorb and solidify soluble phosphorus, fluorine and the like in the phosphogypsum and neutralize organic matters, thereby greatly reducing the adverse effect of harmful substances in the phosphogypsum on the setting time and the early strength of cement, and the aging time of the phosphogypsum-based cement retarder is short, thereby greatly improving the production efficiency of the phosphogypsum-based cement retarder.
Description
Technical Field
The invention belongs to the technical field of cement retarders, and particularly relates to a phosphogypsum-based cement retarder as well as a preparation method and application thereof.
Background
Phosphogypsum is waste residue generated in the wet process of producing phosphoric acid in the phosphate fertilizer industry, and about 5 tons of phosphogypsum are discharged when each 1 ton of phosphoric acid is produced. Due to the rapid and strong development of the phosphorus chemical industry, the yield of the phosphogypsum waste residue is also rapidly increased. At present, the annual emission of phosphogypsum in China is about 8400 million tons, and the comprehensive utilization rate is about 30 percent. At present, the accumulated phosphogypsum stockpiling quantity in China exceeds 3 hundred million tons. The phosphogypsum is piled for a long time, not only occupies a large amount of land, but also contains free acid which can pollute underground water sources, and fluoride can permeate underground polluted soil.
The main component of the phosphogypsum is dihydrate stonePaste (CaSO)4·2H2O), similar to natural gypsum, is an important renewable gypsum resource. At present, the cement retarder is the main utilization way of phosphogypsum, and the utilization amount of the cement retarder accounts for more than 60 percent of the total utilization amount. However, when the phosphogypsum is used as a cement retarder, the phosphogypsum is acidic and has certain corrosivity due to the existence of impurities such as soluble phosphorus, fluorine, organic matters and the like, the setting time of the cement can be seriously delayed, and the early strength of the cement is reduced, so that the application of the phosphogypsum in the cement is limited. In addition, the freshly discharged phosphogypsum is wet coarse granular powder, generally contains 15-25% of attached water, is not beneficial to transportation and metering, and is easy to cause caking and blockage of a discharging bin, paste grinding in a cement mill and the like. Therefore, before the phosphogypsum is used for a cement retarder, modification and granulation molding pretreatment needs to be carried out on the problems of excessive retardation and feeding of the phosphogypsum.
The existing phosphogypsum pretreatment method mainly comprises the following steps: water washing method, neutralization method, lime washing method, flotation method, flash firing method, half-water and half-water phosphogypsum balling method, chemical modification balling method and the like.
Wherein, the washing method has mature technology, the performance of the treated gypsum is more stable, but the washing process is complex, the investment is large, the water consumption and the drying energy consumption are higher, and the sewage after washing can be discharged after being treated. The neutralization method adopts cheap lime to neutralize acid in phosphogypsum and soluble P 2O5Insoluble matters are generated, the soluble matters are changed into inert matters, the process is simple, the investment is small, no pollution is caused, but the performance of the treated phosphogypsum is unstable.
The lime washing method is a combination of a water washing method and a lime neutralization method, and similar to the water washing method, on one hand, soluble impurities of phosphogypsum can be cleaned, and on the other hand, residual acid can be neutralized to generate insoluble matters, but the method has the disadvantages of difficult sewage treatment and high drying energy consumption. The flotation method mainly eliminates the influence of organic impurities on the phosphogypsum, but does not fundamentally eliminate the influence of soluble phosphorus and fluorine impurities, and the problem of excessive slow setting of the phosphogypsum is not solved.
The flash burning method is to calcine phosphogypsum at 800 ℃, decompose and volatilize harmful substances such as fluorine, organic matters and the like at high temperature, and convert soluble phosphorus and eutectic phosphorus into inert pyrophosphate minerals so as to reduce the adverse effect of harmful impurities in the phosphogypsum on the setting time of cement, but the high-temperature calcination needs to consume a large amount of coal and produces a small amount of acidic harmful gas in the calcining process to pollute the atmosphere.
A semi-hydrated phosphogypsum balling method includes calcining and dehydrating phosphogypsum at a certain temperature to form semi-hydrated gypsum, uniformly stirring the semi-hydrated gypsum, the phosphogypsum, lime and water, cementing the uncalcined phosphogypsum, balling, drying and warehousing by utilizing the characteristic that the semi-hydrated gypsum is hydrated to form the dihydrate gypsum with certain strength.
A chemical modified balling method for ardealite features that the ardealite is chemically modified by flyash and lime, and the acid-alkali neutralization reaction between lime and soluble P and F in ardealite and the volcanic ash reaction of flyash under the excitation of lime and ardealite can lower the content of soluble P and F in ardealite, and the ardealite is shaped into a ball with a certain strength by cementing it, but because the chemical reaction is slow and low in strength, the flyash content is 30-35% and ageing at ordinary temp. takes at least 7 days for use, resulting in greatly lowered productivity3The content is greatly reduced.
Disclosure of Invention
Aiming at the problems in the prior art, the invention aims to provide a phosphogypsum-based cement retarder to solve the problems of high production cost, low production efficiency and SO in modified phosphogypsum balls of the existing phosphogypsum retarder3The content is low.
The technical scheme adopted for solving the problems in the prior art is as follows:
a phosphogypsum-based cement retarder is prepared by mixing 90-95% of phosphogypsum, 3-6% of slag powder or fly ash and 2-4% of calcareous quicklime powder or calcareous slaked lime powder or carbide slag powder in percentage by mass, and adding Mixing appropriate amount of alkali activator, and making into ball; the dosage of the alkali activator is converted into Na2The mass of the O is 6-15% of the amount of the slag powder or the fly ash.
The alkali activator is water glass or sodium hydroxide, and the content of the alkali activator in the cement retarder is Na2The percentage of the O equivalent is expressed.
The modulus of the water glass is 1.0-1.5.
The CaO content in the calcareous quicklime powder is more than or equal to 65 percent, and the sieve residue with the particle size of 90 mu m is less than or equal to 7 percent.
The CaO content of the calcareous slaked lime powder or the carbide slag powder excluding free water and bound water is more than or equal to 65 percent, and the residue of a 90 mu m sieve is less than or equal to 7 percent.
The slag powder is S75-grade slag powder.
The fly ash is class II fly ash.
The method for preparing the phosphogypsum-based cement retarder is characterized by comprising the following steps:
step 1, uniformly mixing phosphogypsum, slag powder or fly ash, calcareous quicklime powder or calcareous slaked lime powder or carbide slag powder, adding an alkali activator, and continuously mixing until uniform to obtain a mixed material A;
and 2, preparing the mixed material A into wet material balls by a disc ball forming mill, and aging for 2 days or more to obtain the spherical phosphogypsum-based cement retarder.
The water content of wet pellets in the pelletizing of the mixed material A is 16-18%.
The application of the phosphogypsum-based cement retarder is characterized in that the phosphogypsum-based cement retarder is used as a raw material to prepare cement, and the cement comprises the following components in percentage by mass: 80-85% of silicate cement clinker, 5-8% of electric furnace slag, 5-10% of limestone and 3-7% of phosphogypsum-based cement retarder, and the mixture of the components is ground to specific surface area (350 +/-50) m2/kg。
The invention has the following advantages:
the phosphogypsum-based cement retarder takes phosphogypsum as a main component and is prepared by adding slag powder or powderOn one hand, the lime can effectively solidify soluble phosphorus, fluorine, organic matters and the like in the phosphogypsum to form insoluble calcium phosphate and calcium fluoride, so that the influence of harmful substances in the phosphogypsum on the setting time of the cement is greatly reduced; on the other hand, the addition of the alkali activator in the phosphogypsum-based cement retarder can promote the depolymerization and the re-polymerization of an aluminosilicate mineral phase in slag powder or fly ash to form geopolymer, further adsorb and solidify phosphorus and fluorine, thereby being beneficial to further reducing the influence of harmful substances in phosphogypsum on the setting time of cement; meanwhile, lime and phosphogypsum can also carry out alkaline and sulfate excitation on the slag powder or the fly ash, so that the chemical activity of the slag powder or the fly ash is improved, hydration products with gelling properties, such as calcium silicate hydrate gel, ettringite crystal and the like, are formed at the early stage, the early strength of a phosphogypsum ball is improved together, and the phosphogypsum-based cement retarder can be used after all raw materials are mixed into a ball and aged for 2 days, so that the production efficiency of the phosphogypsum-based cement retarder is greatly improved, the energy consumption in the whole process is extremely low, and the production cost is greatly reduced. In addition, the phosphogypsum-based cement retarder can effectively improve the early and later mechanical properties of cement, and SO in the phosphogypsum-based cement retarder 3The content can be stabilized above 35%, the retarding effect is stable, the adaptability to different clinkers is good, and the requirement of producing high-quality cement performance indexes of 42.5 grades and above can be met.
Detailed Description
The technical scheme of the invention is further specifically described by the following embodiments:
example 1
A phosphogypsum-based cement retarder is prepared by mixing 92% of phosphogypsum, 5% of slag powder and 3% of calcareous quicklime powder in percentage by mass, adding water glass, continuously stirring until the mixture is uniform, and balling; the amount of water glass is converted into Na2The mass of O is 6 percent of the using amount of the slag powder. Wherein the attached water content of the phosphogypsum is 17.2 percent; the CaO content in the calcareous quicklime powder is more than or equal to 65 percent,the 90 mu m sieve allowance is less than or equal to 7 percent; the slag powder is S75 grade slag powder; the modulus of water glass is 1.0.
The phosphogypsum-based cement retarder is prepared by the following steps:
1) according to the component ratio, uniformly mixing phosphogypsum, slag powder and calcareous quicklime powder, adding water glass, and continuously mixing until uniform to obtain a mixed material A;
2) and (3) balling the mixed material A by using a disc balling machine, and aging for 2 days to obtain the phosphogypsum-based cement retarder.
When the disc ball forming machine forms balls, water accounting for 0.2-2.2% of the total amount of the mixed material A is additionally sprayed on the disc according to the requirement of forming balls, so that the water content of the material balls is 16-18%, and the balls are convenient to form.
The phosphogypsum-based cement retarder is used for preparing cement, and the cement is prepared from the following components in percentage by mass: portland cement clinker: 82%, electric furnace slag: 6%, limestone: 7%, phosphogypsum-based cement retarder: 5 percent. Grinding the mixture by a ball mill to specific surface area (350 +/-10) m2/kg。
Example 2
This example differs from example 1 in that: the phosphogypsum-based cement retarder is prepared by mixing 92% of phosphogypsum, 5% of slag powder and 3% of calcareous quicklime powder in percentage by mass, adding water glass, continuously stirring until the mixture is uniform and balling; the amount of water glass is converted into Na2The mass of O is 10 percent of the using amount of the slag powder; wherein the attached water content of the phosphogypsum is 17.2 percent; the CaO content in the calcareous quicklime powder is more than or equal to 65 percent, and the sieve residue with the particle size of 90 mu m is less than or equal to 7 percent; the slag powder is S75 grade slag powder; the modulus of water glass is 1.0.
Example 3
This example differs from example 1 in that: the phosphogypsum-based cement retarder is prepared by mixing 92% of phosphogypsum, 5% of slag powder and 3% of calcareous quicklime powder in percentage by mass, adding water glass, continuously stirring until the mixture is uniform and balling; the amount of water glass is converted into Na 2The mass of O is 6 percent of the using amount of the slag powder. WhereinThe attached water content of the phosphogypsum is 17.2 percent; the CaO content in the calcareous quicklime powder is more than or equal to 65 percent, and the sieve residue with the particle size of 90 mu m is less than or equal to 7 percent; the slag powder is S75 grade slag powder; the modulus of water glass is 1.5.
Example 4
This example differs from example 1 in that: the phosphogypsum-based cement retarder is prepared by mixing 92% of phosphogypsum, 5% of slag powder and 3% of calcareous quicklime powder in percentage by mass, adding water glass, continuously stirring until the mixture is uniform and balling; the amount of water glass is converted into Na2The mass of O is 10 percent of the using amount of the slag powder. Wherein the attached water content of the phosphogypsum is 17.2 percent; the CaO content in the calcareous quicklime powder is more than or equal to 65 percent, and the sieve residue with the particle size of 90 mu m is less than or equal to 7 percent; the slag powder is S75 grade slag powder; the modulus of water glass is 1.5.
Example 5
This example differs from example 1 in that: the phosphogypsum-based cement retarder is prepared by mixing 92% of phosphogypsum, 5% of slag powder and 3% of calcareous quicklime powder in percentage by mass, adding sodium hydroxide, and continuously stirring until the mixture is uniform and formed into balls; the amount of sodium hydroxide is converted to Na2The mass of O is 6 percent of the using amount of the slag powder. Wherein the attached water content of the phosphogypsum is 17.2 percent; the CaO content in the calcareous quicklime powder is more than or equal to 65 percent, and the sieve residue with the particle size of 90 mu m is less than or equal to 7 percent; the slag powder is S75 grade slag powder.
Example 6
This example differs from example 1 in that: the phosphogypsum-based cement retarder is prepared by mixing 92% of phosphogypsum, 5% of slag powder and 3% of calcareous quicklime powder in percentage by mass, adding sodium hydroxide, and continuously stirring until the mixture is uniform and formed into balls; the amount of sodium hydroxide is converted to Na2The mass of O is 10 percent of the using amount of the slag powder. Wherein the attached water content of the phosphogypsum is 17.2 percent; the CaO content in the calcareous quicklime powder is more than or equal to 65 percent, and the sieve residue with the particle size of 90 mu m is less than or equal to 7 percent; the slag powder is S75 grade slag powder.
Example 7
This example differs from example 1 in that: the phosphogypsum-based cement retarder of the embodiment comprises, by mass percent,mixing 92% of phosphogypsum, 5% of slag powder and 3% of calcareous quicklime powder, adding sodium hydroxide, continuously stirring uniformly, and balling to obtain the gypsum; the amount of sodium hydroxide is converted to Na2The mass of O is 15 percent of the using amount of the slag powder. Wherein the attached water content of the phosphogypsum is 17.2 percent; the CaO content in the calcareous quicklime powder is more than or equal to 65 percent, and the sieve residue with the particle size of 90 mu m is less than or equal to 7 percent; the slag powder is S75 grade slag powder.
The performance of the phosphogypsum-based cement retarders of examples 1-7 of the invention was tested and compared with unmodified raw phosphogypsum powder (comparative example 1) and the phosphogypsum-based cement retarder without alkali activator (comparative example 2), and the test results are shown in tables 1 and 2. The compression strength test of the phosphogypsum-based cement retarders in the table 1 is carried out by pressing and forming the mixed material A by using a cylindrical test die with the diameter of 50mm multiplied by 50mm and curing the mixed material A for 3d under the conditions of 20 +/-1 ℃ and 60 +/-5% RH. Phosphogypsum-based cement retarder water-solubility P in Table 2 2O5The content of the water-soluble fluorine is determined according to a standard JC/T2073-2011 'determination method of phosphorus and fluorine in phosphogypsum', and the pH value is determined according to GB/T5484-2012 'gypsum chemical analysis method'.
As shown in Table 1, the comparative example 1 is unmodified phosphogypsum powder which is also used as a cement retarder, but the phosphogypsum powder does not obtain strength after being pressed, formed and cured for 3 days, and the phosphogypsum powder is expected to be modified because the phosphogypsum powder does not have the anti-crushing capability and cannot achieve the required effect even if being pelletized. The comparative example 2 is phosphogypsum-based cement retarder which is not modified by adding alkali activator, and is prepared by mixing 92% of phosphogypsum, 5% of slag powder and 3% of calcareous quicklime powder according to mass percentage, stirring uniformly and balling. Examples 1-7 were further modified by alkali-activated modification with various types and amounts of alkali on the basis of comparative example 2.
The compressive strength of the phosphogypsum-based cement retarder cured 3d in the embodiments 1-7 of the invention exceeds 0.7MPa, and is greatly improved compared with the strength of the comparative example 2, which shows that the phosphogypsum-based cement retarder modified by the alkali-activator obtains higher strength after being aged 3d, and can completely meet the use requirements.
TABLE 1
Harmful substances in the phosphogypsum-based cement retarders of the examples 1 and 4 of the invention are tested and compared with unmodified original phosphogypsum (comparative example 1) and the phosphogypsum cement retarder which is not modified by adding an alkali activator (comparative example 2), and the test results are shown in table 2. As can be seen from Table 2, the water solubility P in the phosphogypsum-based cement retarders of examples 1 and 4 of the invention 2O5Compared with the original unmodified phosphogypsum of the comparative example 1, the content of the water-soluble F harmful substances is greatly reduced, the content of the water-soluble F harmful substances is greatly improved compared with the comparative example 2, the water-soluble F harmful substances completely meet the relevant regulations in the national standard phosphogypsum (GB/T23456-2018), and the obtained phosphogypsum-based cement retarder is stronger in alkalinity, so that the corrosion to a mill when the phosphogypsum-based cement retarder enters a ball mill for grinding cement can be effectively avoided.
TABLE 2
The phosphogypsum-based cement retarders of examples 1-7 of the invention were used in the preparation of cement, and the water consumption for standard consistency, setting time and mortar strength test results for the cement are shown in table 3. As can be seen from table 3, the setting time of the cement prepared by using the phosphogypsum-based cement retarders of examples 1-7 is greatly reduced compared with that of the cement prepared by using the original phosphogypsum (comparative example 1) and the phosphogypsum-based cement retarder (comparative example 2) which is not modified by adding the alkali activator, and the early and later strength performance is improved to different degrees.
TABLE 3
The cements prepared using the phosphogypsum-based cement retarders of examples 1 and 4 of the present invention were tested for mortar fluidity and compatibility with a water reducing agent, and compared with cements prepared using unmodified phosphogypsum (comparative example 1) and natural gypsum (comparative example 3), and the test results are shown in table 4.
As can be seen from table 4, the cement prepared by using the phosphogypsum-based cement retarders of the examples 1 and 4 of the invention is superior to the cement doped with natural gypsum of the comparative example 3 in terms of mortar fluidity, compatibility with a water reducing agent and the like, and is slightly inferior to the cement doped with unmodified raw gypsum of the comparative example 1, but the difference is not significant.
TABLE 4
The protective scope of the present invention is not limited to the above-described embodiments, and it is apparent that various modifications and variations can be made to the present invention by those skilled in the art without departing from the scope and spirit of the present invention. It is intended that the present invention cover the modifications and variations of this invention provided they come within the scope of the appended claims and their equivalents.
Claims (10)
1. An ardealite-based cement retarder is characterized in that: according to the mass percentage, the composite material is prepared by mixing 90-95% of phosphogypsum, 3-6% of slag powder or fly ash and 2-4% of calcareous quicklime powder or calcareous slaked lime powder or carbide slag powder, adding a proper amount of alkali activator, mixing and balling; the dosage of the alkali activator is converted into Na2The mass of the O is 6-15% of the amount of the slag powder or the fly ash.
2. The phosphogypsum-based cement retarder of claim 1, which is characterized in that: the alkali activator is water glass or sodium hydroxide.
3. The phosphogypsum-based cement retarder of claim 2, which is characterized in that: the modulus of the water glass is 1.0-1.5.
4. The phosphogypsum-based cement retarder of claim 1, which is characterized in that: the CaO content in the calcareous quicklime powder is more than or equal to 65 percent, and the sieve residue with the particle size of 90 mu m is less than or equal to 7 percent.
5. The phosphogypsum-based cement retarder of claim 1, which is characterized in that: the CaO content of the calcareous slaked lime powder or the carbide slag powder excluding free water and bound water is more than or equal to 65 percent, and the residue of a 90 mu m sieve is less than or equal to 7 percent.
6. The phosphogypsum-based cement retarder of claim 1, which is characterized in that: the slag powder is S75-grade slag powder.
7. The phosphogypsum-based cement retarder of claim 1, which is characterized in that: the fly ash is class II fly ash.
8. The method for preparing the phosphogypsum-based cement retarder according to any one of claims 1 to 7, which is characterized by comprising the following steps:
step 1, uniformly mixing phosphogypsum, slag powder or fly ash, calcareous quicklime powder or calcareous slaked lime powder or carbide slag powder, adding an alkali activator, and continuously mixing until uniform to obtain a mixed material A;
And 2, preparing the mixed material A into wet material balls by a disc ball forming mill, and aging for 2 days or more to obtain the spherical phosphogypsum-based cement retarder.
9. The method for preparing the phosphogypsum-based cement retarder according to claim 8, which is characterized in that: the water content of wet pellets in the pelletizing of the mixed material A is 16-18%.
10. The use of an ardealite-based cement retarder according to any of claims 1 to 7, characterized in that: the phosphogypsum-based cement retarder is used as a raw material for preparing cement, and is calculated by mass percent,the cement comprises the following components: 80-85% of silicate cement clinker, 5-8% of electric furnace slag, 5-10% of limestone and 3-7% of phosphogypsum-based cement retarder, and the mixture of the components is ground to specific surface area (350 +/-50) m2/kg。
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| CN116375375A (en) * | 2023-04-21 | 2023-07-04 | 哈尔滨理工大学 | Method for improving early strength of magnesium oxysulfide cement |
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