CN110683802A - Preparation method of phosphogypsum-red mud filling body based on MICP technology - Google Patents
Preparation method of phosphogypsum-red mud filling body based on MICP technology Download PDFInfo
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- CN110683802A CN110683802A CN201911023546.8A CN201911023546A CN110683802A CN 110683802 A CN110683802 A CN 110683802A CN 201911023546 A CN201911023546 A CN 201911023546A CN 110683802 A CN110683802 A CN 110683802A
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B28/00—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- 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
- C04B2111/00724—Uses not provided for elsewhere in C04B2111/00 in mining operations, e.g. for backfilling; in making tunnels or galleries
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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
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/91—Use of waste materials as fillers for mortars or concrete
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Organic Chemistry (AREA)
- Treatment Of Sludge (AREA)
Abstract
The invention discloses a preparation method of a phosphogypsum-red mud filling body based on a MICP technology, which comprises the following steps: (1) culturing the bacillus pasteurii in a liquid culture medium to obtain a bacterial liquid, and preparing a urea solution and a calcium chloride solution to obtain a cementing solution; (2) mixing phosphogypsum and red mud according to a preset proportion, uniformly mixing and slurrying to obtain phosphogypsum-red mud filling slurry; (3) adding a bacterial liquid into the phosphogypsum-red mud filling slurry, uniformly stirring, then adding a urea solution, carrying out aeration treatment, after the reaction is set for a set time, adding a calcium chloride solution, reacting for a preset time, making a test block, and curing to obtain the phosphogypsum-red mud filling body. The invention has simple process, only adds bacteria and cementing liquid once in the whole process, and simplifies the process flow; meanwhile, the urea solution and the calcium chloride solution in the cementing liquid are not added simultaneously, the urea is added firstly for reaction for 2 days, and then the calcium chloride is added for reaction for 3 days, so that the activity of bacteria can be released to the maximum extent, and the cementing strength is enhanced.
Description
Technical Field
The invention belongs to the technical field of filling body preparation, and particularly relates to a preparation method of a phosphogypsum-red mud filling body based on a MICP technology.
Background
When the phosphate rock is used for producing chemical products such as phosphoric acid, phosphate fertilizer and the like, a harmful byproduct is phosphogypsum. P per 1t produced in ore utilization2O5Can be accompanied by 4.4-5.5 t of phosphogypsum. More than 90% of the components in phosphogypsum are calcium sulphate dihydrate (CaSO)4·2H2O), in addition, the phosphorus-containing. The treatment problem of phosphogypsum and the environmental problem generated by the treatment problem become bottlenecks which restrict the development of phosphate fertilizer industry.
Red mud is a harmful waste discharged in the process of producing alumina. In the production process, 1-2.5 tons of red mud can be produced when 1 ton of alumina is produced due to low efficiency. At present, the annual red mud production in China is about 1 hundred million tons, and the accumulated accumulation amount is up to 5 hundred million tons. The red mud is waste residue generated in the process of digesting bauxite by sodium hydroxide at high temperature (106-240 ℃) and pressure (1-6 bar) to generate alumina, so the red mud contains a large amount of strong alkali substances, and the pH value is larger than 11. The red mud is difficult to treat due to high alkalinity and high salinity, and is mostly stockpiled in the open air by building red mud dams; the open-air stockpiling not only occupies a large amount of land and consumes the cost of yard construction and maintenance, but also brings potential safety hazards to surrounding soil bodies and water body environment.
Because the red mud and the phosphogypsum are non-hydraulic materials and have no cementing property, the research on filling only by the red mud and the phosphogypsum is less at present. Conventional cement cementing method, high alkalinity and discharging of cementAmplifying CO2(about 0.8 ton CO per ton cement produced)2) High alkalinity and environmental pollution of the mine environment can be caused. According to researches such as sweet bud and the like, fillers filled with phosphogypsum by traditional cementing materials such as cement and the like are strong in alkalinity, and the dissolution release amount of pollution components is influenced. The cementing filling needs to actively seek a filling material which has low price, wide source, energy conservation and environmental protection as a substitute of cement.
The phosphogypsum-red mud filling body is cemented by using the MICP technology, the filling body generates strength and the mine goaf is filled, so that the resource utilization of two industrial wastes is realized. The application of MICP technology in mine filling is a brand new field, and the Paenibacillus pasteurianus can continuously produce a high-activity urease in the growth and metabolism process, the urease can catalyze the hydrolysis of urea to generate ammonia and carbon dioxide, the ammonia and the carbon dioxide are dispersed into a solution through cell walls, and then the ammonia and the carbon dioxide are rapidly hydrolyzed to generate NH4 +And HCO3 -The exopolymers of the microbial cells and of the products of cellular metabolism adsorb the calcium ions present in the solution, eventually the extracellular Ca2+Calcium carbonate precipitate is formed under the action of (1). Therefore, the cementing capability of microorganisms can be utilized, the red mud-phosphogypsum can be used as filling aggregate, sufficient strength is generated through mineralization, and the filling aggregate is conveyed to a mine goaf.
Disclosure of Invention
Aiming at the problems that the treatment of the phosphogypsum and the red mud is difficult, the direct stockpiling not only occupies a large amount of land, but also brings potential safety hazard to surrounding soil bodies and water body environment, the invention aims to provide the preparation method of the phosphogypsum-red mud filling body based on the MICP technology, which has simple process, low cost and environmental friendliness.
In order to achieve the purpose, the invention provides the following technical scheme: a preparation method of a phosphogypsum-red mud filling body based on the MICP technology comprises the following steps:
(1) culturing the bacillus pasteurii in a liquid culture medium to obtain a bacterial liquid, and preparing a urea solution and a calcium chloride solution to obtain a cementing solution;
(2) mixing phosphogypsum and red mud according to a preset proportion, uniformly mixing and slurrying to obtain phosphogypsum-red mud filling slurry;
(3) adding a bacterial liquid into the phosphogypsum-red mud filling slurry obtained in the step (2), uniformly stirring, then adding a urea solution, carrying out aeration treatment, after the reaction is set for a set time, adding a calcium chloride solution, after the reaction is set for a preset time, making a test block, and curing to obtain the phosphogypsum-red mud filling body.
Preferably, in step (1), the culture medium components and concentrations of the pasteurella: soybean peptone 5 g/L; casein peptone 15 g/L; 5g/L of sodium chloride; then adjusting the pH value to 7.3 +/-0.2 by using 1M NaOH; sterilizing liquid culture medium at 120 deg.C under high temperature and high pressure for 20min, cooling to about 30 deg.C, adding 20g/L urea solution filtered by 0.22um filter, stirring, and inoculating at 1% (V/V); then placing the conical flask on a constant temperature shaking bed at 30 ℃ and carrying out shaking culture at 150rpm for 24-36 h until the OD600 of the bacteria is 1.2-1.5.
Preferably, in the step (1), the ratio of the concentration of the urea solution to the concentration of the calcium chloride solution is 2: 1.
preferably, in the step (2), the red mud and the phosphogypsum are mixed with the total phosphorus gypsum according to the mass ratio of 1: 1-1: 11.
The phosphogypsum used by the invention is fresh phosphogypsum, the pH value is 2.0, more impurities are lower than those of the phosphogypsum (pH value is 6.29) which is piled older, and the fresh phosphogypsum has phosphate and fluoride with higher concentration.
Preferably, in the step (3), the concentration of the phosphogypsum-red mud filling slurry is 40-50%, the bacterial liquid and the cementing liquid (urea solution and calcium chloride solution) are prepared according to the mass ratio of 1:1, and in the cementing liquid, the mass ratio of the urea solution to the calcium chloride solution is 5: 1.
preferably, in the step (3), adding a bacterial liquid into the phosphogypsum-red mud filling slurry, uniformly stirring, then adding a urea solution, aerating in the experimental process, adding a calcium chloride solution after reacting for 2d, reacting for 3d, only adding a bacterial liquid and a cementing liquid in the whole process, then making a test block, maintaining for 7d, and measuring the infinite compressive strength.
Preferably, in the step (3), a toxicity leaching experiment is carried out on the filling body, and the dissolution of toxic and harmful elements is tested.
The invention utilizes the microorganism induced calcium carbonate precipitation (MICP) technology, takes the red mud-phosphogypsum as the filling aggregate, generates enough strength through mineralization, and conveys the filling aggregate to the mined-out area of the mine, and carries out toxicity leaching test to research the leaching condition of harmful substances and heavy metals, and emphatically research the reason of generating the strength and the adsorption mechanism of harmful ions, thereby providing test and theoretical basis for applying the MICP technology cemented phosphogypsum-red mud system to mine filling.
The invention has the beneficial effects that:
(1) the invention has simple process, only adds bacteria and cementing liquid once in the whole process, and simplifies the process flow; meanwhile, the urea solution and the calcium chloride solution in the cementing liquid are not added simultaneously, the urea is added firstly for reaction for 2 days, and then the calcium chloride is added for reaction for 3 days, so that the activity of bacteria can be released to the maximum extent, and the cementing strength is enhanced.
(2) The red mud added in the invention has the advantages that: firstly, the phosphorus-containing phosphate can be neutralized with phosphogypsum, so that a better pH environment can be provided; secondly, the red mud has adsorbability and can adsorb phosphorus and fluorine impurities in the phosphogypsum; thirdly, the red mud and the phosphogypsum have an optimal proportion, so that the MICP technology can generate the maximum strength (the optimal proportion is that the red mud and the phosphogypsum are 1: 11); and fourthly, the red mud belongs to dangerous waste, and the red mud is used as a filling body raw material, so that the problem of reutilization of industrial solid waste is solved.
(3) The maximum strength of the phosphogypsum-red mud filling body prepared by the invention reaches 1290 kpa.
(4) The toxic leaching effect of the phosphogypsum-red mud filling body based on the MICP technology is very good, the sufficient strength is generated through mineralization, the leaching concentration of phosphorus and fluorine is low, and the environment-friendly effect is realized.
Detailed Description
The phosphogypsum used in the embodiment is fresh phosphogypsum, has more impurities and stronger acidity, and the pH value is 2.0.
Example 1
The invention relates to a preparation method of a phosphogypsum-red mud filling body based on a MICP technology, which comprises the following steps:
(1) bacterial liquid culture: the culture medium components and concentration of the pasteuria bacillus are as follows: soybean peptone 5 g/L; casein peptone 15 g/L; 5g/L of sodium chloride; then adjusting the pH value to 7.3 +/-0.2 by using 1M NaOH; sterilizing liquid culture medium at 120 deg.C under high temperature and high pressure for 20min, cooling to about 30 deg.C, adding 20g/L urea solution filtered by 0.22um filter, stirring, and inoculating at 1% (V/V); then placing the conical flask on a constant temperature shaking bed at 30 ℃ and carrying out shaking culture at 150rpm for 24-36 h until the OD600 of bacteria is 1.5;
cementing preparation: preparing 2M urea solution and 1M calcium chloride solution as bacterial cementing solution;
(2) phosphogypsum-red mud filling slurry: the red mud and the phosphogypsum are respectively matched with the total phosphorus gypsum in a ratio of 1: 1-1: 11, the experiment is divided into two groups, and deionized water is added into a control group; the experimental group of the invention is added with bacterial liquid, urea solution and calcium chloride solution;
(3) preparing a filling body: preparing the bacterial liquid and the cementing liquid according to a ratio of 1:1, preparing the cementing liquid according to a ratio of 5:1, and respectively adding 2M urea and 1M calcium chloride;
adding a bacterial liquid into the phosphogypsum-red mud filling slurry, uniformly stirring, then adding a urea solution, aerating in the experimental process, adding a calcium chloride solution after reacting for 2d, reacting for 3d, only adding a primary bacterial liquid and a cementing solution in the experimental process, then making a test block, and maintaining for 7d to obtain the phosphogypsum-red mud filling body.
Example 2
Phosphogypsum (PG) -Red Mud (RM) filling slurry phosphorus-fluorine concentration change: in the bacterial liquid reaction 5d, every 24h, the supernatant liquid is taken and filtered, and then fluorine and phosphorus in the slurry solution are measured, and the results are shown in table 1:
TABLE 1 phosphorus concentration (mg/L) in slurry solution
TABLE 2 fluoride ion concentration (mg/L) in the slurry solution
As can be seen from Table 1 and Table 2, the MICP technique has significant adsorption effect on fluorine and phosphorus, as the concentration of phosphorus and fluorine in the slurry changes.
Example 3
Change of filling strength: and testing the infinite pressure measurement intensity of the test block which is reacted for 5 days and maintained for 7 days, and detecting whether the intensity meets the filling requirement. The unconfined compressive strength of the filled sample was tested using a conventional 10kN rock servo tester. The test piece was placed in the center of a pressure plate of a compression testing machine and each set of samples was loaded until failure using a loading rate of 0.5 mm/min.
TABLE 3 filling Strength
As can be seen from table 3, the strength was significantly increased in the experimental group with red mud added, especially in the case of red mud: the ratio of the phosphogypsum to the phosphogypsum is 1:11, the strength reaches 1290kpa to the maximum, and the requirement of filling is completely met. In contrast, in the control group, the phosphogypsum and the red mud are both non-hydraulic, so that the cementing strength is not high, and the strength cannot meet the filling requirement. Therefore, the strength can be better enhanced by adding the microorganisms and the red mud.
Example 4
Toxicity leaching experiment: taking the filling body dried at the temperature of 55 ℃, sieving the filling body and then preparing the filling body into a liquid: calculating and weighing the volume of the required leaching agent deionized water and the mass of the phosphogypsum as 10:1(L/kg), respectively adding the required leaching agent deionized water and the phosphogypsum into a polyethylene bottle, stirring the materials to uniformly mix the materials, and carrying out three groups of parallel tests on each group of tests to obtain an average value; tightly covering the bottle cap and fixing the bottle cap on a horizontal oscillator, setting the speed at 110 +/-10 times/min and the amplitude at 40mm, and oscillating for 8 hours at room temperature and then taking down the bottle cap; standing for 16h, filtering supernatant with 0.22 μm needle filter, drying solid phase, standing in a drier, collecting all filtrate, and performing chemical analysis on water quality.
TABLE 4 toxicity Leaching Experimental analysis (mg/L)
As can be seen from the data in table 4, after adding red mud and microorganisms (experimental group), the concentrations of phosphorus and fluorine in the toxicity leaching test were both lower than those in the control group, and the larger the amount of red mud added, the lower the concentration of fluorine.
While the above description is directed to the preferred embodiments of the present invention, it is intended that the present invention shall not be limited to the particular embodiments described. For the person skilled in the art to which the present invention pertains, variations and modifications of the above-described embodiments may be made, and such variations and modifications may fall within the scope of the appended claims without departing from the spirit of the present invention.
Claims (7)
1. A preparation method of a phosphogypsum-red mud filling body based on the MICP technology is characterized by comprising the following steps:
(1) culturing the bacillus pasteurii in a liquid culture medium to obtain a bacterial liquid, and preparing a urea solution and a calcium chloride solution to obtain a cementing solution;
(2) mixing phosphogypsum and red mud according to a preset proportion, uniformly mixing and slurrying to obtain phosphogypsum-red mud filling slurry;
(3) adding a bacterial liquid into the phosphogypsum-red mud filling slurry obtained in the step (2), uniformly stirring, then adding a urea solution, carrying out aeration treatment, after the reaction is set for a set time, adding a calcium chloride solution, after the reaction is set for a preset time, making a test block, and curing to obtain the phosphogypsum-red mud filling body.
2. The MICP technology-based preparation method of phosphogypsum-red mud filling mass according to claim 1, wherein in the step (1), the culture medium components and concentrations of Paenibacillus pasteurianus are as follows: soybean peptone 5 g/L; casein peptone 15 g/L; 5g/L of sodium chloride; then adjusting the pH value to 7.3 +/-0.2 by using 1M NaOH; sterilizing liquid culture medium at 120 deg.C under high temperature and high pressure for 20min, cooling to about 30 deg.C, adding 20g/L urea solution filtered by 0.22um filter, stirring, and inoculating at 1% (V/V); then placing the conical flask on a constant temperature shaking bed at 30 ℃ and carrying out shaking culture at 150rpm for 24-36 h until the OD600 of the bacteria is 1.2-1.5.
3. The MICP technology-based phosphogypsum-red mud filling body preparation method according to claim 1, wherein in the step (1), the ratio of the concentration of the urea solution to the concentration of the calcium chloride solution is 2: 1.
4. the preparation method of the phosphogypsum-red mud filling body based on the MICP technology as claimed in claim 1, wherein in the step (2), the red mud and the phosphogypsum are respectively mixed with the total phosphogypsum according to the mass ratio of 1: 1-1: 11.
5. The preparation method of the phosphogypsum-red mud filling body based on the MICP technology as claimed in claim 1, wherein in the step (3), the concentration of the phosphogypsum-red mud filling slurry is 40-50%, the bacterial liquid and the cementing liquid are prepared according to the mass ratio of 1:1, and in the cementing liquid, the mass ratio of the urea solution to the calcium chloride solution is 5: 1.
6. the preparation method of the phosphogypsum-red mud filling body based on the MICP technology as claimed in claim 1, wherein in the step (3), the bacterial liquid is added into the phosphogypsum-red mud filling slurry, the urea solution is added after the mixture is uniformly stirred, the aeration is carried out in the experimental process, the calcium chloride solution is added after the reaction lasts for 2d, the reaction lasts for 3d, only the primary bacterial liquid and the cementing liquid are added in the whole process, then the test block is manufactured, the maintenance lasts for 7d, and the infinite compressive strength is measured.
7. The preparation method of the phosphogypsum-red mud filling body based on the MICP technology as claimed in claim 1, wherein in the step (3), a toxicity leaching experiment is carried out on the filling body to test the dissolution condition of toxic and harmful elements.
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Cited By (7)
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| CN111424689A (en) * | 2020-04-20 | 2020-07-17 | 中国科学院地质与地球物理研究所 | Protection method for improving soil slope resistance to rainwater erosion by adopting phosphogypsum and microorganisms |
| CN111424484A (en) * | 2020-04-20 | 2020-07-17 | 中国科学院地质与地球物理研究所 | Construction method for reinforcing loess embankment by combining microbial mineralization and phosphogypsum |
| CN111424687A (en) * | 2020-04-20 | 2020-07-17 | 中国科学院地质与地球物理研究所 | Construction method for ecological protection of expansive soil side slope by using phosphogypsum and microbial mineralization technology |
| CN112122331A (en) * | 2020-08-31 | 2020-12-25 | 南京林业大学 | Method for solidifying and stabilizing heavy metal polluted soil |
| CN112125574A (en) * | 2020-09-30 | 2020-12-25 | 华中科技大学 | Method for improving mechanical properties of microbial cemented sand by using protein cementing material |
| CN114149244A (en) * | 2021-12-10 | 2022-03-08 | 临沂海螺新材料科技有限公司 | Method for preparing red mud building material product based on composite microbial technology |
| CN114751685A (en) * | 2022-05-11 | 2022-07-15 | 辽宁工程技术大学 | MICP principle-based ecological solid carbon filling material and preparation method thereof |
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| CN111424689A (en) * | 2020-04-20 | 2020-07-17 | 中国科学院地质与地球物理研究所 | Protection method for improving soil slope resistance to rainwater erosion by adopting phosphogypsum and microorganisms |
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| CN112125574A (en) * | 2020-09-30 | 2020-12-25 | 华中科技大学 | Method for improving mechanical properties of microbial cemented sand by using protein cementing material |
| CN112125574B (en) * | 2020-09-30 | 2021-08-20 | 华中科技大学 | Method for improving mechanical properties of microbial cemented sand by using protein cementing material |
| CN114149244A (en) * | 2021-12-10 | 2022-03-08 | 临沂海螺新材料科技有限公司 | Method for preparing red mud building material product based on composite microbial technology |
| CN114751685A (en) * | 2022-05-11 | 2022-07-15 | 辽宁工程技术大学 | MICP principle-based ecological solid carbon filling material and preparation method thereof |
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