CN116375444A - Preparation method of improved phosphogypsum-microorganism cement filler - Google Patents
Preparation method of improved phosphogypsum-microorganism cement filler Download PDFInfo
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- CN116375444A CN116375444A CN202310422561.XA CN202310422561A CN116375444A CN 116375444 A CN116375444 A CN 116375444A CN 202310422561 A CN202310422561 A CN 202310422561A CN 116375444 A CN116375444 A CN 116375444A
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- 239000004568 cement Substances 0.000 title claims abstract description 38
- 238000002360 preparation method Methods 0.000 title claims abstract description 34
- 239000000945 filler Substances 0.000 title claims description 24
- PASHVRUKOFIRIK-UHFFFAOYSA-L calcium sulfate dihydrate Chemical compound O.O.[Ca+2].[O-]S([O-])(=O)=O PASHVRUKOFIRIK-UHFFFAOYSA-L 0.000 claims abstract description 82
- 239000002002 slurry Substances 0.000 claims abstract description 53
- 238000011049 filling Methods 0.000 claims abstract description 40
- 239000007788 liquid Substances 0.000 claims abstract description 29
- USFZMSVCRYTOJT-UHFFFAOYSA-N Ammonium acetate Chemical compound N.CC(O)=O USFZMSVCRYTOJT-UHFFFAOYSA-N 0.000 claims abstract description 26
- 239000005695 Ammonium acetate Substances 0.000 claims abstract description 26
- 229940043376 ammonium acetate Drugs 0.000 claims abstract description 26
- 235000019257 ammonium acetate Nutrition 0.000 claims abstract description 26
- 238000002156 mixing Methods 0.000 claims abstract description 25
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 23
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 22
- 239000004202 carbamide Substances 0.000 claims abstract description 22
- 230000001580 bacterial effect Effects 0.000 claims abstract description 20
- 238000012360 testing method Methods 0.000 claims abstract description 20
- 238000006243 chemical reaction Methods 0.000 claims abstract description 11
- 230000035484 reaction time Effects 0.000 claims abstract description 7
- 241000193830 Bacillus <bacterium> Species 0.000 claims abstract description 4
- 230000003213 activating effect Effects 0.000 claims abstract description 3
- 238000012258 culturing Methods 0.000 claims abstract description 3
- 230000000035 biogenic effect Effects 0.000 claims description 20
- 238000000034 method Methods 0.000 claims description 14
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- 239000001963 growth medium Substances 0.000 claims description 5
- 238000009630 liquid culture Methods 0.000 claims description 4
- 235000010469 Glycine max Nutrition 0.000 claims description 3
- 244000068988 Glycine max Species 0.000 claims description 3
- 239000001888 Peptone Substances 0.000 claims description 3
- 108010080698 Peptones Proteins 0.000 claims description 3
- 235000019319 peptone Nutrition 0.000 claims description 3
- 108010009004 proteose-peptone Proteins 0.000 claims description 3
- 239000011780 sodium chloride Substances 0.000 claims description 3
- 239000002609 medium Substances 0.000 claims description 2
- 230000010355 oscillation Effects 0.000 claims description 2
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 abstract description 32
- 229910000019 calcium carbonate Inorganic materials 0.000 abstract description 16
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 238000005065 mining Methods 0.000 abstract description 2
- 230000000052 comparative effect Effects 0.000 description 8
- 241000894006 Bacteria Species 0.000 description 7
- 239000013078 crystal Substances 0.000 description 7
- 239000000203 mixture Substances 0.000 description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- 239000008367 deionised water Substances 0.000 description 4
- 229910021641 deionized water Inorganic materials 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000001879 gelation Methods 0.000 description 3
- 238000002386 leaching Methods 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 239000002910 solid waste Substances 0.000 description 3
- BHPQYMZQTOCNFJ-UHFFFAOYSA-N Calcium cation Chemical compound [Ca+2] BHPQYMZQTOCNFJ-UHFFFAOYSA-N 0.000 description 2
- 238000009825 accumulation Methods 0.000 description 2
- 229910001424 calcium ion Inorganic materials 0.000 description 2
- 244000005700 microbiome Species 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- 238000004064 recycling Methods 0.000 description 2
- 239000013049 sediment Substances 0.000 description 2
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 1
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 241000193395 Sporosarcina pasteurii Species 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000033558 biomineral tissue development Effects 0.000 description 1
- 230000015271 coagulation Effects 0.000 description 1
- 238000005345 coagulation Methods 0.000 description 1
- 239000003349 gelling agent Substances 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 238000011081 inoculation Methods 0.000 description 1
- 239000002054 inoculum Substances 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000004060 metabolic process Effects 0.000 description 1
- 230000000813 microbial effect Effects 0.000 description 1
- 230000006911 nucleation Effects 0.000 description 1
- 238000010899 nucleation Methods 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 238000007781 pre-processing Methods 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 239000011241 protective layer Substances 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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Classifications
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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
- C04B28/34—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 cold phosphate binders
- C04B28/344—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 cold phosphate binders the phosphate binder being present in the starting composition solely as one or more phosphates
-
- 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
-
- 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)
- Biological Treatment Of Waste Water (AREA)
Abstract
The invention discloses a preparation method of an improved phosphogypsum-microorganism cement filling body, which comprises the following steps: 1) Activating and culturing the bacillus pasteurizer to obtain bacterial liquid; preparing urea and bacterial liquid, and uniformly mixing to obtain a biological gelatinizing agent; 2) Pre-treating phosphogypsum by using ammonium acetate solution to obtain phosphogypsum pre-treated slurry; 3) Mixing biological gelatinizer and phosphogypsum pretreated slurry for reaction to obtain modified phosphogypsum slurry; 4) And filling the modified phosphogypsum slurry into test blocks, and curing to obtain the modified phosphogypsum-microorganism cement filling body. According to the invention, the novel phosphogypsum-microorganism cement bond filling body is improved, and after the phosphogypsum is pretreated by using ammonium acetate, the morphology of calcium carbonate in the prepared filling body is changed, so that the mechanical property of the filling body is improved, the reaction time is shortened, the production efficiency is improved, and the mining cost is reduced.
Description
Technical Field
The invention belongs to the technical field of filler preparation, and particularly relates to a preparation method of an improved phosphogypsum-microorganism cement filler.
Background
Microbial induced calcium carbonate precipitation (MICP) technology has made great progress in the field of mine geotechnical engineering. The principle is that the metabolism of microorganism itself is utilized to hydrolyze urea to generate carbonate ions, and calcium carbonate sediment with cementing property is generated by mineralization, which can be used as a novel biological cement with mechanical property. Phosphogypsum is solid waste generated in the field of phosphorus chemical industry, and because phosphogypsum contains harmful components such as phosphide, fluoride, heavy metal and the like, a large amount of accumulation at present has huge damage to environments such as water, soil and the like. Aiming at the recycling utilization of phosphogypsum solid waste, a novel phosphogypsum-microorganism cement cemented filling method is proposed at present, namely calcium carbonate sediment generated by using MICP technology is used as microorganism cement, and phosphogypsum is cemented into a strong whole to meet the requirement of mine filling. The method realizes the aim of secondary recycling of solid waste, but the performance of the filling body is easily influenced by factors such as bacteria, pH, nucleation sites and the like, and finally the problems of slow coagulation rate, to-be-improved strength and the like of the filling body are caused, so that phosphogypsum-microorganism cement needs to be further improved in the aspects of strength, gelation speed and the like.
Disclosure of Invention
The invention aims to provide a preparation method of an improved phosphogypsum-microorganism cement filling body, which ensures that the strength of the prepared filling body is higher and the gelation speed of the filling body is higher.
In order to achieve the technical purpose, the invention provides the following technical scheme:
the preparation method of the modified phosphogypsum-microorganism cement filling body provided by the invention comprises the following steps:
1) Preparation of the biogenic agent: activating the bacillus pasteurizer, and culturing in a liquid culture medium to obtain a bacterial liquid; mixing urea and bacterial liquid in proportion, and obtaining biological gelatinizing agent;
2) Phosphogypsum pretreatment slurry preparation: uniformly mixing phosphogypsum and ammonium acetate solution according to a set proportion, reacting under the conditions of constant temperature and vibration, and obtaining phosphogypsum pretreatment slurry after the reaction is finished;
3) Preparation of modified phosphogypsum slurry: uniformly mixing the biogenic agent in the step 1) with the phosphogypsum pretreatment slurry in the step 2), reacting at a constant temperature, stirring and aerating at intervals of set time, and obtaining improved phosphogypsum slurry after the reaction is finished;
4) Preparation of modified phosphogypsum-microorganism cement filler: and (3) filling the modified phosphogypsum slurry obtained in the step (3) into test blocks, and curing to obtain the modified phosphogypsum-microorganism cement filling body.
Preferably, in the step 1), the liquid medium contains 15g/L casein peptone, 5g/L soybean peptone and 5g/L sodium chloride, and the pH is 7.0 to 8.0.
Preferably, in the step 1), the OD600 value of the bacterial liquid is 2 to 3.
Preferably, in the step 1), the mass ratio of the bacterial liquid to urea is 100: (6-9), namely, the concentration of urea in the biogenic agent is 1-1.5 mol/L.
Preferably, in the step 2), the concentration of the ammonium acetate solution is 1 to 4mol/L; the solid-to-liquid ratio of phosphogypsum to ammonium acetate solution is 1g: (1-0.8) mL.
Preferably, in the step 2), the oscillation rate is 200-220 r/min, the reaction temperature is 70-90 ℃, and the reaction time is 50-60 min.
Preferably, in the step 3), the phosphogypsum pretreatment slurry and the biogenic agent are prepared according to phosphogypsum: bacterial liquid: the mass ratio of urea is 100:100: (6-9) mixing.
Preferably, in the step 3), the reaction temperature is 25-30 ℃, the reaction time is 3-96 h, and the slurry is stirred and aerated every 6 h.
Preferably, in the step 4), the curing temperature is 25-30 ℃ and the curing time is 7-28 d; the modified phosphogypsum-microorganism cement filler was subjected to an infinite compressive strength test.
The invention has the beneficial effects that:
the invention relates to an improvement of a novel phosphogypsum-microorganism cement bond filler, which is characterized in that ammonium acetate is used for preprocessing phosphogypsum to change the morphology of calcium carbonate in the prepared filler, thereby improving the mechanical property of the filler. The strength of the modified phosphogypsum-microorganism cement filling body prepared by the invention is up to 4.15MPa. Meanwhile, the method can shorten the reaction time of preparing phosphogypsum-microorganism cement filler by the MICP technology, and improve the production efficiency, thereby reducing the mining cost.
Drawings
FIG. 1 is a graph of the calcium carbonate morphology at 1000-fold magnification of example 3;
fig. 2 is a graph of the calcium carbonate morphology at 1000 x magnification of the comparative example.
Detailed Description
Phosphogypsum used in the following examples is fresh phosphogypsum and has a pH of 4.0.
Example 1
(1) Preparation of the biogenic agent: the liquid culture medium of Bacillus pasteurii contained 15g/L casein peptone, 5g/L soybean peptone, 5g/L sodium chloride, and was adjusted to pH 7.3 with 1mol/L NaOH. The culture medium was sterilized at 120℃and naturally cooled, and then 20g/L urea solution filtered with a 0.22 μm filter was added thereto, and Bacillus pasteurizer was removed at 1% inoculum size (V/V) and inoculated into the liquid culture medium. After inoculation, the bacteria are cultured on a shaking table at a constant temperature of 30 ℃ for 24 hours at 150rpm, so that the required bacteria liquid is obtained, and the OD600 value of the bacteria liquid is measured to be 2.133. According to the mass ratio of 100: and 9, preparing bacterial liquid and urea, and uniformly mixing to obtain the biological gelling agent.
(2) Phosphogypsum pretreatment slurry preparation: phosphogypsum and 1mol/L ammonium acetate solution are mixed according to a solid-to-liquid ratio of 1g: mixing 1mL, placing into a constant-temperature oscillating box at 80 ℃ after mixing uniformly, oscillating at 200r/min, and leaching for 60min to obtain phosphogypsum pretreatment slurry.
(3) Preparation of modified phosphogypsum slurry: uniformly mixing biogenic agent (wherein, the concentration of urea is 1.5 mol/L) and phosphogypsum pretreatment slurry, wherein, phosphogypsum: bacterial liquid: the mass ratio of urea is 100:100:9, then placing the mixture into a 30 ℃ incubator to react for 96 hours, and stirring and aerating the slurry every 6 hours to obtain the modified phosphogypsum slurry.
(4) Preparation of modified phosphogypsum-microorganism cement filler: and filling phosphogypsum slurry into test blocks, curing for 7 days at a curing temperature of 25-30 ℃ to obtain the improved phosphogypsum-microorganism cement filling body.
Example 2
This example is essentially the same as example 1 except that the 1mol/L ammonium acetate solution is changed to 2mol/L ammonium acetate solution, and the remainder is unchanged.
Example 3
This example is essentially the same as example 1 except that the 1mol/L ammonium acetate solution is changed to 4mol/L ammonium acetate solution, the remainder being unchanged.
The 1000-fold enlarged morphology of calcium carbonate in the modified phosphogypsum-microorganism cement filler prepared in the embodiment is shown in figure 1.
Comparative example 1
(1) Preparation of the biogenic agent: step (1) was performed as in example 1.
(2) Preparing phosphogypsum slurry: mixing biogenic agent (wherein, the concentration of urea is 1.5 mol/L) and phosphogypsum with deionized water according to a set proportion, wherein, phosphogypsum: deionized water: bacterial liquid: the mass ratio of urea is 100:100:100:9, uniformly mixing, then placing the mixture into a 30 ℃ incubator to react for 96 hours, and stirring and aerating the slurry every 6 hours to obtain phosphogypsum slurry.
(3) Preparation of phosphogypsum-microorganism cement filler: and filling phosphogypsum slurry into test blocks, curing for 7 days at the curing temperature of 25-30 ℃ to obtain phosphogypsum-microorganism cement filling bodies, and measuring the maximum uniaxial compressive strength.
The enlarged 1000-fold morphology graph of calcium carbonate in phosphogypsum-microorganism cement filler prepared in the comparative example is shown in figure 2.
FIG. 1 shows the morphology of calcium carbonate at a magnification of 1000 times after addition of 4mol/L ammonium acetate solution in example 3. The calcium carbonate crystal has needle-like and spherical shape, the particle size is increased, and a protective layer is formed on the surface of phosphogypsum. The addition of ammonium acetate promotes the increase of calcium ions in the system, the surface of bacteria is negatively charged, and the positively charged calcium ions are continuously accumulated on the surface of bacteria, and the bacteria are easily adsorbed on the smaller surface, so that the partial supersaturation state is formed near the mutual contact of phosphogypsum particles, the accumulation of calcium carbonate crystal nucleus occurs, and the crystal nucleus continuously grows from beginning to grow to form visible crystals. The whole process forms effective calcium carbonate precipitation, and phosphogypsum particles can be glued into a whole with certain mechanical properties.
Fig. 2 shows the morphology of comparative example 1 at 1000 x magnification of calcium carbonate without ammonium acetate. The calcium carbonate crystals are spherical, but are distributed more dispersedly and attached to the surface of phosphogypsum, the growth among the crystals is not interfered with each other, the phenomenon of agglomeration and overlapping is hardly seen, most of the calcium carbonate crystals are invalid glue, and the whole with good mechanical properties cannot be formed better.
The maximum uniaxial compressive strength of the fillers prepared in examples 1, 2 and 3 and comparative examples was measured and the specific test analysis was as follows:
the filling body is subjected to unconfined compressive strength test by adopting a conventional 10kN microcomputer control pressure testing machine. And placing the filling body test block at the middle position of a lower pressing plate of the pressure testing machine, and pressurizing the filling body test block by using a loading rate of 0.5mm/min until deformation of the filling body test block is destroyed.
The specific test results are shown in table 1.
TABLE 1 compressive Strength results of phosphogypsum-microbial Cement Filler
As is clear from the data in Table 1, when phosphogypsum is pretreated by using ammonium acetate solution, the strength of the prepared filling body is gradually increased along with the increase of the concentration of the ammonium acetate solution, and the strength can reach 4.15MPa when the concentration is 4mol/L, and compared with the comparative example, the strength is increased by 180%.
Example 4
(1) Preparation of the biogenic agent: step (1) was performed as in example 1.
(2) Phosphogypsum pretreatment slurry preparation: phosphogypsum is pretreated by using 1mol/L, 2mol/L and 4mol/L ammonium acetate solutions respectively according to the method of the step (2) of the example 1, so as to obtain different phosphogypsum pretreated slurries.
(3) Preparation of modified phosphogypsum slurry: the biogenic agent and different phosphogypsum pretreatment slurries are respectively mixed and reacted according to the method in the step (3) of the example 1, and the rest conditions are unchanged, but the reaction time is respectively 3 hours and 24 hours, so that different modified phosphogypsum slurries are obtained.
(4) Preparation of modified phosphogypsum-microorganism cement filler: and (3) respectively filling the different modified phosphogypsum slurries into test blocks, curing for 7d at the curing temperature of 25-30 ℃ to obtain the different modified phosphogypsum-microorganism cement filling bodies.
The maximum uniaxial compressive strength was measured for different modified phosphogypsum-microbial cement fills. The specific test results are shown in table 2.
Comparative example 2
(1) Preparation of the biogenic agent: step (1) was performed as in example 1.
(2) Preparing phosphogypsum slurry: mixing biogenic agent (wherein, the concentration of urea is 1.5 mol/L) and phosphogypsum with deionized water according to a set proportion, wherein, phosphogypsum: deionized water: bacterial liquid: the mass ratio of urea is 100:100:100:9, after being uniformly mixed, the mixture is put into a constant temperature box at 30 ℃ to react for 3 hours and 24 hours respectively, and the slurry is stirred and aerated every 6 hours after the reaction for 24 hours, so that different phosphogypsum slurries are obtained.
(3) Preparation of phosphogypsum-microorganism cement filler: and (3) respectively filling the different phosphogypsum slurries into test blocks, curing for 7d at the curing temperature of 25-30 ℃ to respectively obtain different phosphogypsum-microorganism cement fillers, and measuring the maximum uniaxial compressive strength. The specific test results are shown in table 2.
TABLE 2 compressive Strength results of phosphogypsum-microbial Cement Filler
As can be seen from the data in Table 2, comparative example 2 was conducted for 3 hours without adding an ammonium acetate solution, and the strength of the resulting filler was only 0.50MPa; the strength of the filling body is improved after the phosphogypsum is pretreated by the ammonium acetate solution for 3 hours, and particularly, the strength of the filling body can reach 3.77MPa after the phosphogypsum is pretreated by the ammonium acetate solution for 3 hours, so that the requirement of mine filling strength is met, and therefore, after the phosphogypsum is pretreated by the ammonium acetate solution, the gelation time can be effectively shortened, and the filling efficiency can be improved.
Example 5
(1) Preparation of the biogenic agent: substantially the same as in the step (1) of example 1, except that the mass ratio of the bacterial liquid to urea was 100:8, 8;
(2) Phosphogypsum pretreatment: phosphogypsum and 4mol/L ammonium acetate solution are mixed according to a solid-to-liquid ratio of 1g: mixing 0.8mL, placing into a constant temperature oscillating box at 90 ℃ after mixing uniformly, oscillating at 220r/min, and leaching for 50min to obtain phosphogypsum pretreatment slurry.
(3) Preparation of modified phosphogypsum slurry: uniformly mixing biogenic agent and phosphogypsum pretreatment slurry, wherein phosphogypsum: bacterial liquid: the mass ratio of urea is 100:100:8, uniformly mixing, then placing the mixture into a 30 ℃ incubator to react for 96 hours, and stirring and aerating the slurry every 6 hours to obtain the modified phosphogypsum slurry.
(4) Preparation of modified phosphogypsum-microorganism cement filler: and filling the modified phosphogypsum slurry into test blocks, curing for 14 days at a curing temperature of 25-30 ℃ to obtain the modified phosphogypsum-microorganism cement filling body.
Example 6
(1) Preparation of the biogenic agent: substantially the same as in the step (1) of example 1, except that the mass ratio of the bacterial liquid to urea was 100:6, preparing a base material;
(2) Phosphogypsum pretreatment: phosphogypsum and 4mol/L ammonium acetate solution are mixed according to a solid-to-liquid ratio of 1g: mixing 0.9mL, placing into a constant temperature oscillating box at 70 ℃ after mixing uniformly, oscillating at 210r/min, leaching for 55min, and obtaining phosphogypsum pretreatment slurry.
(3) Preparation of modified phosphogypsum slurry: uniformly mixing biogenic agent and phosphogypsum pretreatment slurry, wherein phosphogypsum: bacterial liquid: the mass ratio of urea is 100:100:6, uniformly mixing, then placing the mixture into a constant temperature box at 25 ℃ for reaction for 96 hours, and stirring and aerating the slurry every 6 hours to obtain the modified phosphogypsum slurry.
(4) Preparation of modified phosphogypsum-microorganism cement filler: and filling the modified phosphogypsum slurry into test blocks, curing for 28 days at a curing temperature of 25-30 ℃ to obtain the modified phosphogypsum-microorganism cement filling body.
Claims (9)
1. The preparation method of the modified phosphogypsum-microorganism cement filling body comprises the following steps:
1) Preparation of the biogenic agent: activating the bacillus pasteurizer, and culturing in a liquid culture medium to obtain a bacterial liquid; mixing urea and bacterial liquid in proportion, and obtaining biological gelatinizing agent;
2) Preparation of phosphogypsum pretreatment slurry: uniformly mixing phosphogypsum and ammonium acetate solution according to a set proportion, reacting under the conditions of constant temperature and vibration, and obtaining phosphogypsum pretreatment slurry after the reaction is finished;
3) Preparation of modified phosphogypsum slurry: uniformly mixing the biogenic agent in the step 1) with the phosphogypsum pretreatment slurry in the step 2), reacting at a constant temperature, stirring and aerating at intervals of set time, and obtaining improved phosphogypsum slurry after the reaction is finished;
4) Preparation of modified phosphogypsum-microorganism cement filler: and (3) filling the modified phosphogypsum slurry obtained in the step (3) into test blocks, and curing to obtain the modified phosphogypsum-microorganism cement filling body.
2. The method according to claim 1, wherein in the step 1), the liquid medium contains 15g/L casein peptone, 5g/L soybean peptone and 5g/L sodium chloride, and the pH is 7.0 to 8.0.
3. The method according to claim 1, wherein in the step 1), the OD600 value of the bacterial liquid is 2 to 3.
4. The method according to claim 1, wherein in the step 1), the mass ratio of the bacterial liquid to the urea is 100: (6-9), namely, the concentration of urea in the biogenic agent is 1-1.5 mol/L.
5. The method according to claim 1, wherein in the step 2), the concentration of the ammonium acetate solution is 1 to 4mol/L; the solid-to-liquid ratio of phosphogypsum to ammonium acetate solution is 1g: (1-0.8) mL.
6. The method according to claim 1, wherein in the step 2), the oscillation rate is 200-220 r/min, the reaction temperature is 70-90 ℃, and the reaction time is 50-60 min.
7. The method according to claim 1, wherein in the step 3), phosphogypsum pretreatment slurry and biogenic agent are prepared according to phosphogypsum: bacterial liquid: the mass ratio of urea is 100:100: (6-9) mixing.
8. The method according to claim 1, wherein in the step 3), the reaction temperature is 25 to 30 ℃, the reaction time is 3 to 96 hours, and the slurry is stirred and aerated every 6 hours.
9. The method according to claim 1, wherein in the step 4), the curing temperature is 25 to 30 ℃ and the curing time is 7 to 28d.
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| CN109485367A (en) * | 2019-01-07 | 2019-03-19 | 中南大学 | A kind of preparation method and application of filling phosphorous gypsum body |
| CN111777089A (en) * | 2019-04-04 | 2020-10-16 | 西南科技大学 | Preparation method of high-purity vaterite type calcium carbonate microspheres |
| CN112441606A (en) * | 2019-08-28 | 2021-03-05 | 西南科技大学 | Method for separating valuable components from calcium sulfate raw material and co-producing calcium carbonate |
| CN113800546A (en) * | 2021-09-28 | 2021-12-17 | 中国科学院山西煤炭化学研究所 | CO (carbon monoxide)2Method for preparing micro-nano calcium carbonate by mineralizing calcium-containing solid waste residues |
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| CN107954623A (en) * | 2017-11-17 | 2018-04-24 | 东南大学 | A kind of preparation method of solid waste surface in situ growth nano particle |
| CN109485367A (en) * | 2019-01-07 | 2019-03-19 | 中南大学 | A kind of preparation method and application of filling phosphorous gypsum body |
| CN111777089A (en) * | 2019-04-04 | 2020-10-16 | 西南科技大学 | Preparation method of high-purity vaterite type calcium carbonate microspheres |
| CN112441606A (en) * | 2019-08-28 | 2021-03-05 | 西南科技大学 | Method for separating valuable components from calcium sulfate raw material and co-producing calcium carbonate |
| CN113800546A (en) * | 2021-09-28 | 2021-12-17 | 中国科学院山西煤炭化学研究所 | CO (carbon monoxide)2Method for preparing micro-nano calcium carbonate by mineralizing calcium-containing solid waste residues |
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