CN111191387A - Phosphogypsum-based cementing material optimization method for improving filling roof contact rate - Google Patents
Phosphogypsum-based cementing material optimization method for improving filling roof contact rate Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B28/00—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements
- C04B28/14—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements containing calcium sulfate cements
- C04B28/142—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements containing calcium sulfate cements containing synthetic or waste calcium sulfate cements
- C04B28/143—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements containing calcium sulfate cements containing synthetic or waste calcium sulfate cements the synthetic calcium sulfate being phosphogypsum
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N3/00—Investigating strength properties of solid materials by application of mechanical stress
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
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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
Abstract
The invention discloses an optimization method of an ardealite-based cementing material for improving a filling roof contact rate, which is characterized in that ardealite powder and an excitant in different proportions are added into a filling aggregate to prepare cementing filling body materials in different proportions; carrying out a strength test and a filling body expansion rate test on the cemented filling body materials with different proportions to obtain test data of the strength and the expansion rate of the cemented filling body materials with different proportions; performing stepwise regression analysis on the test data of the strength and the expansion rate of the cemented filling body by using a quadratic polynomial; establishing a proportioning optimization model of the cementing material by taking the 3d strength of the cemented filling body as an optimization target and taking the expansion rate of the 28d filling body as a constraint condition; and solving the optimization model to obtain the optimized proportion of the phosphogypsum-based cementing material in the filling slurry. The design method can realize low-cost and high-value resource utilization of the phosphogypsum; the phosphogypsum can be used in filling mining with low cost and high value.
Description
Technical Field
The invention belongs to the technical field of filling mining, and particularly relates to an optimization method of a phosphogypsum-based cementing material for improving a filling roof contact rate.
Background
With the rapid development of national economy and the continuous development of resources, resources with high grade and good conditions are gradually exhausted, and more difficult-to-mine ore bodies with deep burial depth, large ground pressure, rich water and the like are faced to be exploited. For safe, environment-friendly and green mining, a filling mining method is the primary choice. Particularly for complex and difficult-to-mine ore bodies of weak broken surrounding rocks, safety operation can be realized only by protecting under a filling body false roof, so that a downward layered filling mining method is the only option. The stoping process of the filling mining method is complex, the production capacity is low, and the mining cost is high. In order to improve the production capacity, the requirement on the early strength of the filling body is high, the mining economic benefit is poorer, and enterprises face huge pressure.
The harmful mineral components in the phosphogypsum cause low activity, poor gelling property and unstable volume, thus leading the utilization rate of the phosphogypsum to be less than 5 percent. Exploring the resource utilization way of the phosphogypsum is not slow at all. The phosphogypsum is used for developing the filling cementing material, so that the filling cost can be reduced, and the utilization rate of phosphogypsum solid waste resources can be improved. Especially, the instability of the phosphogypsum can also reduce the shrinkage rate of a filling body and improve the roof-contacting rate of a filling stope. However, studies show that instability of phosphogypsum leads to deterioration of strength, and the instability of phosphogypsum is one of the main problems facing the utilization of phosphogypsum. Therefore, the problem of strength deterioration of improving the early strength of the phosphogypsum and controlling the volume expansion is a key technology for recycling the solid waste of the phosphogypsum.
The Chinese invention patent CN106478041A discloses a preparation method of an early-strength phosphogypsum-based cementing material; the phosphogypsum is dried, crushed, sieved, mixed and ground with ammonia water, then treated with acid such as sulfuric acid solution and the like, stood for impurity removal, ball-milled, filtered, dried and calcined to prepare the pre-treated phosphogypsum, and finally mixed with blast furnace slag, Portland cement, polyaluminium chloride and other substances, thereby preparing the early-strength phosphogypsum-based cementing material. CN106630711B invented a method for preparing modified phosphogypsum cementing material by using phosphogypsum; washing and standing phosphogypsum, adding PAM to remove suspended matters, finally precipitating, dehydrating and drying, and crushing and ball-milling mature phosphogypsum powder; then mixing with phosphorus tailings to obtain modified phosphogypsum, and adding an additive to obtain the modified phosphogypsum cementing material, thereby improving the strength and removing instability of the modified phosphogypsum cementing material. CN108002724A discloses a method for preparing a phosphogypsum-based cementing material by two-step calcination; the phosphogypsum is deeply purified by washing and pickling the phosphogypsum, so that the influence of impurities on the calcining of the phosphogypsum is avoided; then mixing and grinding the mixture with fly ash and active carbon, and performing two-stage calcination of fast-firing dehydration and high-temperature sintering under reducing gas to obtain the phosphogypsum-based cementing material.
The Chinese patent application CN104211313A discloses a phosphogypsum-based cementing material and an application thereof in mine tailing filling; firstly, respectively grinding phosphogypsum, red mud, phosphorous slag and clinker to 800m2/kg、700m2/kg、300m2/kg、300m2More than kg, and then adding the excitant after mixing to improve the early strength of the filling body. The treatment can improve the early strength to a certain extent, but the effect is remarkable without reliable basis, and the requirement of mining early strength by a downward stratified filling method is difficult to meet. CN108191365A discloses a method for cementing and filling metal mines by using phosphogypsum materials, which uses phosphogypsum as a filling cementing material and discloses a filling process applied to filling mines, wherein the strength of phosphogypsum-based cementing materials is not considered, and the pipe conveying characteristics of slurry are not involved.
In summary, the existing method for preparing the early strength cementing material by using the phosphogypsum needs to adopt a plurality of treatment processes, and a plurality of additives and mixed materials are added for grinding or calcining to remove impurities, so that the early strength of the cementing material is improved, and the instability of the volume is solved. Obviously, the treatment processes and methods not only increase the production cost of the cementing material, but also pollute the environment through a series of treatment processes such as mixing grinding, calcining and the like, and are not beneficial to low-cost and large-scale utilization of the phosphogypsum.
Disclosure of Invention
The invention aims to solve the technical problem of providing an optimization method of a phosphogypsum-based cementing material for improving the filling and roof-contacting rate.
In order to solve the technical problems, the technical scheme adopted by the invention is as follows: (1) drying and crushing phosphogypsum into phosphogypsum powder, and then carrying out material particle size analysis and distribution characteristic value calculation;
(2) adding phosphogypsum powder and an exciting agent in different proportions into the filling aggregate to prepare cemented filling materials in different proportions; the excitant is quicklime, NaOH and mirabilite;
(3) carrying out a strength test and a filling body expansion rate test on the cemented filling body materials with different proportions to obtain test data of the strength and the expansion rate of the cemented filling body materials with different proportions;
(4) and (3) performing stepwise regression analysis on the test data of the strength and the expansion rate of the cemented filling body by using a quadratic polynomial to establish the functional relations (I) and (II) of the 3d strength and 28d expansion rate of the cemented filling body and the exciting agent:
R3d=F1(Y) （Ⅰ）；
V28d=F2(Y) （Ⅱ）；
in the formula, R3dRepresents the 3d strength of the cemented filling body; v28dRepresenting the 28d filling body expansion rate; y = (Y)1,y2,…,yn﹜TRepresents a trigger variable; f1(Y) represents a cemented pack 3d strength model; f2(Y) represents a 28d pack expansion model;
(5) according to the expansion rate test result of the filling body, an expansion rate allowable value V of the filling body of the cementing material 28d without strength deterioration is required to be determined28d]；
(6) Establishing a proportioning optimization model of the cementing material by taking the 3d strength of the cemented filling body as an optimization target and taking the expansion rate of the 28d filling body as a constraint condition:
optimizing the target: MaxR3d=MaxF1(Y) （1）；
Constraint conditions are as follows: v28d=F2(Y)≤[V28d]（2）；
(7) And solving the optimization model to obtain the optimized proportion of the phosphogypsum-based cementing material in the filling slurry.
In the step (1), the specific surface area of the phosphogypsum powder is more than or equal to 200m2Kg, water content < 3 wt%.
In the step (2), the ratio of the phosphogypsum powder to the exciting agent in the material of the bonded filler is as follows: 30-45% of phosphogypsum powder, 4.5-6% of quicklime, 0.5-2.0% of NaOH, 1.5-3.0% of mirabilite and the balance of filling aggregate.
Adopt the produced beneficial effect of above-mentioned technical scheme to lie in: the invention utilizes the undisturbed phosphogypsum, optimizes the alkali salt composite exciting agent formula, maximally provides the early strength, controls the expansion rate of the cemented body and avoids the problem of the degradation of the expansion strength. The method does not need the pretreatment of phosphogypsum washing, standing and grinding, and does not need high-temperature calcination; the phosphogypsum-based gelling material prepared by the method has simple process and low material cost; meanwhile, the infill is prepared by reasonably utilizing the instability of the phosphogypsum, and the roof contact rate of a filling stope can be improved. Therefore, the optimization method of the cementing material can realize low-cost and high-value resource utilization of the phosphogypsum.
Drawings
The present invention will be described in further detail with reference to the accompanying drawings and specific embodiments.
FIG. 1 is a particle size grading distribution curve of phosphogypsum in the example of the present invention;
FIG. 2 is a microstructure of the micro surface topography of the phosphogypsum in an embodiment of the invention;
FIG. 3 is an XRD pattern of phosphogypsum in the examples of the present invention;
FIG. 4 shows the micro surface topography of the calcined lime according to the embodiment of the present invention.
Detailed Description
The phosphogypsum-based gelling material optimization method for improving the filling and roof-contacting rate utilizes low-quality phosphogypsum solid waste and adopts a one-step optimization method for proportioning phosphogypsum-based gelling material excitant to make a proportioning decision; the method for designing the phosphogypsum-based gelling material adopts the following steps.
1. Low quality solid waste, and physical and chemical analysis and particle size testing of the packing material.
(1) The low-quality solid waste resources comprise phosphogypsum and mine waste rock. Firstly, drying and crushing the phosphogypsum to obtain the phosphogypsum with the specific surface area more than or equal to 200m2/kg, water content less than or equal to 3wt percent. Then crushing the tunneling waste stone into water with the particle size of-12 mm by adopting a jaw crusherCoarse aggregate with the rate less than or equal to 8 wt%; and finally, carrying out particle size analysis and distribution characteristic value calculation on the phosphogypsum and the waste rock coarse aggregate.
(2) Quicklime, NaOH and mirabilite are selected as excitant materials, and rod-milled sand with the diameter of-5 mm is adopted as a mixture of waste stone aggregates. Grinding quicklime powder into powder with surface area more than or equal to 350m2/kg, water content less than or equal to 3wt percent.
2. The strength test of the early-strength phosphogypsum-based cementing material cement and the formula optimization of the exciting agent.
(1) And (3) according to the phosphogypsum and the excitant material in the step 1, adopting a-5 mm rod mill sand aggregate to carry out the design of the phosphogypsum-based gelling material composite excitant proportioning orthogonal test scheme.
(2) Preparing filling slurry and filling body test blocks according to the exciting agent material, the filling aggregate and the orthogonal test scheme in the step (1). And then carrying out a strength test and an expansion rate test on the cemented filling body according to a cement mortar strength test method (ISO method) B/T17671-1999, thereby obtaining test results of the strength and the expansion rate of the cemented filling body test block with different excitant proportions.
(3) Aiming at the strength test result of the cemented test block in the step (2), a quadratic polynomial is adopted to carry out stepwise regression analysis on the test data, so that the models for establishing the early strength and the later submitted expansion rate of the cemented filling body are respectively as follows:
R3d=F1(Y) （Ⅰ）；
V28d=F2(Y) （Ⅱ）；
wherein R is3dRepresents the strength of the filling body 3 d; v28dRepresenting the 28d filling body expansion rate; y = (Y)1,y2,…,yn﹜TRepresents an activator variable of the phosphogypsum-based gelling material; f1(Y) represents a cemented pack 3d strength model; f2(Y) represents a 28d pack expansion model;
(4) according to the cemented filling body 3d strength and filling body 28d volume expansion rate model in the step (3), establishing an early-strength phosphogypsum-based cementing material activator proportioning optimization model by taking the cemented filling body 3d strength as an optimization target and the filling body 28d volume expansion rate as a constraint condition:
optimizing the target: MaxR3d=MaxF1(Y) （1）；
Constraint conditions are as follows: v28d=F2(Y)≤[V28d]（2）。
(5) And (4) solving the early-strength phosphogypsum-based cementing material proportion optimization model in the step (4) to obtain the optimal formula of the excitant with the maximum 3d strength of the cemented filling body and the filling body expansion rate smaller than an allowable value.
3.① waste stone is used as coarse aggregate, rod grinding is used as mixed aggregate, particle size analysis and characteristic value calculation are carried out on the waste stone and rod grinding sand, ② mixed filling aggregate with different proportions of the waste stone and the rod grinding sand is designed, and a strength test of a cemented filling body is carried out to obtain test results of strength of the cemented filling body and fluidity and stability of filling slurry.
Example (b): the optimization method of the phosphogypsum-based gelling material is specifically described as follows.
1. The activator of the early-strength phosphogypsum-based cementing material is optimized by the following steps:
(1) drying and grinding the low-quality phosphogypsum solid waste, and performing physical and chemical analysis and particle size test. The analysis result of the mineral components of the phosphogypsum is shown in table 1, the grain size grading distribution curve is shown in figure 1, the microcosmic surface morphology structure of the phosphogypsum is shown in figure 2, and the XRD spectrum of the phosphogypsum is shown in figure 3.
Table 1: analysis result of mineral component in phosphogypsum solid waste
(2) Grinding and particle size testing are carried out on the quicklime excitant to obtain the quicklime particle size distribution characteristic value as follows: d10=2.17μm，d30=4.60μm，d60=6.53μm，d50=5.86μm，d90=17.04 μm. The particle size distribution curvature coefficient of the quicklime powder is 1.49, and the nonuniform coefficient is 3.01. The micro surface appearance of the quicklimeThe structure is shown in figure 4.
(3) Quick lime, NaOH and mirabilite are selected as exciting agents to excite the activity of the phosphogypsum to prepare the phosphogypsum-based gelling material. The weight ratio of the phosphogypsum powder to the exciting agent in the material of the packing is as follows: 30-45% of phosphogypsum powder, 4.5-6% of quicklime, 0.5-2.0% of NaOH, 1.5-3.0% of mirabilite and the balance of filling aggregate. The filling aggregate is ground by a rod with the thickness of-5 mm and the weight ratio of 1:4 of mortar, and the filling material is added with water to prepare slurry with the concentration of 82 wt%. The slurry was subjected to a strength test and a volume expansion test of the cemented filling body, and the test results were obtained as shown in Table 2.
Table 2: strength and expansion rate test results of the Filler
(4) According to the testing results of the strength and the volume expansion rate of the phosphogypsum cementing material cemented filling body, a quadratic polynomial is adopted to carry out stepwise regression analysis on the test data, and a regression model of the 3d strength and the 28d filling body expansion rate of the cemented filling body is established:
R3d=0.297-2.58x3-0.00431x1x2+0.667x1x3+0.0465x3x4；
V28d=23.1-37.1x1+2.6x2+16.8x4+4.3x1x1-0.02x2x2+1.87x3x3-0.10x1x2-0.1x1x3-1.3x1x4-0.3x2x4；
wherein R is3dRepresents the 3d strength of the cemented filling body, MPa; v28dRepresents 28d pack expansion,%; x is the number of1Represents the quicklime proportion,%; x is the number of2Represents the proportion of phosphogypsum,%; x is the number of3Represents the NaOH ratio,%; x is the number of4Represents the mirabilite proportion in percent.
(5) According to the 3d strength and 28d filling body expansion rate model of the cemented filling body, the allowable value of the filling body expansion rate is determined to be 8% by means of experience, and the model for optimizing the proportioning of the activator of the early-strength phosphogypsum cementing material is established as follows:
optimizing the target: MaxR3d=Max(0.297-2.58x3-0.00431x1x2+0.667x1x3+0.0465x3x4)；
Constraint conditions are as follows: v28d≤[V28d]=23.1-37.1x1+2.6x2+16.8x4+4.3x1x1-0.02x2x2+1.87x3x3-0.10x1x2-0.1x1x3-1.3x1x4-0.3x2x4≤8%。
(6) Solving an optimization model of the activator proportion of the early-strength phosphogypsum-based cementing material to obtain the proportion of the cementing material in the cemented filling material as follows: 6.0wt% of quicklime, 30.0wt% of phosphogypsum, 2.0wt% of NaOH and 2.0wt% of mirabilite.
(7) According to the proportion of the phosphogypsum-based gelling material and the material cost: the cost of quicklime is 320 yuan/t, the cost of phosphogypsum is 40 yuan/t, the cost of NaOH is 2100 yuan/t, the cost of mirabilite is 550 yuan/t, and the cost of slag micro powder is 140 yuan/t, so that the cost of the early-strength phosphogypsum-based cementing material is 168.2 yuan/ton.
At present, the cost of the 42.5 cement cementing material reaches 380 yuan/ton. Therefore, the cost of the phosphogypsum-based cementing material is reduced by 212 yuan/ton compared with the cost of a cement cementing material.
Claims (3)
1. An optimization method of a phosphogypsum-based cementing material for improving the filling and roof contact rate is characterized by comprising the following steps: (1) drying and crushing phosphogypsum into phosphogypsum powder, and then carrying out material particle size analysis and distribution characteristic value calculation;
(2) adding phosphogypsum powder and an exciting agent in different proportions into the filling aggregate to prepare cemented filling materials in different proportions; the excitant is quicklime, NaOH and mirabilite;
(3) carrying out a strength test and a filling body expansion rate test on the cemented filling body materials with different proportions to obtain test data of the strength and the expansion rate of the cemented filling body materials with different proportions;
(4) and (3) performing stepwise regression analysis on the test data of the strength and the expansion rate of the cemented filling body by using a quadratic polynomial to establish the functional relations (I) and (II) of the 3d strength and 28d expansion rate of the cemented filling body and the exciting agent:
R3d=F1(Y) （Ⅰ）；
V28d=F2(Y) （Ⅱ）；
in the formula, R3dRepresents the 3d strength of the cemented filling body; v28dRepresenting the 28d filling body expansion rate; y = (Y)1,y2,…,yn﹜TRepresents a trigger variable; f1(Y) represents a cemented pack 3d strength model; f2(Y) represents a 28d pack expansion model;
(5) according to the expansion rate test result of the filling body, determining the allowable expansion rate value V of the filling body of the cementing material 28d without strength deterioration according to needs28d]；
(6) Establishing a proportioning optimization model of the cementing material by taking the 3d strength of the cemented filling body as an optimization target and taking the expansion rate of the 28d filling body as a constraint condition:
optimizing the target: MaxR3d=MaxF1(Y) （1）；
Constraint conditions are as follows: v28d=F2(Y)≤[V28d]（2）；
(7) And solving the optimization model to obtain the optimized proportion of the phosphogypsum-based cementing material in the filling slurry.
2. The optimization method of the phosphogypsum-based cementing material for improving the filling and roof-contacting rate according to claim 1, which is characterized in that: in the step (1), the specific surface area of the phosphogypsum powder is more than or equal to 200m2Kg, water content < 3 wt%.
3. The optimization method of the phosphogypsum-based cementing material for improving the filling and roof-contacting rate according to claim 1 or 2, which is characterized in that the weight ratio of the phosphogypsum powder and the exciting agent in the filler material in the step (2) is as follows: 30-45% of phosphogypsum powder, 4.5-6% of quicklime, 0.5-2.0% of NaOH, 1.5-3.0% of mirabilite and the balance of filling aggregate.
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| CN115288780A (en) * | 2022-07-14 | 2022-11-04 | 山东杰控电气技术有限公司 | Optimization design method for utilization of red mud solid waste in filling mining of water-rich mine |
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