CN115677287A - Compression-resistant and acid-resistant solid waste base filling cementing material and preparation method thereof - Google Patents

Compression-resistant and acid-resistant solid waste base filling cementing material and preparation method thereof Download PDF

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Publication number
CN115677287A
CN115677287A CN202110831802.7A CN202110831802A CN115677287A CN 115677287 A CN115677287 A CN 115677287A CN 202110831802 A CN202110831802 A CN 202110831802A CN 115677287 A CN115677287 A CN 115677287A
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China
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acid
cementing material
cement
resistant
solid waste
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郭利杰
王丽娟
张丹
吕国诚
李文臣
廖立兵
那华
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China University of Geosciences Beijing
BGRIMM Technology Group Co Ltd
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China University of Geosciences Beijing
BGRIMM Technology Group Co Ltd
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    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02WCLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
    • Y02W30/00Technologies for solid waste management
    • Y02W30/50Reuse, recycling or recovery technologies
    • Y02W30/91Use of waste materials as fillers for mortars or concrete

Abstract

The invention discloses a compression-resistant and acid-resistant solid waste base filling cementing material and a preparation method thereof, wherein the filling cementing material takes smelting slag, standard sand and cement as raw materials, and the sand-cement ratio is 1-5. The solid waste based filling cementing material with higher compression resistance and stronger acid resistance can be prepared by taking the solid waste smelting slag as a raw material. In addition, the preparation process of the invention has simple steps, is green and energy-saving, and is easy for industrial production.

Description

Compression-resistant and acid-resistant solid waste base filling cementing material and preparation method thereof
Technical Field
The invention belongs to the technical field of environmental science and cementing material preparation, and particularly relates to a compression-resistant and acid-resistant solid waste base filling cementing material and a preparation method thereof.
Background
In recent years, with rapid development of industrialization, gradual increase of demand and more attention paid to the environment, underground mining gradually enters the field of people due to the advantages of high efficiency, low initial investment, benefit for ground pressure management and control in the later period and the like. A large number of goafs, namely underground cavities left after mining, can be formed in the underground mining process. The large amount of goafs can destroy the stress balance of mine rocks, and the collapse and caving of the top rocks seriously affect the production safety of mines.
The filling mining technology is a mining technology for filling an underground goaf by using filling materials, and comprises a plurality of mining methods such as dry type, hydraulic power, cementation and the like. The filling cementing material mainly comprises cementing agent and aggregate. At present, the mine filling cementing material mainly uses cement as a cementing agent, and the aggregate is widely available. In the mining process, a large amount of solid wastes such as tailings, waste rocks, smelting waste residues and sludge are generated, and if the solid wastes are not treated properly, the environment is seriously polluted. The solid wastes can be used as a cementing material, and part of the solid wastes has certain cementing activity after being ground or excited, so that the solid wastes can replace part of cement, and the cost of filling the cementing material is reduced.
Along with the enhancement of the consensus of ecological protection consciousness and green development concept in China, the environmental management problem of a mining area is increasingly emphasized, so that the research on the preparation of the pressure-resistant and acid-resistant solid waste base filling cementing material and the immobilization behavior of harmful substances such as heavy metal and the like has important theoretical and practical significance on the environmental management of the mining area and the development of a novel filling cementing material in the future, but the lack of theoretical research on the acid resistance of the solid waste base filling cementing material is one of the biggest problems restricting the development of the solid waste base filling cementing material at present.
Disclosure of Invention
Aiming at the problems in the prior art, the invention develops a compression-resistant acid-resistant solid waste base filling cementing material and a preparation method thereof, the filling cementing material is obtained by mixing smelting slag with a sand-lime ratio of 1-5, standard sand and cement, and the acid leaching test is carried out on the filling cementing material, and the test result shows that the filling cementing material has stronger acid corrosion resistance, thereby completing the invention.
In order to achieve the above objects, in a first aspect, the present invention provides a pressure-resistant and acid-resistant solid waste base filling cementitious material, which takes smelting slag, standard sand and cement as raw materials, wherein the sand-cement ratio is 1-5.
In a second aspect, the present invention provides a method for preparing a pressure-resistant and acid-resistant solid waste based filling cementitious material, preferably the filling cementitious material of the first aspect, which comprises:
step 1, weighing raw materials, and preparing the raw materials into slurry;
step 2, pouring the slurry into a mold, and performing vibration molding;
and 3, maintaining the molded sample to obtain the filling cementing material.
In a third aspect, the present invention provides the use of the pressure-resistant, acid-resistant solid waste base packing cementitious material produced by the method of the first or second aspect, preferably in road, bridge, building or mining fill.
The compression-resistant and acid-resistant solid waste base filling cementing material and the preparation method thereof have the beneficial effects that:
(1) The solid waste base filling cementing material with higher compression resistance and stronger acid resistance can be prepared by taking the solid waste smelting slag with the sand-cement ratio of 1-5, standard sand and cement as raw materials;
(2) The solid waste base filling cementing material has low preparation cost and high solid waste utilization rate;
(3) The method has simple steps, high efficiency, greenness, energy conservation and easy industrial production;
(4) The method can fully and accurately evaluate the acid leaching resistance of the solid waste base filling cementing material, and further promote the development and application of the solid waste base filling cementing material.
Drawings
Fig. 1 shows ICP test results of acid leachate of examples 1 to 4 of the present invention and comparative example 1;
FIG. 2 shows the ICP test results of acid leach liquor at different acid leach times in example 1 of the present invention;
FIG. 3 shows the results of ICP testing of the acid leachate of example 1 and examples 8 to 11 of the present invention;
fig. 4 shows ICP test results of the acid leachate of example 1, example 5 and comparative example 2 of the present invention.
Detailed Description
The invention is explained in more detail below with reference to the drawings and preferred embodiments. The features and advantages of the present invention will become more apparent from the description.
The word "exemplary" is used exclusively herein to mean "serving as an example, embodiment, or illustration. Any embodiment described herein as "exemplary" is not necessarily to be construed as preferred or advantageous over other embodiments. While the various aspects of the embodiments are presented in drawings, the drawings are not necessarily drawn to scale unless specifically indicated.
In a first aspect, the invention provides a compression-resistant and acid-resistant solid waste base filling cementing material, which takes smelting slag, standard sand and cement as raw materials, wherein the sand-cement ratio is 1-5.
In the invention, the cement is preferably P.O 42.5 Portland cement, which is ordinary Portland cement with the performance meeting the quality requirement of standard general Portland cement (GB 175-2020) and the strength grade of 42.5. The cement and the standard sand are purchased from China building materials research institute.
In the present invention, the smelting slag is preferably copper-nickel ore smelting slag (available from Xinjiang Kalatong mining, inc.). Because the particle size of the smelting slag is larger, the raw materials need to be ground to enable the particle size of the ground smelting slag to be smaller than 400 microns so as to enable the raw materials to be mixed more uniformly.
The solidification capability of the filling cementing material on harmful elements, namely the acid corrosion resistance can be reflected by the concentration of the harmful elements in the leachate, and the low concentration and/or small change of component morphology of the leachate indicate that the acid corrosion resistance is strong, otherwise, the acid corrosion resistance is weak.
Research shows that the cement plays a decisive role in the acid corrosion resistance of the filled cementing material. Along with the increase of the sand-ash ratio, the concentration of harmful elements in the acid leaching liquid also increases, namely the solidification capacity of the filling cementing material to the harmful elements in the smelting slag is reduced, which indicates that the acid resistance of the acid leaching liquid is reduced. The leaching concentration of the harmful elements (Cu, ni, co and Cr) of the filled cementitious material is small when the sand-to-lime ratio is between 1 and 5, preferably between 1 and 4. When the sand-lime ratio is more than 5, the leaching concentration of harmful elements (Cu, ni, co and Cr) of the filling cementing material is higher, and particularly, the Cr element is more obvious. Similarly, the compressive strength of the filled cementitious material decreases as the sand-cement ratio increases, and when the sand-cement ratio is 1 to 5, preferably 1 to 4, the compressive strength of the filled cementitious material is significantly higher than that when the sand-cement ratio is more than 5.
The research shows that the curing time also influences the acid corrosion resistance and the compressive strength of the filled cementing material. The leaching concentrations of the three elements Cu, ni and Co have a small relationship with the curing time of the filled cement, but the leaching concentration of Cr decreases with the curing time of the filled cement. Similarly, as the curing time increases, the compressive strength of the filled cementitious material increases. Therefore, the curing time of the present pack cement is not less than 3 days, preferably not less than 15 days, and more preferably not less than 28 days.
In the present invention, the sand-ash ratio is the mass ratio of standard sand to (cement and smelting slag). Researches show that the sand-lime ratio has an important influence on the acid resistance of the filled cementing material. This is probably because the C-S-H gel generated in the hydration reaction process of cement can produce physical encapsulation to Cu and other elements or the chemical fixation of partial hydration products and harmful elements, and reduce the leaching concentration. Meanwhile, more alkaline substances may be generated, the alkaline substances and acid are subjected to neutralization reaction, the dissolution of harmful elements is reduced, and partial alkaline substances are dissolved in water and can react with the harmful elements to generate precipitates, so that the leaching concentration of elements such as Cu is finally reduced. The solidification of Cr in filled cementitious materials is associated with ettringite hydrate phases and C-S-H gel bonding. Meanwhile, the filled cementing material is decalcified in acid, so that the filled cementing material has stronger acid neutralization capacity, and the dissolution mechanism of Cr element is more complex compared with other elements. Therefore, as the sand-to-ash ratio increases, the ability of the packed cementitious material to solidify the harmful elements in the slag decreases.
Researches show that the curing time of the filled cementing material has small influence on leaching of harmful elements such as Cu and the like, and has large influence on the leaching concentration of Cr. The longer the curing time of the filled cement, the more such cement hydrates and therefore the higher the Cr curing rate.
In a second aspect, the present invention provides a method for preparing a compression-resistant and acid-resistant solid waste base filling cementing material, preferably the filling cementing material of the first aspect, the preparation method mainly comprises the following steps:
step 1, weighing raw materials, and preparing the raw materials into slurry.
In a preferred embodiment of the invention, the raw materials of this step include smelting slag, standard sand and cement. Wherein the sand to ash ratio is 1 to 5, preferably 1 to 4, more preferably 2 to 4, such as 2 or 2.50 or 3.03.
According to the present invention, since the particle size of the smelting slag is large, it is necessary to grind the smelting slag in order to mix the raw materials more uniformly. Therefore, before step 1, the preparation method of the present invention further comprises grinding the smelting slag so that the particle size of the ground smelting slag is less than 400 μm.
Illustratively, the smelting slag is placed in a ball mill for grinding to a particle size of less than 400 μm. For example, the rotating speed of the ball mill is 800-2000 r/min, the grinding time is 4-10 h, wherein the rotating speed and the grinding time of the ball mill are determined according to the mass of the smelting slag added according to actual needs.
According to the invention, the mass ratio of the smelting slag to the cement is 1 (1.5-7), preferably 1 (2-5). The reason is that the smelting slag contains more heavy metal elements, the existence of the heavy metal elements can influence the cement hydration reaction, and the compression strength and the acid corrosion resistance of the filled cementing material are related to cement hydration products, so that the higher the content of the smelting slag is, the less the cement hydration products are in the material, and the compression strength and the acid corrosion resistance of the material are reduced.
According to the present invention, when the amount of water used is large in the process of preparing the slurry, although the smelting slag, the standard sand and the cement can be rapidly and uniformly mixed, the setting time of the slurry increases. When the amount of water used is small, the smelting slag, the standard sand and the cement cannot be uniformly mixed, and the pressure resistance of the slurry is small. Therefore, the present invention preferably has a water to cement ratio of 0.4 to 0.6, for example 0.5.
And 2, pouring the slurry into a mold, and performing vibration molding.
In a preferred embodiment of the invention, the mould specifications are: 120mm x 40mm triple die.
In a preferred embodiment of the invention, the slurry is vibro-molded using a vibro-table, wherein the vibro-time is from 1 to 10 minutes, preferably from 1 to 5 minutes, such as 2 or 3 minutes.
And 3, maintaining the molded sample to obtain the filling cementing material.
In a preferred embodiment of the present invention, step 3 may further comprise:
and 3-1, performing pre-curing on the molded sample to obtain a pre-cured sample.
In order to coagulate the sample, i.e., to fix its shape, pre-curing is performed in a mold. In a preferred embodiment of the present invention, the pre-curing temperature of the step is 20 to 30 ℃ and the pre-curing time is 1 to 4 days; preferably, the pre-curing temperature is 20 to 25 ℃ and the pre-curing time is 1 to 3 days, for example, the pre-curing temperature is 25 ℃ and the pre-curing time is 2 days.
And 3-2, demolding the pre-cured sample, and curing.
Wherein, in order to ensure that the sample has proper hardening conditions and the compressive strength of the sample is continuously increased, the sample needs to be maintained again. Wherein the curing temperature and humidity should be controlled during curing. In a preferred embodiment of the present invention, the curing temperature in this step is 20 to 35 ℃, the curing time is not less than 28 days, and the curing humidity is 91 to 99%.
In a preferred embodiment of the present invention, the preparation method further comprises: and 4, carrying out acid leaching test on the filled cementing material.
According to the invention, step 4 may further comprise the following substeps:
and 4-1, crushing the filling cementing material to obtain a sample to be detected.
In the present invention, before this step, the step may further include placing the filled cementitious material in an oven, baking until the mass does not change any more, and cooling to room temperature. The operation can ensure that the filled cementing material is completely dried without redundant water, thereby avoiding influencing the concentration of acid leaching liquid and ensuring the accuracy of an acid leaching test.
Preferably, the particle size of the crushed filled cement is about 1 cm. Thus, the full mixing of the acid leaching solution and the acid leaching liquid can be ensured, and the high accuracy of the acid leaching test can be kept.
According to the invention, the step also comprises the step of sieving the crushed filled cementing material, and taking the sample with smaller mesh as a sample to be measured. This operation enables the particle size of the sample to be measured to be uniform and small, so that it can be sufficiently and rapidly mixed with the acid leachate.
And 4-2, preparing acid leaching liquid.
According to the invention, the acid leachate in this step comprises at least two strong inorganic acids. Preferably, the strong inorganic acid includes at least one of concentrated sulfuric acid, concentrated nitric acid, concentrated hydrochloric acid, perchloric acid, hydroiodic acid, and hydrobromic acid.
In the invention, the leaching solution with different pH values is preferably prepared by adopting a mixed solution of concentrated sulfuric acid with the mass fraction of 85-98% and concentrated nitric acid with the mass fraction of 55-65%, wherein the pH value is 1-6.
Specifically, the mass ratio of concentrated sulfuric acid to concentrated nitric acid is (4-1): 1, preferably (3-1): 1, and more preferably 2:1.
The method is based on a solid waste toxicity leaching method, namely a sulfuric acid-nitric acid method, and a leachate is prepared by selecting a mixed solution of concentrated sulfuric acid and concentrated nitric acid with the mass ratio of 2:1 in a simulated natural environment.
And 4-3, mixing the sample to be detected with the acid leaching solution, and determining the concentration of harmful elements in the acid leaching solution.
The mixing mode of the sample to be detected and the acid leaching solution is not particularly limited, and can be determined by a person skilled in the art according to the actual situation. Such as shaking, stirring, mixing, and the like. Illustratively, the sample to be tested and the acid leachate are mixed by shaking in a roll-over shaker. Preferably, the rotating speed of the turnover type oscillator is 20-80 r/min, the oscillation time is 5-30 h, more preferably, the rotating speed is 20-50 r/min, and the oscillation time is 10-20 h.
According to the invention, this step also comprises adjusting the pH of the acid leachate so that the pH is constant. This is because the alkaline substances contained in the cement react with the acid to lower the pH value of the leachate, which greatly affects the leaching reaction of the acid on the harmful elements. Thus, the pH of the acid leach liquor should be adjusted so that it is constant during the duration of the leaching test.
Specifically, the pH value of the acid leaching solution is adjusted at preset time intervals during the mixing of the sample to be detected and the acid leaching solution.
The preset time is not specifically limited, and can be determined by those skilled in the art according to the mixing time of the actual sample to be tested and the acid leaching solution. For example, the predetermined time is 1 to 3 hours, and generally 2 hours.
In the invention, the influence of the sand ash ratio on the leaching performance of the filled cementing material is only reflected on Cr, the solidification of Cr is mainly related to ettringite, and the content of the ettringite in the material is increased after the material is cured. The curing efficiency of the filling cementing material to harmful elements such as Cu is more than 95 percent, and the curing efficiency to Cr is close to 70 percent. The filled cementing material is proved to have excellent harmful element solidification capability. Compared with smelting slag, the filled cementing material is less corroded. The component analysis shows that the component change before and after leaching is small, which proves that the cementing material has excellent acid corrosion resistance and also proves that harmful elements are fixed in a cement hydration product.
In a third aspect, the present invention provides the use of a pressure resistant, acid resistant solid waste based packing cementitious material prepared by the method of the first or second aspect, preferably in road, bridge, building or mining fill.
For further understanding of the present invention, the following examples are provided to describe the pressure-resistant and acid-resistant solid waste based packing cementitious material provided by the present invention, and the scope of the present invention is not limited by the following examples.
Examples
Example 1
Placing 2000g of smelting slag in a ball mill, and ball-milling for 6h at the rotating speed of 1000r/min to ensure that the particle size of the grinded smelting slag is less than 400 mu m, and then mixing 150g of smelting slag, 1000g of standard sand and 350g of cement (the sand-ash ratio is 2, and the water-ash ratio is 0.5) to prepare slurry;
pouring the slurry into a mold with the thickness of 120mm multiplied by 40mm, and vibrating on a vibrating table for 120s to form the slurry;
placing the molded sample at normal temperature for 48h, demolding, and curing in a curing box for 28 days to obtain a filling cementing material, wherein the temperature of the curing box is 22 ℃, and the humidity is 99%;
crushing 100g of filling cementing material to ensure that the particle size of the crushed cementing material is about 1cm, thereby obtaining a sample to be detected;
preparing 1000mL acid leaching solution with pH value of 3 by using 98% concentrated sulfuric acid and 65% concentrated nitric acid in the mass ratio of 2:1;
placing a sample to be detected and 1000mL of acid leaching solution in a turnover type oscillator, oscillating for 16h at the rotating speed of 30r/min, adjusting the pH value of the acid leaching solution every 2h, and controlling the pH value to be 3.
Examples 2 to 4
The procedure was similar to that of example 1 except that the standard sands had masses of 1250g, 1515g and 2120g, respectively, giving sand-to-ash ratios of 2.50, 3.03 and 4.24, respectively.
Examples 5 to 7
The procedure was similar to that of example 1, except that the curing was carried out in a curing box for 15 days, 20 days and 40 days after the demolding.
Examples 8 to 11
A similar procedure to that of example 1, except that the pH values of the acid leachate were 2, 4, 5 and 6, respectively.
Comparative example 1
The procedure was similar to that of example 1 except that the standard sands each had a mass of 3780g and the sand-to-ash ratio was 7.65.
Comparative example 2
The procedure was similar to that of example 1, except that the mold was removed and cured in a curing box for 3 days.
Examples of the experiments
Experimental example 1 compressive Strength test
The filled gelled materials prepared in the examples 1-7 and the comparative examples 1-2 are dried, and the samples are subjected to compression resistance test by adopting a microcomputer-controlled electro-hydraulic servo universal tester, wherein the test data are shown in table 1.
TABLE 1 compressive Strength data of samples at different Sand to Ash ratios or curing times
Figure BDA0003175732080000111
As can be seen from Table 1, the compressive strength of the filled cement decreases as the sand to cement ratio increases. The compressive strength of the filled cement was 12.7MPa when the sand-cement ratio was 2, and only 1.71MPa when the sand-cement ratio was 7.65.
Similarly, the compressive strength of the filled cementing material is increased along with the increase of the curing time, and when the curing is carried out for 3 days, the compressive strength is 10.4MPa and is less than the compressive strength of the curing for 28 days.
Experimental example 2 acid erosion resistance test
(1) The acid leachate of examples 1 to 4 and comparative example 1 was filtered and subjected to ICP test, and the test results are shown in fig. 1.
As can be seen from figure 1, the solidification effects of the filled cementitious materials with different sand-to-ash ratios on Cu, ni and Co elements are not very different and are far less than the leaching concentration of the smelting slag. The leaching concentrations of Cu, ni and Co elements in the filled cementing material of the example 1 are 5.60 mu g/L, 2.31 mu g/L and 1.50 mu g/L respectively; the leaching concentrations of Cu, ni and Co elements in the filled cement of example 3 are 7.81. Mu.g/L, 2.926. Mu.g/L and 1.94. Mu.g/L respectively. The leaching concentrations of Cu, ni and Co elements in the filled cement of comparative example 1 were 9.38. Mu.g/L, 6.19. Mu.g/L and 6.35. Mu.g/L, respectively. It shows that the solidification capacity of the filling cementing material to harmful elements in smelting slag is reduced along with the increase of the sand-ash ratio. In which the degree of solidification of Cr is relatively poor compared to the elements Cu, ni and Co. When the sand-lime ratio is 7.65, the leaching concentration of Cr is 70.9 mug/L, the curing rate is only 35%, and the curing efficiency is poor. When the sand-cement ratio reaches 2.50, the solidification rate of Cr reaches 68%. When the sand-lime ratio is 2.00, the solidification rate of Cr can reach 70%.
(2) The acid corrosion resistance performance test was carried out for six periods of 30min, 1h, 3h, 6h, 10h and 16h for example 1, and the ICP test was carried out after filtering the acid leachate, with the test results shown in fig. 2. FIGS. 2 (a-d) are ICP data for Cu, ni, co and Cr elements at different leaching times, respectively.
As can be seen from fig. 2, the leaching concentrations of Cu, ni, co and Cr elements in the smelting slag increase with the increase of the leaching time, and the leaching concentrations are all larger. After the smelting slag is leached for 16 hours, the concentrations of Cu, ni, co and Cr elements are 361.4 mu g/L, 244.4 mu g/L, 170.3 mu g/L and 283.6 mu g/L respectively. This is because the smelting slag contains metal oxides which, when exposed directly to an acid environment, react with the acid and dissolve in the leach solution. And the leaching concentrations of Cu, ni, co and Cr elements in the leaching solution after the filling cementing material of the example 1 is leached for 16 hours are respectively 5.6 mu g/L, 2.3 mu g/L, 3.7 mu g/L and 86.3 mu g/L. Wherein, the solidification efficiency of Cu, ni and Co is above 95%, and the solidification efficiency of Cr is close to 70%. Therefore, the packed cement of example 1 has high acid leaching resistance.
(3) The acid leachate of example 1 and examples 8 to 11 was filtered and subjected to ICP test, and the test results are shown in fig. 3. FIGS. 3 (a-d) are ICP data for Cu, ni, co and Cr elements at different pH values, respectively.
As can be seen from fig. 3, the concentration of harmful elements in the acid leachate gradually decreased as the pH value increased. When the pH value is 2, the concentrations of Cu, ni, co and Cr elements in the acid leachate of the smelting slag are 652.4 mu g/L, 556.5 mu g/L, 361.0 mu g/L and 456.0 mu g/L respectively, and the concentrations of Cu, ni, co and Cr elements in the acid leachate of the filled cementing material are 5.9 mu g/L, 2.6 mu g/L, 1.8 mu g/L and 321.5 mu g/L respectively. At pH 6, the concentrations of the elements Cu, ni, co and Cr in the acid leachate of the slag were 198.0. Mu.g/L, 103.0. Mu.g/L, 124.0. Mu.g/L and 57.9. Mu.g/L, respectively, while the concentrations of the elements Cu, ni, co and Cr in the acid leachate of the filled cementitious material were 1.5. Mu.g/L, 1.9. Mu.g/L, 0.1. Mu.g/L and 21.8. Mu.g/L, respectively. Therefore, the pH value of the acid leaching liquid has larger influence on the leaching concentration of the smelting slag, and has smaller influence on the leaching concentration of the filled cementing material, so the filled cementing material has higher acid resistance.
(4) The acid leachate of example 1, example 5 and comparative example 2 was filtered and subjected to ICP test, and the test results are shown in fig. 4.
As can be seen from FIG. 4, the leaching concentrations of the three elements Cu, ni and Co have a small relationship with the curing time of the filled cementitious material. Leaching concentrations of the three elements of the filling cementing material cured for 3 days, 15 days and 28 days are 5.8 mu g/L, 2.5 mu g/L and 1.6 mu g/L respectively; 5.8. Mu.g/L, 2.4. Mu.g/L and 1.6. Mu.g/L as well as 5.6. Mu.g/L, 2.3. Mu.g/L and 1.5. Mu.g/L.
Relatively speaking, the leaching concentration of Cr is greatly influenced by the curing time of the filled cementing material, and the leaching concentrations of Cr of the cementing material cured for 3 days, 15 days and 28 days are 157.4. Mu.g/L, 144.6. Mu.g/L and 86.3. Mu.g/L respectively. Therefore, the acid resistance of the filled cementitious material can be improved by prolonging the curing time.
The invention has been described in detail with reference to the preferred embodiments and illustrative examples. It should be noted, however, that these specific embodiments are only illustrative of the present invention and do not limit the scope of the present invention in any way. Various modifications, equivalent substitutions and alterations can be made to the technical content and embodiments of the present invention without departing from the spirit and scope of the present invention, and these are within the scope of the present invention. The scope of the invention is defined by the appended claims.

Claims (10)

1. The pressure-resistant and acid-resistant solid waste base filling cementing material is characterized in that the filling cementing material takes smelting slag, standard sand and cement as raw materials, wherein the sand-cement ratio is 1-5.
2. The solid waste based filling cement as claimed in claim 1, wherein the curing time of the filling cement is not less than 28 days.
3. The preparation method of the pressure-resistant and acid-resistant solid waste base filling cementing material is characterized by comprising the following steps of:
step 1, weighing raw materials, and preparing the raw materials into slurry;
step 2, pouring the slurry into a mold, and performing vibration molding;
and 3, maintaining the molded sample to obtain the filling cementing material.
4. The method according to claim 3, wherein in step 1, the raw materials comprise smelting slag, standard sand and cement, wherein the sand-cement ratio is 1-5;
preferably, before step 1, the following steps are also performed: and grinding the smelting slag to ensure that the particle size of the ground smelting slag is less than 400 mu m.
5. The method for preparing a composite material according to claim 3, wherein the step 3 comprises the following substeps:
step 3-1, performing pre-curing on the molded sample to obtain a pre-cured sample;
and 3-2, demolding the pre-cured sample, and then curing.
6. The production method according to claim 5,
in the step 3-1, the pre-curing temperature is 20-30 ℃, and the pre-curing time is 1-4 days;
in the step 3-2, the curing temperature is 20-35 ℃, the curing time is not less than 28 days, and the curing humidity is 91-99%.
7. The method of manufacturing according to claim 3, further comprising the steps of:
and 4, carrying out acid leaching test on the filled cementing material.
8. The method according to claim 7, wherein step 4 comprises the following substeps:
step 4-1, crushing the filled cementing material to obtain a sample to be detected;
step 4-2, preparing an acid leaching solution;
and 4-3, mixing the sample to be detected with the acid leaching solution, and determining the concentration of harmful elements in the acid leaching solution.
9. The test method according to claim 8,
in step 4-2, the acid leachate comprises at least two strong inorganic acids, preferably, the strong inorganic acids comprise at least one of concentrated sulfuric acid, concentrated nitric acid, concentrated hydrochloric acid, perchloric acid, hydroiodic acid, and hydrobromic acid; and/or
And 4-3, adjusting the pH value of the acid leaching solution to ensure that the pH value is constant.
10. Use of a pressure-resistant, acid-resistant solid waste based packing cement made according to claim 1 or 2 or according to the method of any of claims 3-9, preferably in road, bridge, construction or mining fill.
CN202110831802.7A 2021-07-22 2021-07-22 Compression-resistant and acid-resistant solid waste base filling cementing material and preparation method thereof Pending CN115677287A (en)

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Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103641346A (en) * 2013-12-10 2014-03-19 北京科技大学 Method for preparing geopolymer gelled material from heavy metal gypsum
CN110482966A (en) * 2019-09-26 2019-11-22 北京矿冶科技集团有限公司 Compound cemented filling material and its preparation method and application
CN112458290A (en) * 2020-11-06 2021-03-09 金川集团股份有限公司 Harmless treatment method for solid waste of nickel-containing iron slag
CN112723831A (en) * 2021-01-08 2021-04-30 西安建筑科技大学 Lead-zinc slag-based ecological cementing material for cementing and curing heavy metals and preparation method thereof
CN113045226A (en) * 2021-03-10 2021-06-29 中国新型建材设计研究院有限公司 Low-cost solid waste base cementing material
CN115452927A (en) * 2022-08-15 2022-12-09 湖南军信环保股份有限公司 Method for detecting toxicity of leaching solution
US20230036470A1 (en) * 2021-04-12 2023-02-02 Brimstone Energy, Inc. Cementitious material production from non-limestone material

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103641346A (en) * 2013-12-10 2014-03-19 北京科技大学 Method for preparing geopolymer gelled material from heavy metal gypsum
CN110482966A (en) * 2019-09-26 2019-11-22 北京矿冶科技集团有限公司 Compound cemented filling material and its preparation method and application
CN112458290A (en) * 2020-11-06 2021-03-09 金川集团股份有限公司 Harmless treatment method for solid waste of nickel-containing iron slag
CN112723831A (en) * 2021-01-08 2021-04-30 西安建筑科技大学 Lead-zinc slag-based ecological cementing material for cementing and curing heavy metals and preparation method thereof
CN113045226A (en) * 2021-03-10 2021-06-29 中国新型建材设计研究院有限公司 Low-cost solid waste base cementing material
US20230036470A1 (en) * 2021-04-12 2023-02-02 Brimstone Energy, Inc. Cementitious material production from non-limestone material
CN115452927A (en) * 2022-08-15 2022-12-09 湖南军信环保股份有限公司 Method for detecting toxicity of leaching solution

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
周正立等: "《水泥化验与质量控制实用操作技术手册》", 北京:中国建材工业出版社, pages: 8 *

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