CN109824304B - Coal gangue regenerated slope protection brick and preparation method thereof - Google Patents
Coal gangue regenerated slope protection brick and preparation method thereof Download PDFInfo
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- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
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Abstract
The invention discloses a coal gangue regeneration slope protection brick and a preparation method thereof, wherein the raw materials comprise the following raw materials in parts by weight: 300-400 parts of cement, 300-400 parts of mountain flour, 250-350 parts of uncalcined coal gangue, 2-5 parts of accelerator, 2-5 parts of aluminum powder, 0.1-1 part of thickener, 10-30 parts of early strength agent and 2-18 parts of beta-sodium naphthalene sulfonate formaldehyde condensate. Some additives are added into the waste residue of the non-calcined coal gangue to be used as the components of the coal gangue regeneration slope protection brick, so that the performance of the coal gangue becomes excellent, the strength is enhanced, the demoulding time is shortened, and the coal gangue can be used as a building block brick of a novel wall material; the waste gangue residues are recycled, and the waste is changed into valuable.
Description
Technical Field
The invention relates to the technical field of coal gangue regeneration slope protection bricks, in particular to a coal gangue regeneration slope protection brick and a preparation method thereof.
Background
Coal gangue is the coal mining processAnd solid waste discharged in the coal washing process, which is a black and gray rock with lower carbon content and harder than coal and is associated with the coal bed in the coal forming process. Comprises tunneling waste rocks in the tunneling process of a roadway, waste rocks extracted from a top plate, a bottom plate and an interlayer in the mining process, and washing waste rocks extracted in the coal washing process. The main component of which is Al2O3、SiO2And in addition, Fe in different quantities2O3、CaO、MgO、Na2O、K2O、P2O5、SO3And trace rare elements (gallium, vanadium, titanium, cobalt). China stores about 1000Mt of coal gangue over the years, and continues to discharge about 100Mt every year, not only accumulating land, but also spontaneously combusting to pollute air or cause fire. The coal gangue is not used for disposal, and occupies a large area of land. The escape or leaching of sulfides in the coal gangue can pollute the atmosphere, farmlands and water bodies. The gangue dump can also be spontaneous combustion to cause fire, or collapse in rainy season, and cause disasters due to river congestion. The coal gangue accumulated in China reaches more than 10 hundred million tons, and 1 hundred million tons of coal gangue are discharged every year. In order to eliminate pollution, the treatment and utilization of coal gangue are valued in many countries since the 60 s. The following routes are available:
recovery of coal and pyrite: good coal is washed from coal gangue by a simple process, poor coal is selected from the coal gangue by screening, and pyrite is selected at the same time. Or the pyrite, the washing coal and the middlings are recovered from the flow of a jigger-plane shaking table for coal dressing. The recovered coal can be used as fuel of power boiler, the washing waste rock can be used as building material, and the pyrite can be used as chemical raw material.
Secondly, the generator is used for generating electricity: the mixed combustion power generation is mainly realized by using the washed middlings and the washed gangue. China has used a boiling furnace to burn a mixture of washed middlings and washed gangue (the calorific value is about 2000 kilocalories per kilogram) to generate electricity. The slag can be used for producing slag bricks and slag cement. There are more than 10 such plants in japan; the heat productivity of the mixture of the medium coal and the gangue is generally 3500 kilocalories per kilogram; when the firepower is insufficient, heavy oil is used for supporting combustion. The republic of Germany and the Federal republic of Dutch and the Netherlands build coal mine self-service power plants and coal preparation plants together to generate electricity by using middlings, coal slime and coal gangue. The calorific capacity of the coal gangue is tested by using a special instrument, and the microcomputer calorimeter can meet the requirement of the calorific capacity test.
Manufacturing a building material: instead of clay, the brick can be used as raw material for making brick, and can be used for digging less fertile farmland. When the brick is fired, the coal can be saved by using the combustible material of the coal gangue. The coal gangue can partially or completely replace clay raw materials to produce ordinary cement. The coal gangue after spontaneous combustion or artificial combustion has certain activity, and can be used as an active mixed material of cement to produce ordinary portland cement (the mixing amount is less than 20%), pozzolanic cement (the mixing amount is 20-50%) and low-clinker cement (the mixing amount is more than 50%). It can also be directly ground into clinker-free cement with lime and gypsum in a proper proportion, and can be used as cementing material, and the building materials of concrete building blocks or concrete hollow building blocks, etc. can be made by using boiling furnace slag as aggregate or using pebble and boiling furnace slag as coarse and fine aggregates. The special coal gangue in British, Belgium and other countries replaces siliceous raw materials to produce cement.
Although the coal gangue can be used for building materials, the unprocessed coal gangue has a plurality of disadvantages and is directly used for cement production, and the coal gangue has the following hazards: the traditional non-calcined coal gangue is easy to collapse after being foamed by the porous foamed brick, has low compressive strength, long demoulding and curing time and high curing cost, and is not beneficial to large-scale production of factories and enterprises.
Therefore, the coal gangue is required to be reformed while being utilized, otherwise, the coal gangue cannot be correctly used in the actual life and can be accumulated in the field, and the effect of waste utilization cannot be achieved. How to utilize the waste of coal gangue is a serious problem at present.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a coal gangue regeneration slope protection brick, wherein a plurality of additives are added into coal gangue waste residues to serve as the components of the coal gangue regeneration slope protection brick, so that the performance of coal gangue is excellent, the problem that the conventional coal gangue porous foaming brick is easy to collapse after foaming is solved, and the compressive strength is improved; the demolding and curing time is greatly shortened, the curing cost is saved, and the large-scale production of factory enterprises is facilitated; the waste gangue residues are recycled, and the waste is changed into valuable.
The invention is realized by the following steps:
one purpose of the invention is to provide a coal gangue regeneration slope protection brick, which comprises the following raw materials in parts by weight: 300-400 parts of cement, 300-400 parts of mountain flour, 250-350 parts of uncalcined coal gangue, 2-5 parts of accelerator, 2-5 parts of aluminum powder, 0.1-1 part of thickener, 10-30 parts of early strength agent and 2-18 parts of beta-sodium naphthalene sulfonate formaldehyde condensate.
Preferably, the coal gangue regeneration slope protection brick comprises the following raw materials in parts by weight: 340-360 parts of cement, 340-360 parts of mountain flour, 290-310 parts of uncalcined coal gangue, 3-4 parts of an accelerator, 3-4 parts of aluminum powder, 0.3-0.7 part of a thickening agent, 15-25 parts of an early strength agent and 5-15 parts of a beta-sodium naphthalene sulfonate formaldehyde condensate.
Most preferably, the coal gangue regeneration slope protection brick comprises the following raw materials in parts by weight: 350 parts of cement, 350 parts of mountain flour, 300 parts of uncalcined coal gangue, 3.5 parts of accelerant, 3.7 parts of aluminum powder, 0.5 part of thickening agent, 19.5 parts of early strength agent and 10 parts of beta-sodium naphthalenesulfonate formaldehyde condensate.
Preferably, the accelerator comprises sodium hexametaphosphate.
Preferably, the thickener comprises at least one of gypsum, ethoxylated sodium alkyl sulfide and sodium dodecyl sulfate.
Preferably, the early strength agent comprises at least one of calcium formate, sodium sulfate, potassium sulfate, calcium sulfate and triisopropanolamine. The early strength agent can improve the early strength of the non-calcined coal gangue and has no obvious influence on the later strength.
Preferably, the early strength agent is a mixture of calcium sulfate and triisopropanolamine, and the weight ratio of calcium sulfate: the mass ratio of triisopropanolamine is 10-20: 4 to 5.
The invention also aims to provide a preparation method of the coal gangue regenerated slope protection brick, which comprises the following steps:
step 1, weighing raw materials according to a formula, adding weighed cement, stone powder and uncalcined coal gangue into a stirring kettle, and uniformly stirring to obtain mixed slurry;
step 2, adding an accelerator, an early strength agent, a beta-sodium naphthalenesulfonate formaldehyde condensate, a thickening agent and aluminum powder into the mixed slurry for mixing and stirring to uniformly mix the materials until the surface of the mixture has no metallic luster, and stopping stirring;
and 3, pouring the mixture in the stirring kettle into a mold, drying until the mixture is not foamed any more, taking out, and naturally drying at normal temperature.
Compared with the prior art, the invention has the following advantages and effects:
1. according to the coal gangue regenerated slope protection brick provided by the invention, the raw materials have a mutual synergistic effect, and the thickening agent increases the viscosity; the early strength agent can improve the early strength of the non-calcined coal gangue; the accelerator can promote the hardening of cement; the aluminum powder can promote the foaming of the coal gangue and increase the porosity; on the premise of reducing the weight of the building block brick, the foam holes are increased, which is beneficial to the evaporation of water; and a beta-sodium naphthalenesulfonate formaldehyde condensate is further added, and the raw materials are matched with each other, so that the compressive strength of the coal gangue building block brick is enhanced, and the demolding time of the coal gangue building block brick is obviously shortened.
2. The industrial solid waste coal gangue is recycled, the prepared building block brick is mainly used for paving or greening, the production process is free of steam curing, and the brick is more green and environment-friendly compared with the traditional firing process.
3. The coal gangue regeneration slope protection brick provided by the invention has the advantages that the strength of the building brick prepared from the raw material is enhanced, the demoulding time is shortened, and specifically:
(1) in the experimental example, compared with a blank control group, the strength of the coal gangue building block brick can be improved by adding the beta-sodium naphthalenesulfonate formaldehyde condensate; solves the problem that the traditional gangue porous foaming brick is easy to collapse after foaming, and improves the compressive strength.
(2) In the experimental example of the invention, compared with a blank control group, the demolding and curing time is greatly shortened, the curing cost is saved, and the large-scale production of factory enterprises is facilitated.
(3) The prepared building block brick is a coal gangue steam-curing-free porous foamed brick, has good water permeability, accords with the concept of a cavernous city, and can be used for relevant municipal construction.
Drawings
FIG. 1 is a Scanning Electron Microscope (SEM) image of an uncalcined coal gangue as provided in an experimental example of the present invention;
fig. 2 is a Scanning Electron Microscope (SEM) image of the brick provided in example 1 of the present invention.
Detailed Description
Example 1
1. A coal gangue regeneration slope protection brick comprises the following raw materials in parts by weight: 350 parts of cement, 350 parts of mountain flour, 300 parts of uncalcined coal gangue, 3.5 parts of accelerant (sodium hexametaphosphate), 3.7 parts of aluminum powder, 0.5 part of thickening agent (gypsum), 19.5 parts of early strength agent (calcium sulfate) and 10 parts of beta-sodium naphthalenesulfonate formaldehyde condensate.
2. The preparation method of the coal gangue regenerated slope protection brick comprises the following steps:
step 1, weighing raw materials according to a formula, adding weighed cement, stone powder and uncalcined coal gangue into a stirring kettle, and uniformly stirring to obtain mixed slurry;
step 2, adding an accelerator into the mixed slurry, stirring, then sequentially adding an early strength agent and a beta-sodium naphthalenesulfonate formaldehyde condensate, adding a part of water stirrer for stirring, then adding a thickening agent under a stirring state, then adding a certain amount of water to make the viscosity of the stirring kettle consistent with the initial viscosity, adding aluminum powder, stirring again to make the materials uniformly mixed until the surface of the mixture has no metallic luster, and stopping stirring;
and 3, pouring the mixture in the stirring kettle into a mold, baking for 30 minutes in a baking oven at 50 ℃ until the mixture is not foamed any more, taking out and naturally drying at normal temperature.
Example 2
A coal gangue regeneration slope protection brick comprises the following raw materials in parts by weight: 300 parts of cement, 300 parts of stone powder, 250 parts of uncalcined coal gangue, 2 parts of accelerator (sodium hexametaphosphate), 2 parts of aluminum powder, 0.1 part of thickener (sodium dodecyl sulfate), 10 parts of early strength agent (sodium sulfate) and 2 parts of beta-sodium naphthalene sulfonate formaldehyde condensate. The preparation method of the coal gangue regenerated slope protection brick is the same as that of the example 1.
Example 3
A coal gangue regeneration slope protection brick comprises the following raw materials in parts by weight: 400 parts of cement, 400 parts of stone powder, 350 parts of uncalcined coal gangue, 5 parts of accelerator (sodium hexametaphosphate), 5 parts of aluminum powder, 1 part of thickener (ethoxylated sodium alkyl sulfide), 30 parts of early strength agent (potassium sulfate) and 18 parts of beta-sodium naphthalene sulfonate formaldehyde condensate. The preparation method of the coal gangue regenerated slope protection brick is the same as that of the example 1.
Example 4
A coal gangue regeneration slope protection brick comprises the following raw materials in parts by weight: 340 parts of cement, 340 parts of mountain flour, 290 parts of uncalcined coal gangue, 3 parts of an accelerant (sodium hexametaphosphate), 3 parts of aluminum powder, 0.3 part of a thickening agent (gypsum and ethoxylated sodium alkyl sulfide), 15 parts of an early strength agent (calcium sulfate) and 5 parts of a beta-sodium naphthalenesulfonate formaldehyde condensate. The preparation method of the coal gangue regenerated slope protection brick is the same as that of the example 1.
Example 5
A coal gangue regeneration slope protection brick comprises the following raw materials in parts by weight: 360 parts of cement, 360 parts of stone powder, 310 parts of uncalcined coal gangue, 4 parts of accelerator (sodium hexametaphosphate), 4 parts of aluminum powder, 0.7 part of thickening agent (ethoxylated sodium alkyl sulfide and sodium dodecyl sulfate), 25 parts of early strength agent (triisopropanolamine) and 15 parts of beta-sodium naphthalene sulfonate formaldehyde condensate. The preparation method of the coal gangue regenerated slope protection brick is the same as that of the example 1.
Example 6
This example is performed except that the early strength agent is replaced with a mixture of calcium sulfate and triisopropanolamine, and the calcium sulfate: the mass ratio of triisopropanolamine is 15: 4.5 otherwise, the same procedure is followed as in example 1 (the total amount of calcium sulfate + triisopropanolamine is the same as the total amount of the early strength agent used in example 1). Specifically, the method comprises the following steps: 350 parts of cement, 350 parts of mountain flour, 300 parts of uncalcined coal gangue, 3.5 parts of accelerant, 3.7 parts of aluminum powder, 0.5 part of thickening agent, 15 parts of calcium sulfate, 4.5 parts of triisopropanolamine and 10 parts of beta-sodium naphthalene sulfonate formaldehyde condensate.
Example 7
This example is performed except that the early strength agent is replaced with a mixture of calcium sulfate and triisopropanolamine, and the calcium sulfate: the mass ratio of triisopropanolamine is 10: in addition to example 5, the same procedure is followed as in example 1 (the total amount of calcium sulfate + triisopropanolamine is the same as the total amount of the early strength agent used in example 1). Specifically, the method comprises the following steps: 350 parts of cement, 350 parts of mountain flour, 300 parts of uncalcined coal gangue, 3.5 parts of accelerant, 3.7 parts of aluminum powder, 0.5 part of thickening agent, 13 parts of calcium sulfate, 6.5 parts of triisopropanolamine and 10 parts of beta-sodium naphthalene sulfonate formaldehyde condensate.
Example 8
This example is performed except that the early strength agent is replaced with a mixture of calcium sulfate and triisopropanolamine, and the calcium sulfate: the mass ratio of triisopropanolamine is 20: in addition to 4, the same procedure is followed as in example 1 (the total amount of calcium sulfate + triisopropanolamine is the same as the total amount of the early strength agent used in example 1). Specifically, the method comprises the following steps: 350 parts of cement, 350 parts of mountain flour, 300 parts of uncalcined coal gangue, 3.5 parts of accelerator, 3.7 parts of aluminum powder, 0.5 part of thickener, 16.25 parts of calcium sulfate, 3.25 parts of triisopropanolamine and 10 parts of beta-sodium naphthalenesulfonate formaldehyde condensate.
Comparative example 1
The raw materials and contents and preparation method were the same as in example 1 except that no sodium β -naphthalenesulfonate formaldehyde condensate was added.
Comparative example 2
The comparative example was conducted in the same manner as in example 1 except that the sodium β -naphthalenesulfonate formaldehyde condensate was replaced with the same amount of sodium lignosulfonate.
Comparative example 3
Except that the beta-sodium naphthalenesulfonate formaldehyde condensate is replaced by the same amount of polycarboxylic acid water reducer, the rest raw materials, the content and the preparation method of the comparative example are the same as those of the example 1.
Comparative example 4
This comparative example is the same as example 1 except that the calcium sulfate early strength agent is replaced with an equivalent amount of triisopropanolamine.
Comparative example 5
The comparative example is the same as example 1 except that the calcium sulfate early strength agent is replaced with an equal amount of calcium formate.
Comparative example 6
The comparative example is the same as example 1 except that the calcium sulfate early strength agent is replaced with an equal amount of sodium sulfate.
Comparative example 7
This comparative example except that the early strength agent was replaced with a mixture of calcium sulfate and triisopropanolamine, and the ratio of calcium sulfate: the mass ratio of triisopropanolamine is 6: in addition to 6, the same procedure is followed as in example 1 (the total amount of calcium sulfate + triisopropanolamine is the same as the total amount of the early strength agent used in example 1). Specifically, the method comprises the following steps: 350 parts of cement, 350 parts of mountain flour, 300 parts of uncalcined coal gangue, 3.5 parts of accelerant, 3.7 parts of aluminum powder, 0.5 part of thickening agent, 9.75 parts of calcium sulfate, 9.75 parts of triisopropanolamine and 10 parts of beta-sodium naphthalenesulfonate formaldehyde condensate.
Comparative example 8
This comparative example except that the early strength agent was replaced with a mixture of calcium sulfate and triisopropanolamine, and the ratio of calcium sulfate: the mass ratio of triisopropanolamine is 24: in addition to 2, the same procedure is followed as in example 1 (the total amount of calcium sulfate + triisopropanolamine is the same as the total amount of the early strength agent used in example 1). Specifically, the method comprises the following steps: 350 parts of cement, 350 parts of mountain flour, 300 parts of uncalcined coal gangue, 3.5 parts of accelerant, 3.7 parts of aluminum powder, 0.5 part of thickening agent, 18 parts of calcium sulfate, 1.5 parts of triisopropanolamine and 10 parts of beta-sodium naphthalene sulfonate formaldehyde condensate.
Experimental example 1
The compression strength and the demolding time of the building blocks prepared in the examples 1 to 5 and the comparative examples 1 to 3 are improved. The test results are shown in table 1 below:
TABLE 1
| Item | Compressive strength (Mpa) | Time to demold |
| Example 1 | 4.52 | 36h |
| Example 2 | 2.43 | 42h |
| Example 3 | 2.73 | 40h |
| Example 4 | 3.51 | 39h |
| Example 5 | 3.68 | 37h |
| Comparative example 1 | 1.50 | 72h |
| Comparative example 2 | 1.87 | 65h |
| Comparative example 3 | 1.93 | 58h |
As can be seen from Table 1, the addition of the sodium β -naphthalenesulfonate formaldehyde condensate significantly increases the compressive strength of the block brick compared to comparative example 1. Compared with the comparative examples 2-3, the addition of other water reducing agents can increase the compressive strength of the block brick but the increase is smaller, and the effect is not as good as that of the addition of the beta-sodium naphthalene sulfonate formaldehyde condensate. Examples 4 and 5 are preferred examples. Example 1 is the best mode.
Comparative example 1 the addition of the sodium beta-naphthalenesulfonate formaldehyde condensate significantly reduced the demold time of the block brick. From comparative examples 2 and 3, it can be seen that the addition of other water reducing agents is not as effective in reducing the demold time of the block brick as the addition of the sodium β -naphthalenesulfonate formaldehyde condensate. Further, it is understood that the best example is embodiment 1, and the mold release time is 36 hours at the shortest.
Experimental example 2 selection of different early strength Agents
The strength of the bricks prepared in examples 1, 6 to 8 and comparative examples 4 to 8 was measured and the demold time was calculated, and the results are shown in table 2 below:
TABLE 2
| Item | Compressive strength (Mpa) | Time to demold |
| Example 1 | 4.52 | 36h |
| Example 6 | 5.48 | 34h |
| Example 7 | 5.13 | 35h |
| Example 8 | 5.01 | 36h |
| Comparative example 4 | 3.36 | 40h |
| Comparative example 5 | 3.27 | 40h |
| Comparative example 6 | 3.63 | 40h |
| Comparative example 7 | 4.13 | 38h |
| Comparative example 8 | 3.42 | 39h |
As can be seen from table 2, the early strength agent is preferably a mixture of calcium sulfate and triisopropanolamine, and the ratio of calcium sulfate: the mass ratio of triisopropanolamine is 10-20: 4 to 5. The coal gangue building block brick is matched with other raw materials such as a beta-sodium naphthalene sulfonate formaldehyde condensate and the like, so that the compressive strength of the coal gangue building block brick is obviously enhanced, and the demoulding time is shortened.
It should be noted that the cement, stone powder and uncalcined coal gangue used above are provided by jinmen's mingxiang mechanical responsibility limited company; the accelerator, aluminum powder, thickener, early strength agent, beta-sodium naphthalene sulfonate formaldehyde condensate and the like are provided by the national medicine group chemical reagent company Limited.
The invention is not to be considered as limited to the particular embodiments shown, but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (9)
1. The coal gangue regeneration slope protection brick is characterized by comprising the following raw materials in parts by weight: 300-400 parts of cement, 300-400 parts of mountain flour, 250-350 parts of uncalcined coal gangue, 2-5 parts of accelerator, 2-5 parts of aluminum powder, 0.1-1 part of thickener, 10-30 parts of early strength agent and 2-18 parts of beta-sodium naphthalene sulfonate formaldehyde condensate; the early strength agent is a mixture of calcium sulfate and triisopropanolamine, and the calcium sulfate: the mass ratio of triisopropanolamine is 10-20: 4 to 5.
2. The coal gangue regeneration slope protection brick as claimed in claim 1, which comprises the following raw materials in parts by weight: 340-360 parts of cement, 340-360 parts of mountain flour, 290-310 parts of uncalcined coal gangue, 3-4 parts of an accelerator, 3-4 parts of aluminum powder, 0.3-0.7 part of a thickening agent, 15-25 parts of an early strength agent and 5-15 parts of a beta-sodium naphthalene sulfonate formaldehyde condensate.
3. The coal gangue regeneration slope protection brick as claimed in claim 1, which comprises the following raw materials in parts by weight: 350 parts of cement, 350 parts of mountain flour, 300 parts of uncalcined coal gangue, 3.5 parts of accelerant, 3.7 parts of aluminum powder, 0.5 part of thickening agent, 19.5 parts of early strength agent and 10 parts of beta-sodium naphthalenesulfonate formaldehyde condensate.
4. The coal gangue regeneration slope protection brick as claimed in claim 1, wherein the accelerant comprises sodium hexametaphosphate.
5. The coal gangue regeneration slope protection brick as claimed in claim 1, wherein the thickener comprises at least one of gypsum, ethoxylated sodium alkyl sulfide, and sodium dodecyl sulfate.
6. The preparation method of the coal gangue regeneration slope protection brick as set forth in any one of claims 1 to 5, characterized in that the method comprises the following steps:
step 1, weighing raw materials according to a formula, adding weighed cement, stone powder and uncalcined coal gangue into a stirring kettle, and uniformly stirring to obtain mixed slurry;
step 2, adding an accelerator, an early strength agent, a beta-sodium naphthalenesulfonate formaldehyde condensate, a thickening agent and aluminum powder into the mixed slurry for mixing and stirring to uniformly mix the materials until the surface of the mixture has no metallic luster, and stopping stirring;
and 3, pouring the mixture in the stirring kettle into a mold, drying until the mixture is not foamed any more, taking out, and naturally drying at normal temperature.
7. The method for preparing the coal gangue regeneration slope protection brick as claimed in claim 6, wherein in the step 2, the accelerant is added into the mixed slurry first, the mixed slurry is stirred, then the early strength agent and the beta-sodium naphthalenesulfonate formaldehyde condensate are sequentially added, a part of water stirrer is added for stirring, then the thickening agent is added under the stirring state, then some water is added to make the viscosity of the stirring kettle consistent with the initial viscosity, the aluminum powder is added, the stirring is carried out again to make the materials mixed uniformly until the surface of the mixture has no metallic luster, and the stirring is stopped.
8. The preparation method of the coal gangue regeneration slope protection brick as claimed in claim 6, wherein the stirring speed in the step 2 is 300-700 r/min, and the stirring time is 1-30 min.
9. The preparation method of the coal gangue regeneration slope protection brick as claimed in claim 8, wherein the drying step in the step 3 is specifically: baking in an oven at 50 ℃ for 30 minutes.
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