CN111875332A - Method for preparing carbonized brick by wet grinding of carbide slag - Google Patents
Method for preparing carbonized brick by wet grinding of carbide slag Download PDFInfo
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- CN111875332A CN111875332A CN202010771454.4A CN202010771454A CN111875332A CN 111875332 A CN111875332 A CN 111875332A CN 202010771454 A CN202010771454 A CN 202010771454A CN 111875332 A CN111875332 A CN 111875332A
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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
- C04B28/144—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 a flue gas desulfurization product
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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
- C04B40/00—Processes, in general, for influencing or modifying the properties of mortars, concrete or artificial stone compositions, e.g. their setting or hardening ability
- C04B40/02—Selection of the hardening environment
- C04B40/0231—Carbon dioxide hardening
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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 provides a method for preparing carbonized bricks by wet grinding of carbide slag, which comprises the following steps: carrying out wet grinding on 150-300 parts of carbide slag and 75-150 parts of water to realize refinement of carbide slag particles and high alkalinity of a liquid phase; and (2) using 120-200 parts of wet-grinding carbide slag slurry, 10-35 parts of gypsum and 50-120 parts of slag as a cementing material, adding 420-865 parts of fine aggregate and 0-18 parts of water, fully stirring uniformly, pressing and forming the uniformly stirred raw materials, and curing in a carbonization chamber to obtain the wet-grinding carbide slag carbonized brick. The method can solidify the gas carbon dioxide, and reduce the pollution of industrial waste gas to the environment; the advantage that the wet-grinding carbide slag is easy to carbonize is utilized, the wet-grinding carbide slag is easy to react with carbon dioxide to form calcium carbonate, and the precipitation and crystallization growth have cohesive force; the prepared brick has high strength and short curing period, improves the production efficiency and can effectively replace the ordinary brick for construction.
Description
Technical Field
The invention relates to the technical field of comprehensive utilization of resources, in particular to a method for preparing carbonized bricks by wet grinding of carbide slag.
Background
Carbide slag is a by-product of acetylene gas generated by adding water to calcium carbide. The chemical reaction formula is as follows:
CaC2+2H2O＝C2H2+Ca(OH)2+127kJ
according to calculation, each 1t of standard calcium carbide is used for generating acetylene gas (C)2H2) Approximately 1.16t of carbide slag is produced. According to the introduction of data, about 135t of calcium carbide for synthesizing acetylene every year in China generates 150 ten thousand of calcium carbide slag, so that enterprises and environmental protection departments worry about the palpitation and reasonably solve the problems of storage, use and the like of the calcium carbide slag. If the carbide slag is utilized in such a large amount, obvious social and economic benefits can be obtained.
The carbide slag is gray fine powder, the main component of the carbide slag is calcium hydroxide, the carbide slag exists in a crystal form, is relatively coarse, and is wrapped with other substances, and the gelation characteristic is difficult to be formed by reaction of hydrated lime and carbon dioxide in air to form calcium carbonate, so that the activity of the carbide slag is excited by wet grinding treatment, the particle refinement and the liquid phase high alkalinity of the carbide slag are realized, and the carbonizability of the carbide slag is increased. The prepared carbonized brick has high strength and good durability, can be used as various forms such as carbonized plates, artificial fish reefs, building blocks and the like, can replace some existing building materials, and is widely applied.
The invention patent CN107879704A discloses a preparation method of a composite steel slag carbonized brick, which is a method for preparing the carbonized brick by taking steel slag as a main raw material. The method is characterized in that: mixing steel slag, kerosene and a grinding aid, performing ball milling, igniting, cooling to obtain combustion slag, crushing and sieving the obtained combustion slag to obtain pretreated steel slag powder, stirring and mixing aggregate, the pretreated steel slag powder, slaked lime and a dispersion liquid, pouring and forming, standing at constant temperature and constant humidity to obtain a green brick, performing autoclaved curing on the green brick, fumigating with vinegar to obtain a fumigated green brick, transferring the fumigated green brick into a carbonization box, carbonizing at constant temperature and constant humidity, and discharging to obtain the composite steel slag carbonized brick. Although the technology can consume the steel slag, the process flow is complex, the efficiency is low, and chemical agents such as table vinegar, kerosene, grinding aid and the like are also needed, so that the energy conservation, emission reduction and cost reduction are not facilitated; in addition, the process flow also requires steam normal pressure maintenance or steam pressure maintenance, which causes harsh requirements on production conditions and overhigh capital construction and maintenance costs.
The invention patent CN201510377931.8 discloses a method for preparing a building brick by directly carbonizing slag. Grinding and sieving the slag, adding a proper amount of water, fully and uniformly stirring, and filling the uniformly mixed raw materials into a mold for molding to prepare a brick blank. And (3) putting the prepared green body into a reaction kettle, introducing carbon dioxide with different pressures into the reaction kettle for curing (the curing condition is that the humidity is 80-95 percent and the temperature is 30-150 ℃), and curing for 12-168 hours to prepare the hardened brick body. The method can well solidify gaseous carbon dioxide, reduce the pollution of industrial waste gas to the environment, consume slag and promote the utilization of industrial solid waste. The early compressive strength is small, a reaction kettle is needed, the steps are complicated, and the large-scale production and application cannot be realized.
Global warming is mainly dependent on CO2Accumulated emissions of until 2019, CO produced by global combustion of fossil fuels2Emissions will be as high as 368 hundred million tons. (from the U.S. scientific news website 2019, 12 months and 4 days). China is a big country for cement production, and 1 ton of CO is adopted in the clinker calcining process2Per 1 ton cement clinker estimation, CO annually2The total emission amount is about 17 hundred million tons, and accounts for 7 percent of the total emission amount of the whole world.
If the carbide slag which is not effectively utilized is carbonized to prepare useful materials, not only the waste is changed into valuable, but also the consumption of cement can be reduced, and CO in the cement production process is reduced2The carbon dioxide can be solidified in the production process of the carbonized brick, and the environmental pollution can be prevented.
Therefore, the invention aims to provide a method for preparing carbonized bricks by utilizing wet-milled carbide slag, which aims to solve the problems of low utilization rate of industrial solid waste carbide slag and environmental pollution, change waste into valuable and relieve the greenhouse effect; meanwhile, the technical problems that similar carbonized products are difficult to be industrially utilized, the preparation cost is high, the efficiency is low and the like are solved, and the added value of the product can be improved.
Disclosure of Invention
The technical scheme adopted for solving the problems in the prior art is as follows:
a method for preparing carbonized bricks by wet grinding of carbide slag is characterized by comprising the following steps:
step 1, adding 150-300 parts of carbide slag, 1/2 parts of water and 0.5-3 parts of grinding aid by mass into wet stirred grinding, and carrying out wet grinding at a rotation speed of 400r/min for 0.5-1 h in wet stirring grinding, wherein the ratio of grinding medium ceramic balls is 1.2mm to 0.8mm to 0.6mm to 2 to 4, so as to obtain wet-ground carbide slag slurry with a median particle size D (50) of 0.9-3 mu m;
step 2, mixing and stirring 120-200 parts of wet-milled carbide slag slurry, 5-35 parts of gypsum, 50-120 parts of slag, 420-865 parts of fine aggregate and 0-18 parts of water in the step 1 for 90-180 seconds to obtain mixed mortar;
step 3, weighing the mixed mortar obtained in the step 2, putting the mixed mortar into a forming die for press forming, wherein the forming pressure of the press forming is 2-35 MPa, the pressure maintaining time is 30-60s, and demoulding is carried out immediately after forming;
step 4, putting the test block formed and demoulded in the step 3 into a carbonization chamber with constant temperature and humidity for carbonization and maintenance, wherein CO is in the carbonization chamber2The pressure is 35-250 Pa, and CO is2The volume concentration is 17-23%, and the carbonized brick is obtained.
The carbide slag in the step 1 comprises calcium hydroxide, silicon dioxide, aluminum oxide, ferric oxide, magnesium oxide and the like, and the mass content of the calcium hydroxide in the carbide slag is 60-75%;
in the step 1, the grinding aid is one or more mixed solutions of a polycarboxylic acid water reducing agent, a calcium lignosulfonate water reducing agent and an aliphatic high-efficiency water reducing agent.
The gypsum in the step 2 is desulfurized gypsum or natural gypsum generated by a power plant or an iron and steel plant;
the fine aggregate in the step 2 is one or more of iron tailings, river sand, deposited sand, tailing sand and sand made of construction waste.
And (4) curing at the temperature of 20-40 ℃ for carbonization and curing, at the relative humidity of 60-100% for 2-6 h, and storing in an open air environment.
The carbonization chamber maintenance gas CO in the step 42The waste gas rich in carbon dioxide is discharged from a factory, wherein the volume fraction of the carbon dioxide accounts for 17-30%.
The reaction principle of the invention is as follows:
the carbide slag carbonization process is essentially as follows: granular calcium hydroxide absorbs carbon dioxide gas under appropriate moisture to form calcium carbonate, which in turn forms crystals (mainly calcite). The crystals grow and develop in the gaps, not only can fill the pores, but also can build each other or build with aggregates to form a net structure to finally form strength, so that the aim of preparing the carbonized brick after carbide slag carbonization is realized.
Of course, the reaction mechanism of this carbonization process is by no means so simple, involving a series of physical adsorption and diffusion processes. Most people accept the theory of gas-liquid-solid phase reaction, namely when the water content is proper, gaseous carbon dioxide diffuses through a capillary tube in carbide slag, and water dissolved in the wall of the capillary tube generates H2CO3It follows the following reaction:
CO2+H2O＝H2CO3
the carbonic acid formed is extremely unstable and a part of the carbonic acid is dissociated according to the following formula:
granular calcium hydroxide is dissolved in capillary and carbide slag surface water film to generate solution and dissociate according to the following formula:
Ca(OH)2＝Ca2++2OH-
the four ions in aqueous solution meet and react immediately according to the following formula:
Ca2++H++2OH-+HCO3-＝CaCO3↓+2H2O
the reaction process is completed in liquid phase through gas phase-liquid phase-solid phase interface, and the precipitated calcium carbonate is crystallized slowly in warm and wet condition and has cohesion for crystal growth.
The invention has the following advantages:
1. the raw material carbide slag utilized by the invention is industrial waste, the cost of the raw material is lower, the process equipment is simple, and the industrial production is facilitated.
2. The slag carbonized brick prepared by the method has high compressive strength, 1d compressive strength of 17MPa, 3d compressive strength of more than 30MPa and good volume stability, and can effectively replace common bricks.
3. The invention is carbonized in carbon dioxide atmosphere, can permanently solidify greenhouse gas carbon dioxide, relieve greenhouse effect, greatly reduce the consumption of cement and protect environment.
4. Because the activity of the original carbide slag is low, the calcium hydroxide crystals are relatively thick and thick, and are mutually wrapped with other substances, and the gelation property equivalent to that of hydrated lime is difficult to exert. Therefore, the wet grinding treatment is adopted to excite the activity of the calcium hydroxide, change the crystal morphology of the calcium hydroxide and promote Ca2+And OH-The dissolution of ions, the refinement and the high alkalinity of the carbide slag particles can accelerate the hydration rate and generate more compact calcium carbonate crystals. The calcium carbonate is endowed with great strength by forming a space network structure through precipitation and crystal growth, and meets the daily design requirements.
5. The hydration and carbonization processes can be accelerated by adding a certain amount of industrial by-products of gypsum and slag, researches show that the gypsum plays a role in catalyzing a system, the development of the strength of a test block can be promoted by a small amount of gypsum, and the slag has potential pozzolanic activity and is beneficial to the development of the strength of a carbonized brick.
6. Because the durability of the carbide slag is poor, the cost can be saved and the density of the building material can be reduced by adding the fine aggregate, and when the fine aggregate is the iron tailings of the ultrabasic rock, the function also comprises the synergistic carbon fixation.
Drawings
FIG. 1 is a flow chart of the method of the present invention.
Detailed Description
The technical scheme of the invention is further described in detail by the following embodiments and the accompanying drawings:
example 1:
step 1, adding 150 parts of carbide slag, 75 parts of water and 0.5-3 parts of grinding aid into a wet stirring mill, and wet-milling at a rotation speed of 400r/min for 0.5, wherein the ratio of a grinding medium ceramic ball to a grinding medium ceramic ball is 1.2mm to 0.8mm to 0.6mm to 2 to 4, so as to obtain wet-milled carbide slag slurry with a median particle size D (50) of 3 mu m;
step 2, mixing 120 parts of wet-milled carbide slag slurry, 5 parts of desulfurized gypsum, 50 parts of slag, 420 parts of river sand and iron tailings and stirring for 90 seconds to obtain mixed mortar;
step 3, weighing the mixed mortar obtained in the step 2, putting the mixed mortar into a forming die for press forming, wherein the forming pressure of the press forming is 2MPa, the pressure maintaining time is 30s, and demoulding is carried out immediately after the forming;
step 4, putting the test block formed and demoulded in the step 3 into a carbonization chamber with constant temperature and humidity for carbonization and maintenance, wherein CO is in the carbonization chamber2Pressure range of 35Pa, CO2The volume concentration is 17 percent, and the curing time is 2 hours, thus obtaining the carbonized brick.
Example 2
Step 1, adding 175 parts of carbide slag into 87.5 parts of water, 2 parts of a mixed solution of a polycarboxylic acid water reducer and an aliphatic high-efficiency water reducer, adding the mixture into a wet stirring mill, and wet-milling the mixture at a rotation speed of 400r/min for 0.8h, wherein the ratio of a grinding medium ceramic ball to the grinding medium ceramic ball is 1.2mm:0.8mm:0.6 mm: 2:4:4, so as to obtain wet-milled carbide slag slurry with the median particle size D (50) of 2.3 mu m;
step 2, taking 150 parts of the wet-milled carbide slag slurry in the step 1, 15 parts of phosphogypsum, 85 parts of slag, 600 parts of river sand, sediment sand mixed fine aggregate and 10 parts of water, and mixing and stirring for 90-180 seconds to obtain mixed mortar;
step 3, weighing the mixed mortar obtained in the step 2, putting the mixed mortar into a forming die for press forming, wherein the forming pressure of the press forming is 2-35 MPa, the pressure maintaining time is 30-60s, and demoulding is carried out immediately after forming;
step 4, putting the test block formed and demoulded in the step 3 into a carbonization chamber with constant temperature and humidity for carbonization and maintenance, wherein CO is in the carbonization chamber2The pressure is 35-250 Pa, and CO is2The volume concentration is 17-23%, and the curing time is 4h, thus obtaining the carbonized brick.
Example 3
Step 1, adding 112.5 parts of water, 2 parts of a polycarboxylic acid water reducer and a calcium lignosulfonate water reducer into 225 parts of carbide slag, adding the mixture into a wet stirring mill, and wet-milling for 1h at a rotation speed of 400r/min, wherein the ratio of a grinding medium ceramic ball is 1.2mm to 0.8mm to 0.6mm to 2 to 4, so as to obtain wet-milled carbide slag slurry with a median particle size D (50) of 0.9 mu m;
step 2, taking 175 parts of the wet-milled carbide slag slurry in the step 1, mixing 27 parts of a mixture of desulfurized gypsum and phosphogypsum, 100 parts of slag, 731 parts of river sand and tailing sand, mixing fine aggregate and 14 parts of water, and mixing and stirring for 120s to obtain mixed mortar;
step 3, weighing the mixed mortar obtained in the step 2, putting the mixed mortar into a forming die for press forming, wherein the forming pressure of the press forming is 30MPa, the pressure maintaining time is 45s, and demoulding is carried out immediately after the forming;
step 4, putting the test block formed and demoulded in the step 3 into a carbonization chamber with constant temperature and humidity for carbonization and maintenance, wherein CO is in the carbonization chamber2Pressure range of 200Pa, CO2The volume concentration is 19 percent, and the curing time is 5 hours, thus obtaining the carbonized brick.
Example 4
Step 1, adding 150 parts of water and 3 parts of aliphatic superplasticizer into 300 parts of carbide slag, wet-grinding in a wet stirring mill at a rotation speed of 400r/min for 1h to obtain wet-ground carbide slag slurry with a median particle size D (50) of 1.8 mu m, wherein the ratio of grinding medium ceramic balls is 1.2mm to 0.8mm to 0.6mm to 2:4 to 4;
step 2, mixing and stirring 200 parts of the wet-milled carbide slag slurry in the step 1, 35 parts of titanium gypsum, 120 parts of slag, 865 parts of river sand and 18 parts of sand fine mixed fine aggregate made of construction waste and 18 parts of water for 180 seconds to obtain mixed mortar;
step 3, weighing the mixed mortar obtained in the step 2, putting the mixed mortar into a forming die for press forming, wherein the forming pressure of the press forming is 35MPa, the pressure maintaining time is 60s, and demoulding is carried out immediately after the forming;
step 4, putting the test block formed and demoulded in the step 3 into a carbonization chamber with constant temperature and humidity for carbonization and maintenance, wherein CO is in the carbonization chamber2Pressure range of 250Pa, CO2The volume concentration is 23 percent, and the curing time is 6 hours, thus obtaining the carbonized brick.
Table 1 shows the values of the compressive strength of the carbonized bricks obtained in examples 1 to 4
As can be seen from the table of compressive strength values for the carbonized bricks, the compressive strength in both early and late stages of example 3 is optimal. The 1d compressive strength can reach 15.3MPa, the construction requirement is met, and the later strength is not inverted and contracted. This may be related to the particle size of the wet ground carbide slag slurry, the smaller the particle size of the wet ground carbide slag, the stronger the activation to the carbide slag and the higher the early strength. From the analysis of reaction mechanism, the original carbide slag has low activity, the calcium hydroxide crystals are relatively coarse and are mutually wrapped with other substances, the better gelation property is difficult to exert, the wet grinding treatment stimulates the activity of the carbide slag, the crystal morphology of the main component calcium hydroxide in the carbide slag is changed, and the Ca is promoted2+And OH-The dissolution of ions, the refinement and the high alkalinity of the carbide slag particles can accelerate the hydration rate, and the precipitation and the crystal growth form a more compact calcium carbonate space network structure, so that the calcium carbonate has great strength and meets the daily design requirements.
The protective scope of the present invention is not limited to the above-described embodiments, and it is apparent that various modifications and variations can be made to the present invention by those skilled in the art without departing from the scope and spirit of the present invention. It is intended that the present invention cover the modifications and variations of this invention provided they come within the scope of the appended claims and their equivalents.
Claims (7)
1. A method for preparing carbonized bricks by wet grinding of carbide slag is characterized by comprising the following steps:
step 1, adding 150-300 parts of carbide slag, 1/2 parts of water and 0.5-3 parts of grinding aid by mass into wet stirred grinding, and carrying out wet grinding at a rotation speed of 400r/min for 0.5-1 h in wet stirring grinding, wherein the ratio of grinding medium ceramic balls is 1.2mm to 0.8mm to 0.6mm to 2 to 4, so as to obtain wet-ground carbide slag slurry with a median particle size D (50) of 0.9-3 mu m;
step 2, mixing and stirring 120-200 parts of wet-milled carbide slag slurry, 5-35 parts of gypsum, 50-120 parts of slag, 420-865 parts of fine aggregate and 0-18 parts of water in the step 1 for 90-180 seconds to obtain mixed mortar;
step 3, weighing the mixed mortar obtained in the step 2, putting the mixed mortar into a forming die for press forming, wherein the forming pressure of the press forming is 2-35 MPa, the pressure maintaining time is 30-60s, and demoulding is carried out immediately after forming;
step 4, putting the test block formed and demoulded in the step 3 into a carbonization chamber with constant temperature and humidity for carbonization and maintenance, wherein CO is in the carbonization chamber2The pressure is 35-250 Pa, and CO is2The volume concentration is 17-23%, and the carbonized brick is obtained.
2. The method for preparing carbonized bricks by wet grinding of carbide slag as claimed in claim 1, wherein: in the step 1, the calcium hydroxide in the carbide slag accounts for 60-75% by mass.
3. The method for preparing carbonized bricks by wet grinding of carbide slag as claimed in claim 1, wherein: in the step 1, the grinding aid is one or more mixed solutions of a polycarboxylic acid water reducing agent, a calcium lignosulfonate water reducing agent and an aliphatic high-efficiency water reducing agent.
4. The method for preparing carbonized bricks by wet grinding of carbide slag as claimed in claim 1, wherein: and the gypsum in the step 2 is desulfurized gypsum or natural gypsum produced by a power plant or an iron and steel plant.
5. The method for preparing carbonized bricks by wet grinding of carbide slag as claimed in claim 1, wherein: the fine aggregate in the step 2 is one or more of iron tailings, river sand, deposited sand, tailing sand and sand made of construction waste.
6. The method for preparing carbonized bricks by wet grinding of carbide slag as claimed in claim 1, wherein: and (4) curing at the temperature of 20-40 ℃ for carbonization and curing, at the relative humidity of 60-100% for 2-6 h, and storing in an open air environment.
7. The method for preparing carbonized bricks by wet grinding of carbide slag as claimed in claim 1, wherein: the carbonization chamber maintenance gas CO in the step 42The waste gas rich in carbon dioxide is discharged from a factory, wherein the volume fraction of the carbon dioxide accounts for 17-30%.
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| CN112429982A (en) * | 2020-12-10 | 2021-03-02 | 唐山三友氯碱有限责任公司 | Cementing material and mortar material based on wet-based alkaline residue-wet-based carbide slag and preparation method thereof |
| CN112679179A (en) * | 2020-12-10 | 2021-04-20 | 广东广业检测有限公司 | Carbonized brick containing industrial calcium slag and preparation method thereof |
| CN113526937A (en) * | 2021-08-19 | 2021-10-22 | 武汉理工大学 | Method for improving strength of calcium hydroxide carbonized hardened body and product |
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| CN115772013A (en) * | 2023-02-15 | 2023-03-10 | 河北工业大学 | Concrete containing silt powder and solidified carbide slag |
| CN116283139A (en) * | 2023-03-03 | 2023-06-23 | 湖北工业大学 | Autoclaved aerated concrete waste carbonization recycling method |
| CN116396019A (en) * | 2023-03-06 | 2023-07-07 | 湖北工业大学 | Preparation method of gel-reducing type alkali residue carbon-fixing concrete |
| CN116283139B (en) * | 2023-03-03 | 2024-04-19 | 湖北工业大学 | Autoclaved aerated concrete waste carbonization recycling method |
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