CN113735548B - All-solid-waste building material with boric sludge as main raw material and preparation method thereof - Google Patents
All-solid-waste building material with boric sludge as main raw material and preparation method thereof Download PDFInfo
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- CN113735548B CN113735548B CN202111302836.3A CN202111302836A CN113735548B CN 113735548 B CN113735548 B CN 113735548B CN 202111302836 A CN202111302836 A CN 202111302836A CN 113735548 B CN113735548 B CN 113735548B
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- boric sludge
- boron mud
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- magnesium sulfate
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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
- C04B28/30—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 magnesium cements or similar cements
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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
- C04B18/00—Use of agglomerated or waste materials or refuse as fillers for mortars, concrete or artificial stone; Treatment of agglomerated or waste materials or refuse, specially adapted to enhance their filling properties in mortars, concrete or artificial stone
- C04B18/04—Waste materials; Refuse
- C04B18/0481—Other specific industrial waste materials not provided for elsewhere in C04B18/00
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
- C04B2111/00017—Aspects relating to the protection of the environment
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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
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/91—Use of waste materials as fillers for mortars or concrete
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Organic Chemistry (AREA)
- Environmental & Geological Engineering (AREA)
- Civil Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Treatment Of Sludge (AREA)
Abstract
The invention discloses a full-solid waste building material taking boric sludge as a main raw material and a preparation method thereof, wherein the preparation method comprises the following steps: (1) b, boron mud pretreatment: drying the boric sludge, crushing and sieving by a 10-mesh sieve; (2) activating magnesium oxide in the boric sludge; (3) acidifying the boric sludge to prepare acidified boric sludge containing magnesium sulfate; (4) the boron mud is prepared from the boron mud solid waste building material to obtain boron mud building material finished products, such as baking-free bricks, building blocks, plates and the like, and can also be used for preparing other artware. The method effectively solves the problem of boron mud treatment, is simple to operate, has large boron mud usage amount, reduces the production cost of magnesium oxysulfate cement, saves the cost of boron mud and waste acid treatment, and can obtain good economic benefit and ecological benefit.
Description
Technical Field
The invention relates to a comprehensive utilization technology of industrial solid wastes, in particular to a full-solid waste building material taking boric sludge as a main raw material and a preparation method thereof.
Background
The boron mud is waste produced in the process of preparing borax and boric acid from boron ore in chemical plants, and mainly contains forsterite magnesium silicate, basic magnesium carbonate or magnesium carbonate, a small amount of ferromagnetic ore, plagioclase feldspar, serpentine, potash feldspar and a plurality of amorphous particles. The storage amount of boron mud in China is rich, the total amount of the boron mud discharged every year reaches more than 200 million tons, and the accumulation amount of the boron mud reaches more than 2000 million tons. The boric sludge is mainly treated in a stacking mode, not only occupies a large amount of land, but also causes pollution to the environment. The boric sludge contains alkaline substances such as magnesium oxide, calcium oxide, sodium oxide and the like, which have serious harm to farmlands, underground water and atmosphere. The alkali liquor generated by the boric sludge can be dissolved into underground water, so that the yield of the surrounding farmland is reduced, the crops can be dead-grown in severe conditions, and the surrounding drinking water is polluted. Because the boric sludge particles are fine, the boric sludge can be scattered along with wind after losing moisture, and the atmospheric environment is polluted. The pollution of boron sludge to the ecological environment and the pollution of the atmospheric environment become public nuisance.
The boron mud mainly comprises 45-50% of forsterite magnesium silicate, about 20% of basic magnesium carbonate or magnesium carbonate, a small amount of ferromagnetic ore, plagioclase feldspar, serpentine, potash feldspar and the like. The forsterite magnesium silicate and the magnesium carbonate have great utilization value, and if the boron mud is discarded at will, serious waste of resources is caused, so that the method has great practical significance for resource utilization of the boron mud. At present, the utilization mode of boron mud in China mainly focuses on producing magnesium products, preparing flocculating agents to treat wastewater, manufacturing microcrystalline glass, preparing refractory materials and the like. However, in the process of preparing magnesium products and other technologies by using boron mud, the usage amount of the boron mud is small, magnesium resources in the boron mud are not fully utilized, a large amount of magnesium resources are wasted in the using process, and a large amount of secondary waste residues are generated. Therefore, a method capable of not only absorbing a large amount of boron mud, but also effectively utilizing the magnesium element in the boron mud is developed, and the method has important environmental significance and social benefit.
Disclosure of Invention
The invention aims to improve the comprehensive utilization rate of industrial waste boric sludge and provides a full-solid waste building material taking boric sludge as a main raw material and a preparation method thereof.
Aiming at the above purposes, the invention is realized by the following technical scheme:
a preparation method of a full-solid waste building material with boric sludge as a main raw material comprises the following steps:
(1) b, boron mud pretreatment: drying the boric sludge, crushing and sieving by a 10-mesh sieve;
(2) activating magnesium oxide in the boric sludge: calcining the pretreated boron mud to decompose magnesium carbonate therein to generate magnesium oxide to obtain calcined boron mud containing active magnesium oxide, and then crushing and sieving;
(3) acidifying boric sludge to prepare acidified boric sludge containing magnesium sulfate: reacting the pretreated boric sludge with waste sulfuric acid to prepare a magnesium sulfate-containing mixture; wherein the mass ratio of the boric sludge to the waste sulfuric acid is 3: 1-1: 2, and the reaction time is 2-24 h; adding fly ash after the reaction is finished (which can be embodied by controlling the pH value to obtain the acidified boric sludge containing magnesium sulfate, wherein the pH value of the mixture containing magnesium sulfate after the reaction is finished is 1-5, and the pH value of the acidified boric sludge containing magnesium sulfate after the fly ash is added is 5-8;
(4) preparing the boron mud full-solid waste building material: mixing and stirring the prepared acidified boron mud containing magnesium sulfate, a modifier and the prepared calcined boron mud containing active magnesium oxide into slurry, and performing slurry flow or semi-dry pressure forming and maintenance on the prepared slurry to obtain a boron mud building material finished product; wherein the molar ratio of the active magnesium oxide in the calcined boric sludge to the magnesium sulfate in the acidified boric sludge is 6.5-10, and the doping amount of the modifier is 0.5-3 wt% of the mass of the calcined boric sludge.
Preferably, in the step (2), the calcining temperature is 550-900 ℃, and the calcining time is 0.5-3 hours. More preferably, the calcination temperature is 600-650 ℃ and the calcination time is 2-2.5 h.
Preferably, in the step (2), the content of the active magnesium oxide in the calcined boric sludge is 2.8wt% to 16.7 wt%.
Preferably, in step (2), the calcined product is sieved below 100 meshes.
Preferably, in step (4), the magnesium sulfate content in the acidified boric sludge is 8-25 wt%.
Preferably, in step (4), the molar ratio of the active magnesium oxide in the calcined boric sludge to the magnesium sulfate in the acidified boric sludge is 7-8.
Preferably, in the step (4), the modifier is at least one of citric acid, oxalic acid, phosphoric acid, phosphate, sodium citrate, ferrous sulfate and malic acid. More preferably, the modifier is citric acid, and the mixing amount is 1.5wt% of the mass of the calcined boron mud.
Meanwhile, the invention also provides a full-solid waste building material prepared by the preparation method.
Preferably, in the step (4), the prepared slurry is subjected to semi-dry pressure forming.
Preferably, the 3d compressive strength of the all-solid-waste building material is 3-25MPa, the 7d compressive strength is 4-35MPa, and the 28d compressive strength is 10-45 MPa.
The advantages and effects of the invention at least comprise: the method is characterized in that boron mud is directly calcined to obtain sintered boron mud containing active magnesium oxide, magnesium sulfate mixture obtained by acid leaching of the boron mud is adopted, industrial waste fly ash is adopted as pH adjusting material and reinforcing material of acid leaching solution, magnesium oxysulfate cement slurry with solid waste as main raw materials is prepared, and further, building materials such as baking-free bricks, building blocks, plates and the like can be prepared, and other artware can also be prepared. The invention effectively solves the problem of boron mud treatment, has simple operation and large boron mud usage amount, simultaneously reduces the production cost of magnesium oxysulfate cement, saves the cost of boron mud and waste acid treatment, and can obtain good economic benefit and ecological benefit.
Drawings
Fig. 1 is a general process flow diagram of the method for preparing a building material using boric sludge according to the present invention.
FIG. 2 is the effect of boron mud calcination temperature on the mechanical properties of building materials.
FIG. 3 is the effect of boron mud calcination time on the mechanical properties of building materials.
Fig. 4 shows the results of different molding methods.
Detailed Description
FIG. 1 shows the general process flow of the present invention for preparing building materials using boric sludge. The present invention is further illustrated by the following examples, but is not limited to the details of the description.
1. Parameter optimization of substituted raw material for preparing light-burned magnesia by calcining boric sludge
Crushing the boric sludge, sieving the boric sludge by a 10-mesh sieve, drying the boric sludge, and then carrying out high-temperature calcination treatment.
(1) Calcination temperature
The calcination time of the calcination temperature experiment is preset to be 2 hours, different calcination temperature gradient experiments are set, the temperature is 600-900 ℃, and the optimal data are selected from the loss of boron mud ignition and the activity of calcined magnesia.
TABLE 1 boron sludge loss on ignition and magnesia activity (time: 2 h) at different calcination temperatures
FIG. 2 is the effect of boron mud calcination temperature on the mechanical properties of building materials. From the boron mud calcination experimental data, the calcination is started at 600 ℃, the activity inflection point is obtained by calcination at 650 ℃, the activity maximum value is reached, and the activity of magnesium oxide burnt by the boron mud is gradually reduced along with the increase of the temperature. Combining with the experiment of the embodiment, the preferable calcining temperature for the activity of the boron mud for calcining the magnesium oxide is 600-750 ℃, the optimal temperature is 600-650 ℃, and the calcining temperature is far lower than 900 ℃ for preparing the light-calcined magnesium oxide from the magnesite.
(2) Calcination time
The calcination time preference experiment was carried out at an optimum calcination temperature of 650 deg.C, with the results as given in the following table:
TABLE 2 loss on ignition and MgO activity (temperature: 650 ℃ C.) for different calcination times
FIG. 3 is the effect of boron mud calcination time on the mechanical properties of building materials. From the experimental data of the boron sludge calcination time, the calcination time inflection point appears in the whole calcination process from 0.5h to 3h, and the highest point of the boron sludge magnesium oxide calcination activity is 2.5 h. Combining with the experiment of the embodiment, the boron mud calcined for more than 1h has higher activity, and the optimal calcination time for the activity of the boron mud to burn out the magnesium oxide is 2-2.5 h.
2. Test of boron mud full-solid waste building material
Acidification experiments (acidification conditions are that boric sludge is sieved by a 10-mesh sieve, the mass concentration of waste sulfuric acid is 25 percent, the mass ratio of boric sludge to waste sulfuric acid (25 percent) is =1:2, and acid leaching time is 24 h)
And putting the calcined boron mud, the modifier and the acidified boron mud containing magnesium sulfate into a stirrer, stirring for 2-10 minutes until the slurry is uniform, pouring the obtained slurry into a mold, vibrating or pressing for molding, and curing to obtain the sintered boron mud building material finished product.
The experiment investigates the influence of the boron mud calcining temperature, the boron mud calcining time and the magnesium oxide active content, and the experiment adopts a semidry method for forming.
Table 3: experiment groups with different calcination temperatures (acidified boric sludge containing 16wt% magnesium sulfate; modifier: citric acid (1.5 wt%); molar ratio: 7; calcination time of boric sludge: 2 h)
Table 3 shows the effect of boron sludge calcination temperature on the mechanical properties of building materials. The magnesium oxide burnt by the boron mud with different calcination temperatures has different activity, the acidified boron mud containing magnesium sulfate is the same, the modifying agents are citric acid (the addition amount is 1.5 percent of the mass of the calcined boron mud), and the result shows that the calcination temperature is 600-650 ℃, the better result is obtained, and the compressive strength is better.
Table 4: experimental groups (acidified boric sludge containing 16wt% magnesium sulfate) with different calcination times; modifying agent: citric acid (1.5 wt%); the molar ratio is as follows: 7; the calcination temperature of the boric sludge is as follows: 650 deg.C)
Table 4 shows that the effect of the boron sludge calcination time on the mechanical properties of the building material (calcination temperature is 650 ℃), the magnesium sulfate-containing acid-dipped boron sludge mixture is the same, the modifying agents are citric acid (the addition amount is 1.5% of the mass of the calcined boron sludge), and the results show that the calcination time is more than 1h, and the strength is better from 2h to 2.5 h.
Table 5: experimental groups of different forming modes (calcining temperature: 650 ℃, calcining time: 2h, molar ratio: 7, active magnesium oxide content: 16.7wt%, acidified boric sludge containing 16wt% magnesium sulfate, modifier: citric acid (1.5 wt%))
Fig. 4 shows the results of different molding methods. As shown in Table 5, the modifier citric acid (added in an amount of 1.5% by mass of boron mud) was selected as 16.7wt% of active sintered boron mud (i.e., 650 ℃, 2h calcination), and the results show that the compressive strength of the slurry flow test is not as high as that of the semi-dry test.
It should be noted that the terms "first", "second", "third", and the like in the description are used for distinguishing various components, elements, steps, and the like in the description, and are not used for indicating a logical relationship or a sequential relationship between the various components, elements, steps, and the like, unless otherwise specified.
It is to be understood that while the present invention has been described in conjunction with the preferred embodiments thereof, it is not intended to limit the invention to those embodiments. It will be apparent to those skilled in the art from this disclosure that many changes and modifications can be made, or equivalents modified, in the embodiments of the invention without departing from the scope of the invention. Therefore, any simple modification, equivalent change and modification made to the above embodiments according to the technical essence of the present invention are still within the scope of the protection of the technical solution of the present invention, unless the contents of the technical solution of the present invention are departed.
Claims (12)
1. A preparation method of a full-solid waste building material with boric sludge as a main raw material is characterized by comprising the following steps:
(1) b, boron mud pretreatment: drying the boric sludge, crushing and sieving by a 10-mesh sieve;
(2) activating magnesium oxide in the boric sludge: calcining the pretreated boron mud to decompose magnesium carbonate therein to generate magnesium oxide to obtain calcined boron mud containing active magnesium oxide, and then crushing and sieving;
(3) acidifying boric sludge to prepare acidified boric sludge containing magnesium sulfate: reacting the pretreated boric sludge with waste sulfuric acid to prepare a magnesium sulfate-containing mixture; wherein the mass ratio of the boric sludge to the waste sulfuric acid is 3: 1-1: 2, and the reaction time is 2-24 h; adding fly ash after the reaction is finished to obtain acidified boric sludge containing magnesium sulfate; after the reaction is finished, the pH value of the magnesium sulfate-containing mixture is 1-5, and the pH value of the acidified boric sludge containing magnesium sulfate after the fly ash is added is 5-8;
(4) preparing the boron mud full-solid waste building material: mixing and stirring the prepared acidified boron mud containing magnesium sulfate, a modifier and the prepared calcined boron mud containing active magnesium oxide into slurry, and performing slurry flow or semi-dry pressure forming and maintenance on the prepared slurry to obtain a boron mud building material finished product; wherein the molar ratio of the active magnesium oxide in the calcined boric sludge to the magnesium sulfate in the acidified boric sludge is 6.5-10; the mixing amount of the modifier is 0.5 to 3 weight percent of the mass of the calcined boric sludge.
2. The method of claim 1, wherein in the step (2), the calcination temperature is 550 ℃ to 900 ℃ and the calcination time is 0.5 to 3 hours.
3. The method according to claim 2, wherein in the step (2), the calcination temperature is 600-650 ℃ and the calcination time is 2-2.5 h.
4. The method according to claim 1, wherein in the step (2), the content of the active magnesium oxide in the calcined boric sludge is 2.8wt% to 16.7 wt%.
5. The method of claim 1, wherein in step (2), the calcined product is sieved through a sieve of 100 mesh or less.
6. The method according to claim 1, wherein in the step (4), the magnesium sulfate is contained in the acidified boric sludge in an amount of 8 to 25 wt%.
7. The method of claim 1, wherein the molar ratio of active magnesium oxide in the calcined boric sludge to magnesium sulfate in the acidified boric sludge is from 7 to 8.
8. The method of claim 1, wherein in the step (4), the modifier is at least one of citric acid, oxalic acid, phosphoric acid, phosphate, sodium citrate, ferrous sulfate, and malic acid.
9. The method of claim 8, wherein the modifying agent is citric acid and is added in an amount of 1.5wt% based on the mass of the calcined boric sludge.
10. The method according to claim 1, wherein in the step (4), the obtained slurry is subjected to semi-dry press molding.
11. An all-solid-waste building material obtained by the method according to any one of claims 1 to 10.
12. The all-solid-waste building material of claim 11, wherein the 3d compressive strength is 3-25MPa, the 7d compressive strength is 4-35MPa, and the 28d compressive strength is 10-45 MPa.
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| CN116161942B (en) * | 2023-03-22 | 2024-05-31 | 东北大学 | Method for preparing magnesium oxysulfide board by utilizing boric sludge base material |
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| CN107619237A (en) * | 2017-10-19 | 2018-01-23 | 沈阳建筑大学 | A kind of method using boric sludge for mortar specimen |
| CN111153610A (en) * | 2020-02-28 | 2020-05-15 | 辽宁科大中驰镁建材科技有限公司 | Method for comprehensively utilizing high-iron high-calcium high-silicon waste magnesite and boron mud |
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| CN107619237A (en) * | 2017-10-19 | 2018-01-23 | 沈阳建筑大学 | A kind of method using boric sludge for mortar specimen |
| CN111153610A (en) * | 2020-02-28 | 2020-05-15 | 辽宁科大中驰镁建材科技有限公司 | Method for comprehensively utilizing high-iron high-calcium high-silicon waste magnesite and boron mud |
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