CN112079589A - Modified lithium slag complex mineral admixture and preparation and application thereof - Google Patents
Modified lithium slag complex mineral admixture and preparation and application thereof Download PDFInfo
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- CN112079589A CN112079589A CN202010965344.1A CN202010965344A CN112079589A CN 112079589 A CN112079589 A CN 112079589A CN 202010965344 A CN202010965344 A CN 202010965344A CN 112079589 A CN112079589 A CN 112079589A
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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
- C04B40/0028—Aspects relating to the mixing step of the mortar preparation
- C04B40/0039—Premixtures of ingredients
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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
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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
Abstract
The invention provides a modified lithium slag complex mineral admixture, and belongs to the technical field of building materials. The method comprises the following steps of: 40-70 parts of acid method lithium slag, 20-55 parts of limestone powder, 5-10 parts of active calcium salt modifier and 0.1-0.2 part of reinforcing activator. The acid method lithium slag comprises the following components in percentage by mass: loss: 6 to 12% of SiO2：45～60％，Al2O3：13～22％，CaO：5～11％，SO3: 3-10% of the total mass percentage, and the balance of impurities, wherein the total mass percentage sum is 100%. The invention also provides a preparation method and application of the modified lithium slag complex mineral admixture. The admixture of the invention introduces the active calcium salt modifier, makes up the deficiency of the performance of the acid lithium slag by compounding the acid lithium slag and the limestone powder, can obviously improve the performance of the concrete and realize the high performance of the concreteAnd (4) greening. The modified lithium slag compound mineral admixture provided by the invention can replace the existing admixtures such as fly ash and mineral powder, so that the cement consumption is reduced, the concrete production cost is further reduced, and the economic benefit and the social benefit are obvious.
Description
Technical Field
The invention belongs to the technical field of building materials, and particularly relates to a modified lithium slag complex mineral admixture and preparation and application thereof.
Background
The lithium slag is an industrial waste generated in the process of extracting lithium carbonate by a sulfuric acid-calcium carbonate method using spodumene ore as a raw material. And in the smelting process, about 10 tons of lithium slag are produced when 1 ton of lithium carbonate is produced. With the increase of the total demand of lithium carbonate in global development, the amount of the lithium slag discharged by acid smelting is increased day by day, most of the discharged lithium slag is treated by open-air accumulation or deep pit landfill, but the waste of lithium slag resources is caused, the environment is polluted, and the geological environment is more likely to be damaged, so that the treatment of the lithium slag becomes a problem to be solved at present.
SiO in chemical composition of lithium slag2And Al2O3Has high content and latent volcanic ash activity, and thus can be used as admixture for concrete. The lithium slag doped in the concrete can play a role in improving the pore structure of the concrete, reducing the shrinkage and permeability of the concrete, improving the elastic modulus of the concrete and the like. But the resource utilization of the lithium slag has a plurality of problems at present, firstly, the lithium slag resource is unevenly distributed and mainly focuses on Xinjiang, Sichuan and other places in China; second, in the lithium slagSO of (A)3The content (in the form of gypsum) is higher than 6%, and the problem of poor stability can be caused when the mixing amount is higher; and thirdly, the lithium slag has high water absorption rate, is inconvenient to use in the actual production process of concrete, and often needs to be dried for pretreatment.
Disclosure of Invention
The invention aims to provide a modified lithium slag complex mineral admixture, which can excite the activity of acid-process lithium slag, exert the additive effect of complex doping with limestone powder, improve the comprehensive performance of concrete, provide a new way for resource utilization of lithium slag and improve the economic benefit and the environmental benefit of the lithium slag.
The purpose of the invention is realized by the following technical scheme:
the modified lithium slag complex mineral admixture comprises the following components in parts by mass: 40-70 parts of acid method lithium slag, 20-55 parts of limestone powder, 5-10 parts of active calcium salt modifier and 0.1-0.2 part of reinforcing activator.
Further, the method comprises the following steps of: 45-65 parts of acid method lithium slag, 30-45 parts of limestone powder, 7-9 parts of active calcium salt modifier and 0.1-0.15 part of reinforcing activator.
Furthermore, the composite material comprises the following components in parts by mass: 50-60 parts of acid method lithium slag, 35-40 parts of limestone powder, 7.5-8 parts of active calcium salt modifier and 0.12-0.15 part of reinforcing activator.
SO in lithium slag3Usually in CaSO4·2H2O or CaSO4The form of the additive is beneficial to exciting the activity of the lithium slag or forming AFt (early stage) in concrete, enhancing the compactness of the concrete and having little influence on the stability. Therefore, the main reason for restricting the use of the calcium-based lithium iron phosphate as the admixture is Ca in the lithium slag+Low content of SiO2And Al2O3The amorphous state exists in an indefinite state, and the activity of the amorphous state needs to be excited, so that the activity at the early stage is lower; and the lithium slag has a porous structure with a large inner surface area and strong water absorption, and reduces the flowability of the fresh concrete after being doped. The limestone powder has wide and easily available source, low price and potential volcanic ash activity, and is adopted to fully exert the positive effect of the mineral admixture, improve the dosage of the mineral admixture in concreteThe mineral admixture compounding technology is used for realizing the advantage complementation among different mineral admixtures and improving the comprehensive performance of the concrete.
When the modified lithium slag compound mineral admixture is applied to concrete, firstly, the clinker minerals are hydrated to generate C-S-H, AFt and Ca (OH)2Etc. a part of C3A and CaCO3Reaction to generate 3CaO & Al2O3·CaCO3·11H2O; wherein the micro-crystal nuclear effect of the limestone powder accelerates the hydration reaction rate of the cement, so that hydration products are increased within a certain hydration period; and Ca (OH) in the hydration product2But also is an active activator of the lithium slag, so that the hydration rate of the lithium slag is improved, and the lithium slag is Ca (OH)2The consumption of the lime stone powder is a promoting effect on the hydration reaction of cement particles, and the limestone powder has direct and indirect promoting effects on the hydration of cement and the hydration of lithium slag, so that the strength of concrete can be obviously improved when the limestone powder and the lithium slag are compounded. Therefore, the modified lithium slag complex mineral admixture of the invention exerts the super-overlapping effect, makes up for the performance deficiency of the lithium slag, improves the hydration performance of the cementing material system and further improves the comprehensive performance of the concrete.
The reinforcing activator improves the grindability of the composite mineral admixture and improves the dispersibility of the cementing material in concrete; active cations are introduced into the active calcium salt modifier, and the lithium slag is activated through mechanical grinding; the limestone powder can reduce the negative effect of the lithium slag used as the concrete admixture independently and comprehensively improve various performance indexes of the concrete.
Further, the acid method lithium slag is residue generated in the process of preparing lithium carbonate by a sulfuric acid-calcium carbonate method, is earthy yellow in appearance, has strong water absorption, is powdery after being dried, and has small particles. Which comprises the following components in percentage by mass: loss: 6 to 12% of SiO2：45～60％，Al2O3：13～22％，CaO：5～11％，SO3: 3-10% of the total mass percentage, and the balance of impurities, wherein the total mass percentage sum is 100%. Wherein, SiO2、Al2O3Mostly in an amorphous, non-glassy state and active; the impurities include MgO and Fe2O3、K2O、Na2O and the like.
Further, the limestone powder is white or light gray in appearance, CaCO3The content is not less than 85 wt%. The limestone powder is preferably crushed limestone or ground powder produced during production of machine-made sand.
Further, the active calcium salt modifier is one or more of calcium aluminate, calcium ferrite and calcium sulfate.
Further, the enhancing activator is one or more of triethanolamine, glycerol and triisopropanolamine.
A preparation method of a modified lithium slag complex mineral admixture comprises the steps of weighing raw materials according to parts by weight, respectively drying acid-process lithium slag, limestone powder and an active calcium salt modifier, cooling, uniformly mixing, adding a reinforcing active agent, mixing and grinding.
In the preparation process of the modified lithium slag composite mineral admixture, the limestone powder and the acid method lithium slag are mutually adhered to the surface in the grinding process to prevent agglomeration, so that the grinding efficiency is improved; the specific surface energy of the acid method lithium slag and the limestone powder is obviously reduced by the enhanced activating agent in the grinding process, and the enhanced activating agent is selectively adsorbed on the surface of the superfine powder, so that the stability of the superfine powder is improved, the agglomeration is prevented, and the grinding efficiency is improved; the active calcium salt modifier provides active cations which are lacked in the lithium slag, and a new interface is generated by grinding to excite the activity of the acid method lithium slag.
Further, the drying temperature is 95-105 ℃, and the grinding time is 30-50 min.
An application of a modified lithium slag complex mineral admixture in concrete.
Furthermore, the admixture is applied to improving the working performance of concrete and enhancing the strength of concrete. .
Compared with the prior art, the invention has the following beneficial effects:
1. the invention provides a new way for resource utilization of the lithium slag and the limestone powder, and has important significance for protecting the environment and saving resources.
2. The invention introduces the active calcium salt modifier, makes up the deficiency of the performance of the lithium slag by compounding the lithium slag and the limestone powder, can obviously improve the performance of the concrete, and realizes the high performance and the greening of the concrete.
3. The modified lithium slag compound mineral admixture provided by the invention can replace the existing admixtures such as fly ash and mineral powder, so that the cement consumption is reduced, the concrete production cost is further reduced, and the economic benefit and the social benefit are obvious.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Example 1
The modified lithium slag complex mineral admixture of the embodiment comprises the following components in parts by mass: 70 parts of acid method lithium slag and 30 parts of limestone powder (CaCO)390 wt%), 2 parts of calcium aluminate, 4 parts of calcium ferrite, 4 parts of calcium sulfate and 0.2 part of triethanolamine.
The acid method lithium slag is residue generated in the process of preparing lithium carbonate by a sulfuric acid-calcium carbonate method, is earthy yellow in appearance, has strong water absorption, is powdery after being dried, and has small particles. According to the mass percentage, the material comprises the following components: 6% of SiO2：54％，Al2O3：15％，CaO：11％，SO3: 8 percent, and the balance of MgO and Fe2O3、K2O、Na2O and the like.
Weighing the components, drying the acid-process lithium slag, the limestone powder, the calcium aluminate, the calcium ferrite and the calcium sulfate at 105 ℃, cooling, uniformly mixing, adding triethanolamine, mixing, placing in a ball mill, and grinding for 40min to obtain the finished product of the modified lithium slag composite mineral admixture of the embodiment.
Example 2
The modified lithium slag complex mineral admixture of the embodiment comprises the following components in parts by mass: 52 parts of acid method lithium slag and 35 parts of limestone powder (CaCO)3Content (wt.)90 wt%), 2 parts of calcium aluminate, 3 parts of calcium ferrite, 3 parts of calcium sulfate, 0.04 part of triethanolamine, 0.05 part of glycerol and 0.04 part of triisopropanolamine.
The acid method lithium slag is residue generated in the process of preparing lithium carbonate by a sulfuric acid-calcium carbonate method, is earthy yellow in appearance, has strong water absorption, is powdery after being dried, and has small particles. According to the mass percentage, the material comprises the following components: 8% of SiO2：55％，Al2O3：18％，CaO：8％，SO3: 7 percent, and the balance of MgO and Fe2O3、K2O、Na2O and the like.
Weighing the components, drying the acid-process lithium slag, the limestone powder, the calcium aluminate, the calcium ferrite and the calcium sulfate at 100 ℃, cooling, uniformly mixing, adding triethanolamine, mixing, placing in a ball mill, and grinding for 40min to obtain the finished product of the modified lithium slag composite mineral admixture of the embodiment.
Example 3
The modified lithium slag complex mineral admixture of the embodiment comprises the following components in parts by mass: 56 parts of acid method lithium slag and 38 parts of limestone powder (CaCO)3Content of 90 wt%), 2 parts of calcium aluminate, 3 parts of calcium ferrite, 2.5 parts of calcium sulfate, 0.05 part of triethanolamine, 0.03 part of glycerol and 0.04 part of triisopropanolamine.
The acid method lithium slag is residue generated in the process of preparing lithium carbonate by a sulfuric acid-calcium carbonate method, is earthy yellow in appearance, has strong water absorption, is powdery after being dried, and has small particles. According to the mass percentage, the material comprises the following components: 10% of SiO2：55％，Al2O3：17％，CaO：7％，SO3: 8 percent, and the balance of MgO and Fe2O3、K2O、Na2O and the like.
Weighing the components, drying the acid-process lithium slag, the limestone powder, the calcium aluminate, the calcium ferrite and the calcium sulfate at 105 ℃, cooling, uniformly mixing, adding triethanolamine, mixing, placing in a ball mill, and grinding for 35min to obtain the finished product of the modified lithium slag composite mineral admixture of the embodiment.
Example 4
The true bookThe embodiment modified lithium slag complex mineral admixture comprises the following components in parts by weight: 60 parts of acid method lithium slag and 30 parts of limestone powder (CaCO)395 wt%), 2 parts of calcium aluminate, 3 parts of calcium ferrite, 5 parts of calcium sulfate and 0.2 part of glycerol.
The acid method lithium slag is residue generated in the process of preparing lithium carbonate by a sulfuric acid-calcium carbonate method, is earthy yellow in appearance, has strong water absorption, is powdery after being dried, and has small particles. According to the mass percentage, the material comprises the following components: 12% of SiO2：48％，Al2O3：22％，CaO：5％，SO3: 10 percent, and the balance of MgO and Fe2O3、K2O、Na2O and the like.
Weighing the components, drying the acid-process lithium slag, the limestone powder, the calcium aluminate, the calcium ferrite and the calcium sulfate at 105 ℃, cooling, uniformly mixing, adding triethanolamine, mixing, placing in a ball mill, and grinding for 45min to obtain the finished product of the modified lithium slag composite mineral admixture of the embodiment.
Example 5
The modified lithium slag complex mineral admixture of the embodiment comprises the following components in parts by mass: 50 parts of acid method lithium slag and 45 parts of limestone powder (CaCO)395 wt%), 1 part of calcium aluminate, 2 parts of calcium ferrite, 2 parts of calcium sulfate and 0.1 part of triisopropanolamine.
The acid method lithium slag is residue generated in the process of preparing lithium carbonate by a sulfuric acid-calcium carbonate method, is earthy yellow in appearance, has strong water absorption, is powdery after being dried, and has small particles. According to the mass percentage, the material comprises the following components: 10% of SiO2：55％，Al2O3：20％，CaO：10％，SO3: 3 percent, and the balance of MgO and Fe2O3、K2O、Na2O and the like.
Weighing the components, drying the acid-process lithium slag, the limestone powder, the calcium aluminate, the calcium ferrite and the calcium sulfate at 100 ℃, cooling, uniformly mixing, adding triethanolamine, mixing, placing in a ball mill, and grinding for 45min to obtain the finished product of the modified lithium slag composite mineral admixture of the embodiment.
Example 6
The modified lithium slag complex mineral admixture of the embodiment comprises the following components in parts by mass: 40 parts of acid method lithium slag and 55 parts of limestone powder (CaCO)395 wt%), 1 part of calcium aluminate, 2 parts of calcium ferrite, 2 parts of calcium sulfate, 0.03 part of triethanolamine, 0.03 part of glycerol and 0.04 part of triisopropanolamine.
The acid method lithium slag is residue generated in the process of preparing lithium carbonate by a sulfuric acid-calcium carbonate method, is earthy yellow in appearance, has strong water absorption, is powdery after being dried, and has small particles. According to the mass percentage, the material comprises the following components: 10% of SiO2：55％，Al2O3：20％，CaO：10％，SO3: 3 percent, and the balance of MgO and Fe2O3、K2O、Na2O and the like.
Weighing the components, drying the acid-process lithium slag, the limestone powder, the calcium aluminate, the calcium ferrite and the calcium sulfate at 100 ℃, cooling, uniformly mixing, adding triethanolamine, mixing, placing in a ball mill, and grinding for 45min to obtain the finished product of the modified lithium slag composite mineral admixture of the embodiment.
Comparative example 1
Based on example 2, the mass part of the acid method lithium slag is changed to 85 parts, and the rest is not changed.
Comparative example 2
Based on example 2, limestone powder was not added, and the rest was unchanged.
Comparative example 3
Based on example 2, calcium aluminate, calcium ferrite and calcium sulfate were not added, and the others were unchanged.
The net slurry fluidity and mortar activity of the modified lithium slag complex mineral admixtures prepared in examples 1 to 6 and the lithium slag complex mineral admixtures prepared in comparative examples 1 to 3 when applied to cement are shown in Table 1.
TABLE 1
| Group of | Mixing amount/% | Neat paste fluidity/mm | 28d Activity/%) |
| Reference sample | 0 | 200 | 100 |
| Example 1 | 30 | 235 | 84 |
| Example 2 | 30 | 255 | 95 |
| Example 3 | 30 | 260 | 94 |
| Example 4 | 30 | 240 | 88 |
| Example 5 | 30 | 245 | 84 |
| Example 6 | 30 | 240 | 86 |
| Comparative example 1 | 30 | 225 | 77 |
| Comparative example 2 | 30 | 230 | 70 |
| Comparative example 3 | 30 | 235 | 64 |
As can be seen from Table 2, when 30% by mass of cement was replaced with the lithium slag admixture, the performances such as the net paste fluidity and the activity index were the best in examples 2 and 3, and the performances were inferior in examples 1 and 4 to 6, and in comparative examples 1 to 3. The comparison shows that the working performance of the cement paste can be improved by adjusting the proportion of the lithium slag, the active calcium salt modifier and the reinforcing activator of the modified lithium slag composite admixture provided by the invention, and the activity of the novel modified lithium slag composite mineral admixture can be obviously improved.
Concrete trial mixing is carried out on the novel modified lithium slag complex mineral admixture prepared in the embodiment 2 according to the mixing proportion shown in the table 2, the admixture is respectively marked as application examples 1-3 according to different mixing proportions, the working performance and the compressive strength of the concrete trial mixed are shown in the table 3, and the embodiment 3 can also achieve the equivalent technical effect.
TABLE 2
TABLE 3
From table 3, it can be known that the modified lithium slag complex mineral admixture prepared by the invention is used in concrete to replace part of fly ash, and from the performance, the concrete workability is good, the initial slump expansion and the 2h time loss are obviously improved compared with the reference group without the modified lithium slag complex mineral admixture, the early strength is higher than the reference group, the later strength is stable, and the 60d strength is equivalent to the reference group; from the aspect of cost and environmental protection, under the same strength grade, because the lithium slag and the limestone powder with lower price are mixed, the single-side concrete has lower cost, and simultaneously, a solution is provided for the efficient resource utilization of the lithium slag, and the better environment-friendly effect is achieved.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the present invention.
Claims (9)
1. The modified lithium slag complex mineral admixture is characterized by comprising the following components in parts by mass: 40-70 parts of acid method lithium slag, 20-55 parts of limestone powder, 5-10 parts of active calcium salt modifier and 0.1-0.2 part of reinforcing activator.
2. The modified lithium slag complex mineral admixture according to claim 1, wherein the acid process lithium slag comprises, in mass percent: loss: 6 to 12% of SiO2：45～60％，Al2O3：13～22％，CaO：5～11％，SO3: 3-10% of the total mass percentage, and the balance of impurities, wherein the total mass percentage sum is 100%.
3. The modified lithium slag complex mineral admixture of claim 1, wherein the limestone powder is white or light gray in appearance, CaCO3The content is not less than 85 wt%.
4. The modified lithium slag complex mineral admixture of claim 1, wherein the active calcium salt modifier is one or more of calcium aluminate, calcium ferrite and calcium sulfate.
5. The modified lithium slag complex mineral admixture according to claim 1, wherein the enhancing activator is one or more of triethanolamine, glycerol, triisopropanolamine.
6. The method of any one of claims 1 to 5, wherein the modified lithium slag complex mineral admixture is prepared by weighing raw materials in parts by weight, drying the acid-process lithium slag, the limestone powder and the active calcium salt modifier respectively, cooling, mixing uniformly, adding the enhancing active agent, mixing and grinding.
7. The method of claim 6, wherein the drying temperature is 95-105 ℃ and the milling time is 30-50 min.
8. The use of the modified lithium slag complex mineral admixture according to any one of claims 1 to 5 in concrete.
9. The use of the modified lithium slag complex mineral admixture of claim 8, wherein the admixture is used for improving the workability of concrete and enhancing the strength of concrete.
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