CN115872695B - Lepidolite slag concrete - Google Patents

Lepidolite slag concrete Download PDF

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CN115872695B
CN115872695B CN202211307459.7A CN202211307459A CN115872695B CN 115872695 B CN115872695 B CN 115872695B CN 202211307459 A CN202211307459 A CN 202211307459A CN 115872695 B CN115872695 B CN 115872695B
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parts
stirring
lepidolite
concrete
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CN115872695A (en
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刘红霞
刘澜涛
王红英
黄高明
吴炎平
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Jiangxi Building Materials Research And Design Institute Co ltd
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Jiangxi Building Materials Research And Design Institute Co ltd
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    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02WCLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
    • Y02W30/00Technologies for solid waste management
    • Y02W30/50Reuse, recycling or recovery technologies
    • Y02W30/91Use of waste materials as fillers for mortars or concrete

Abstract

The invention provides a preparation method of lepidolite slag concrete. The lepidolite lithium extraction tailings are subjected to coating modification treatment, and excessive sodium, potassium and sulfur elements in the lepidolite lithium extraction tailings are adsorbed to a coating layer. The high molecular polymer and the polyvinyl alcohol fiber in the coating layer are effectively combined to form a grid structure in the concrete, so that the influence of free sodium, potassium and sulfate radicals on the performance of the concrete is avoided. The air entraining agent does not contain sodium, potassium, sulfate radical and other ions, and after the air entraining agent is added, a micro-pore structure appears in the structure of the air entraining agent, so that the mechanical property of the concrete is improved. The additive does not contain sodium, potassium and sulfate ions, the vegetable gum reduces the slump of the concrete in the stirring process, improves the gelation of the concrete, and can simultaneously "wrap" the sodium, potassium and sulfate ions in the modified lepidolite extracted lithium tailings together with the coating agent.

Description

Lepidolite slag concrete
Technical Field
The invention belongs to the field of building materials, and particularly relates to lepidolite slag concrete.
Technical Field
The Jiangxi has abundant lepidolite ore resources, a large amount of lithium extraction waste residues can be generated after the lithium extraction of minerals, and the comprehensive utilization of the lithium extraction waste residues is of great significance to the reasonable application of the resources. The current research is mainly focused on directly applying to building materials such as concrete, cement mortar, cement and the like, preparing ceramic, building ceramsite molecular sieves and the like. The active components of silicon dioxide and aluminum oxide contained in the lithium slag have a certain volcanic ash activity, and the active components are added into the concrete to effectively improve the mechanical property, carbonization resistance and wear resistance of the concrete, but excessive elements such as potassium and sodium contained in the active components are directly used in the concrete, so that the quality problems of frosting, severe alkali efflorescence, collapse and the like of the concrete surface are easily caused, and therefore, the influence of high-content elements such as potassium and sodium after the addition of the lepidolite is solved.
Aiming at the problems, the invention provides a preparation method of modified lepidolite lithium extraction tailings, which is matched with an air entraining agent and an additive for use, so that the performance of concrete is improved.
Disclosure of Invention
The invention mainly aims to provide a preparation method of lepidolite slag concrete.
The second purpose of the invention is to provide a preparation method of modified lepidolite lithium extraction tailings in lepidolite slag concrete.
The invention provides a method for preparing an air entraining agent in lepidolite slag concrete.
The fourth purpose of the invention is to provide a preparation method of the additive in lepidolite slag concrete.
The invention is obtained by the following method:
a preparation method of lepidolite slag concrete.
The preparation process of the modified lepidolite lithium extraction tailings comprises the following steps:
(1) Taking 10-15 parts of lepidolite extracted lithium tailings, putting the lepidolite extracted lithium tailings into a ball mill for ball milling, wherein the specific surface area of the lepidolite extracted lithium tailings is not less than 400m 2 Particles per kg for use;
(2) Taking 18-25 parts of butyl acrylate, 4-6 parts of 1,4,7,10,13, 16-hexaoxacyclooctadecane, 15-20 parts of styrene, adding methyl acetate solution, heating to 230-240 ℃ at the speed of 4-6 ℃/min, preserving heat and stirring for 5-7 hours, adding 15-crown ether-5 2-4 parts, 3-5 parts of hexafluoroisopropanol, 5-7 parts of pentenoate and 4-6 parts of polyvinyl alcohol fibers, transferring the polyvinyl alcohol fibers into a reaction kettle, controlling the temperature to 270-280 ℃, preserving heat and stirring for 4-6 hours, adding the mixture into the lepidolite extracted lithium tailings of the step (1), and stirring uniformly to obtain the lithium ion battery pack.
The preparation method of the air entraining agent comprises the following steps:
4-6 parts of dodecyl dimethyl amine ethyllactone, 3-5 parts of cyclopropylmethyl ketone and methyl acetate are taken, the temperature is raised to 320-330 ℃ at the speed of 3-5 ℃/min, the temperature of the solution is controlled to be 150-160 ℃ after heat preservation and stirring for 4-5 hours, 6-8 parts of humic acid and 4-5 parts of hexahydrophthalic anhydride are added, the temperature is raised to 210-215 ℃ after heat preservation and stirring for 6-7 hours, 3-4 parts of methyltributylketone oxime silane and 4-6 parts of isooctyl hydroxystearate are added, and the mixture is poured into a homogenizing and emulsifying reaction kettle to be uniformly mixed, heated to 160 ℃, and homogenized and emulsified to obtain the product.
Preparation method of additive
Adding 5-7 parts of sesbania gum, 4-6 parts of guar gum and 4-6 parts of alkylphenol ethoxylates into ethanol solution, heating to 140-150 ℃ at the speed of 2-4 ℃/min, insulating and stirring for 3-5 hours, adding 4-6 parts of ethyl cyanoacrylate and 2-4 parts of 3,3', 4' -biphenyl tetracarboxylic dianhydride, controlling the temperature of the solution to 230-240 ℃, insulating and stirring for 5-6 hours, adding 2-4 parts of polyoxyethylene sorbitan palmitate and 1-2 parts of 2' -hydroxy-3-phenylpropionyl acetone, heating to 260-265 ℃ at the speed of 1-2 ℃/min, insulating and stirring for 5-6 hours, adding 5-6 parts of microcrystalline wax, controlling the temperature of the solution to 60-70 ℃, and insulating and stirring for 4-6 hours.
The formula of the concrete raw materials is as follows: 10-15 parts of cement model P.042.5R10-35 parts of sand, 40-45 parts of broken stone, 6.5-7.5 parts of water, 1.5-2.5 parts of mineral powder, 1.5-2.5 parts of modified lepidolite lithium extraction tailings, 0.1-0.2 part of air entraining agent and 0.1-0.2 part of additive;
the preparation method of the concrete comprises the following steps:
1) Weighing crushed stone and sand according to a proportion, putting the crushed stone and the sand into a stirrer, mixing and stirring for 1 minute, adding cement, modified lithium extraction tailings and mineral powder, and stirring for 1 minute for later use;
2) Adding the water reducer and the air entraining agent into water, controlling the temperature of the solution to be 60-70 ℃, stirring for 5-8min, adding the mixture in the step 1), and stirring for 3-5min together to obtain the water reducer.
Wherein the crushed stone is 15-18mm in particle size and has a mud content of 0.3%;
the sand is natural sand, preferably river sand, with fineness modulus range of 2.5-2.7 and mud content less than or equal to 0.45%.
The invention has the advantages that:
according to the invention, the lepidolite lithium extraction tailings are modified, so that the lepidolite lithium extraction tailings are suitable for concrete. By modifying the lepidolite lithium extraction tailings, the precipitation of harmful elements such as sodium, potassium, sulfur and the like is reduced, and the phenomenon of performance degradation of concrete caused by the excessive content of the harmful elements in the concrete is solved. And the excessive sodium, potassium and sulfur elements are adsorbed to the coating layer, so that the influence of free sodium, potassium and sulfate radicals on the performance of the concrete is avoided, and the performance of the concrete after lepidolite slag is added is improved. The high molecular polymer and the polyvinyl alcohol fiber in the coating layer are effectively combined to form a grid structure in the concrete, and the 15-crown ether-5 can be subjected to complexation reaction with sodium ions, but is extremely easy to oxidize, so that other substances are required to be added to prevent oxidation failure. Active groups such as hydroxyl, carboxyl, double bonds and the like in the coating layer can be complexed with sodium, potassium, sulfate radical and the like, so that the active groups can be effectively adsorbed and wrapped, the influence of free sodium, potassium and sulfate radical on the performance of the concrete is avoided, and the performance of the concrete after lepidolite slag is added is improved. The addition of the polyvinyl alcohol fiber not only improves the cracking resistance of the concrete, but also acts together with the high molecular structure in the coating agent to reduce the influence of sodium, potassium and sulfate ions in the lepidolite lithium extraction tailings.
The air entraining agent is added to improve the frost resistance of the concrete, improve the pore structure of the concrete and improve the mechanical property of the concrete, so the advantages and disadvantages of the air entraining agent are directly related to the property of the concrete. Common air entraining agents often contain anionic surfactants such as sodium lignin sulfonate, but conventional air entraining agents cannot be selected because lepidolite lithium extraction tailings exist in the concrete to further reduce the influence of sodium, potassium, sulfate radical and other ions in the concrete on the concrete. The air entraining agent provided by the invention does not contain sodium, potassium, sulfate radical and other ions, and the added humic acid can be used as a water reducing agent for concrete, but has the effect of entraining air in the concrete by modifying and compounding the air entraining agent with other surface active ions, organic silicon solution and the like, so that tiny bubbles appear in the air entraining agent in the concrete in the stirring process of the concrete, a tiny pore structure appears in the structure of the air entraining agent, and the mechanical property of the concrete is improved.
Because the modified lepidolite extracted lithium tailings and the air entraining agent are added into the concrete, although the mechanical property of the concrete is improved, the coating agent and the air entraining agent in the modified lepidolite extracted lithium tailings have larger shrinkage values after the concrete is dried, are easy to generate cracks, are easy to generate water separation phenomenon in the stirring process, and cause the workability of the concrete to be reduced, the additive is required to be added into the concrete, the activity of the concrete is improved, and the cracks generated after the concrete is dried are reduced. The additive does not contain sodium, potassium and sulfate radical plasma, wherein the added vegetable gum reduces the slump of the concrete in the stirring process, improves the gelation of the concrete, and can simultaneously co-act with the coating agent of modified lepidolite extracted lithium tailings to further reduce the content of sodium, potassium, sulfate radical plasma and the like. The ethyl cyanoacrylate in the admixture is solidified after being wetted, and after 3,3', 4' -biphenyl tetracarboxylic dianhydride is added, the crosslinking degree of the polymer is further improved, so that the compressive strength of the concrete is further improved. The added microcrystalline wax cooperates with polyoxyethylene sorbitan palmitate, 2' -hydroxy-3-phenylpropionic acid and the like to prevent the vegetable gum from being oxidized in the concrete solidification and heat release process, thereby losing efficacy and improving the gelation of the concrete.
Example 1
A preparation method of lepidolite slag concrete.
The preparation process of the modified lepidolite lithium extraction tailings comprises the following steps:
(1) Taking 13 parts of lepidolite extracted lithium tailings, putting the 13 parts of lepidolite extracted lithium tailings into a ball mill for ball milling, wherein the specific surface area of the lepidolite extracted lithium tailings is 450m 2 Particles per kg for use;
(2) Taking 21 parts of butyl acrylate, 5 parts of 1,4,7,10,13, 16-hexaoxa-octadecane, 18 parts of styrene, adding methyl acetate solution, heating to 235 ℃ at the speed of 5 ℃/min, preserving heat and stirring for 6 hours, adding 15-crown ether-5 3 parts of hexafluoroisopropanol, 6 parts of pentenoate and 5 parts of polyvinyl alcohol fiber, transferring the mixture into a reaction kettle, controlling the temperature to 275 ℃, preserving heat and stirring for 5 hours, adding the mixture into the lepidolite extracted lithium tailings obtained in the step (1), and stirring uniformly to obtain the product.
The preparation method of the air entraining agent comprises the following steps:
5 parts of dodecyl dimethyl amine ethyllactone, 4 parts of cyclopropylmethyl ketone and methyl acetate are taken, the temperature is raised to 325 ℃ at the speed of 4 ℃/min, the temperature is kept for 4.5 hours after stirring, the solution temperature is controlled to 155 ℃,7 parts of humic acid and 4.5 parts of hexahydrophthalic anhydride are added, the temperature is raised to 213 ℃, the temperature is kept for 6.5 hours after stirring, 3.5 parts of methyl tributyl ketoxime silane is added, 5 parts of isooctyl hydroxystearate is poured into a homogenizing emulsification reaction kettle, the homogenizing emulsification reaction kettle is heated to 160 ℃, and the homogenizing emulsification is carried out, thus obtaining the product.
Preparation method of additive
Adding 6 parts of sesbania gum, 5 parts of guar gum and 5 parts of alkylphenol ethoxylate into an ethanol solution, heating to 145 ℃ at the speed of 3 ℃/min, adding 5 parts of ethyl cyanoacrylate and 3,3', 4' -biphenyl tetracarboxylic dianhydride after heat preservation and stirring for 4 hours, controlling the temperature of the solution to 235 ℃, adding 3 parts of polyoxyethylene sorbitan palmitate and 1.5 parts of 2' -hydroxy-3-phenylpropionyl ketone after heat preservation and stirring for 5.5 hours at the speed of 1.5 ℃/min, adding 5.5 parts of microcrystalline wax after heat preservation and stirring for 5 hours, and controlling the temperature of the solution to 65 ℃ to obtain the finished product.
The formula of the concrete raw materials is as follows: cement model P.042.5R13 parts, sand 33 parts, broken stone 43 parts, water 7 parts, mineral powder 2 parts, modified lepidolite lithium extraction tailings 2 parts, air entraining agent 0.15 parts and additive 0.15 parts;
the preparation method of the concrete comprises the following steps:
1) Weighing crushed stone and sand according to a proportion, putting the crushed stone and the sand into a stirrer, mixing and stirring for 1 minute, adding cement, modified lithium extraction tailings and mineral powder, and stirring for 1 minute for later use;
2) Adding the water reducer and the air entraining agent into water, controlling the temperature of the solution to be 60-70 ℃, stirring for 5-8min, adding the mixture in the step 1), and stirring for 4min together to obtain the water reducer.
Wherein, the broken stone is broken stone with the particle diameter of 17mm and the mud content is 0.3 percent;
the sand is natural sand, preferably river sand, with fineness modulus range of 2.6 and mud content of 0.2%.
Example 2
A preparation method of lepidolite slag concrete.
The preparation process of the modified lepidolite lithium extraction tailings comprises the following steps:
(1) 10 parts of lepidolite extracted lithium tailings are taken and put into a ball mill, and the specific surface area is 450m 2 Particles per kg for use;
(2) Taking 18 parts of butyl acrylate, 6 parts of 1,4,7,10,13, 16-hexaoxa-octadecane, 15 parts of styrene, adding methyl acetate solution, heating to 230 ℃ at the speed of 6 ℃/min, preserving heat and stirring for 7 hours, adding 5 parts of 15-crown ether-5 2 parts of hexafluoroisopropanol, 5 parts of pentenoate and 6 parts of polyvinyl alcohol fiber, transferring the mixture into a reaction kettle, controlling the temperature to 270 ℃, preserving heat and stirring for 6 hours, adding the mixture into the lepidolite extracted lithium tailings obtained in the step (1), and stirring uniformly to obtain the product.
The preparation method of the air entraining agent comprises the following steps:
4 parts of dodecyl dimethyl amine ethyllactone, 5 parts of cyclopropylmethyl ketone and methyl acetate are taken, the temperature is raised to 330 ℃ at the speed of 3 ℃/min, the temperature is kept for 4 hours after stirring, the solution temperature is controlled to 160 ℃, 6 parts of humic acid and 5 parts of hexahydrophthalic anhydride are added, the temperature is raised to 210 ℃, the temperature is kept for 7 hours after stirring, 3 parts of methyl tributyl ketoxime silane and 6 parts of isooctyl hydroxystearate are added, and the mixture is poured into a homogenizing emulsification reaction kettle for uniform mixing, heated to 160 ℃, and homogenized and emulsified to obtain the finished product.
Preparation method of additive
Adding 5 parts of sesbania gum, 6 parts of guar gum and 4 parts of alkylphenol polyoxyethylene ether into an ethanol solution, heating to 140 ℃ at the speed of 4 ℃/min, insulating and stirring for 5 hours, adding 4 parts of ethyl cyanoacrylate and 4 parts of 3,3', 4' -biphenyl tetracarboxylic dianhydride, controlling the temperature of the solution to 230 ℃, insulating and stirring for 6 hours, adding 2 parts of polyoxyethylene sorbitan palmitate and 2 parts of 2' -hydroxy-3-phenylpropionyl ketone, heating to 265 ℃ at the speed of 1 ℃/min, insulating and stirring for 5 hours, adding 6 parts of microcrystalline wax, controlling the temperature of the solution to 60 ℃, and insulating and stirring for 6 hours to obtain the finished product.
The formula of the concrete raw materials is as follows: cement model P.042.5R10 parts, sand 35 parts, broken stone 40 parts, water 7.5 parts, mineral powder 1.5 parts, modified lepidolite lithium extraction tailings 2.5 parts, air entraining agent 0.1 part and additive 0.2 part;
the preparation method of the concrete comprises the following steps:
1) Weighing crushed stone and sand according to a proportion, putting the crushed stone and the sand into a stirrer, mixing and stirring for 1 minute, adding cement, modified lithium extraction tailings and mineral powder, and stirring for 1 minute for later use;
2) Adding the water reducer and the air entraining agent into water, controlling the temperature of the solution to 60 ℃, stirring for 8min, adding the mixture in the step 1), and stirring for 3min together to obtain the water reducer.
Wherein, the broken stone is selected from broken stone with the grain diameter of 18mm, and the mud content is 0.3 percent;
the sand is natural sand, preferably river sand, with fineness modulus range of 2.5 and mud content of 0.45%.
Example 3
A preparation method of lepidolite slag concrete.
The preparation process of the modified lepidolite lithium extraction tailings comprises the following steps:
(1) 15 parts of lepidolite extracted lithium tailings are taken and put into a ball mill, and the specific surface area is 450m 2 Particles per kg for use;
(2) Taking 25 parts of butyl acrylate, 4 parts of 1,4,7,10,13, 16-hexaoxa-octadecane, 20 parts of styrene, adding methyl acetate solution, heating to 240 ℃ at the speed of 4 ℃/min, preserving heat and stirring for 5 hours, adding 15-crown ether-5 4 parts of hexafluoroisopropanol 3 parts, 7 parts of pentenoate and 4 parts of polyvinyl alcohol fiber, transferring the mixture into a reaction kettle, controlling the temperature to 280 ℃, preserving heat and stirring for 4 hours, adding the mixture into the lepidolite extracted lithium tailings obtained in the step (1), and stirring uniformly to obtain the product.
The preparation method of the air entraining agent comprises the following steps:
and (3) taking 6 parts of dodecyl dimethyl amine ethyllactone, 3 parts of cyclopropylmethyl ketone, adding methyl acetate, heating to 320 ℃ at a speed of 5 ℃/min, preserving heat and stirring for 5 hours, controlling the temperature of the solution to 150 ℃, adding 8 parts of humic acid and 4 parts of hexahydrophthalic anhydride, heating to 215 ℃, preserving heat and stirring for 6 hours, adding 4 parts of methyltributylketone oximido silane and 4 parts of isooctyl hydroxystearate, pouring the mixture into a homogenizing and emulsifying reaction kettle, uniformly mixing, heating to 160 ℃, and homogenizing and emulsifying the mixture to obtain the finished product.
Preparation method of additive
Adding 7 parts of sesbania gum, 4 parts of guar gum and 6 parts of alkylphenol ethoxylate into an ethanol solution, heating to 150 ℃ at the speed of 2 ℃/min, insulating and stirring for 3 hours, adding 6 parts of ethyl cyanoacrylate and 2 parts of 3,3', 4' -biphenyl tetracarboxylic dianhydride, controlling the temperature of the solution to 240 ℃, insulating and stirring for 5 hours, adding 4 parts of polyoxyethylene sorbitan palmitate and 1 part of 2' -hydroxy-3-phenylpropionyl ketone, heating to 260 ℃ at the speed of 2 ℃/min, insulating and stirring for 6 hours, adding 5 parts of microcrystalline wax, controlling the temperature of the solution to 70 ℃, and insulating and stirring for 4 hours to obtain the finished product.
The formula of the concrete raw materials is as follows: 15 parts of cement type P.042.5R15 parts, 30 parts of sand, 45 parts of broken stone, 6.5 parts of water, 2.5 parts of mineral powder, 1.5 parts of modified lepidolite lithium extraction tailings, 0.2 part of air entraining agent and 0.1 part of additive;
the preparation method of the concrete comprises the following steps:
1) Weighing crushed stone and sand according to a proportion, putting the crushed stone and the sand into a stirrer, mixing and stirring for 1 minute, adding cement, modified lithium extraction tailings and mineral powder, and stirring for 1 minute for later use;
2) Adding the water reducer and the air entraining agent into water, controlling the temperature of the solution to be 70 ℃, stirring for 5min, adding the mixture in the step 1), and stirring for 5min together to obtain the water reducer.
Wherein, the broken stone is selected from broken stone with the grain diameter of 15mm, and the mud content is 0.3 percent;
the sand is natural sand, preferably river sand, with fineness modulus range of 2.7 and mud content of 0.3%.
Comparative example 1
A preparation method of lepidolite slag concrete.
The preparation process of the modified lepidolite lithium extraction tailings comprises the following steps:
(1) Taking 13 parts of lepidolite extracted lithium tailings, and putting the 13 parts into a ball mill, wherein the specific surface area of the lepidolite extracted lithium tailings is 450m 2 Particles per kg for use;
(2) 21 parts of butyl acrylate, 18 parts of styrene, adding methyl acetate solution, heating to 235 ℃ at a speed of 5 ℃/min, preserving heat and stirring for 6 hours, adding 15-crown ether-5 3 parts, 4 parts of hexafluoroisopropanol and 6 parts of pentenoate, transferring 5 parts of polyvinyl alcohol fibers into a reaction kettle, controlling the temperature to 275 ℃, preserving heat and stirring for 5 hours, adding the obtained product into the lepidolite lithium extraction tailings obtained in the step (1), and stirring uniformly to obtain the product.
The procedure is as in example 1.
Comparative example 2
A preparation method of lepidolite slag concrete.
The preparation process of the modified lepidolite lithium extraction tailings comprises the following steps:
(1) Taking 13 parts of lepidolite extracted lithium tailings, and putting the 13 parts into a ball mill, wherein the specific surface area of the lepidolite extracted lithium tailings is 450m 2 Particles per kg for use;
(2) Taking 21 parts of butyl acrylate, 5 parts of 1,4,7,10,13, 16-hexaoxa-octadecane, 18 parts of styrene, adding methyl acetate solution, heating to 235 ℃ at a speed of 5 ℃/min, preserving heat and stirring for 6 hours, adding 4 parts of hexafluoroisopropanol, 6 parts of pentenoate, transferring 5 parts of polyvinyl alcohol fiber into a reaction kettle, controlling the temperature to 275 ℃, preserving heat and stirring for 5 hours, adding the lepidolite extracted lithium tailings in the step (1), and stirring uniformly to obtain the lithium ion battery.
The procedure is as in example 1.
Comparative example 3
A preparation method of lepidolite slag concrete.
The preparation process of the modified lepidolite lithium extraction tailings comprises the following steps:
(1) Taking 13 parts of lepidolite extracted lithium tailings, and putting the 13 parts into a ball mill, wherein the specific surface area of the lepidolite extracted lithium tailings is 450m 2 Particles per kg for use;
(2) Taking 21 parts of butyl acrylate, 5 parts of 1,4,7,10,13, 16-hexaoxa-octadecane, 18 parts of styrene, adding methyl acetate solution, heating to 235 ℃ at the speed of 5 ℃/min, preserving heat and stirring for 6 hours, adding 15-crown ether-5 3 parts of hexafluoroisopropanol and 6 parts of pentenoate, transferring the mixture into a reaction kettle, controlling the temperature to 275 ℃, preserving heat and stirring for 5 hours, adding the mixture into the lepidolite extracted lithium tailings obtained in the step (1), and stirring uniformly to obtain the lithium-ion battery lithium-acid battery.
The procedure is as in example 1.
Comparative example 4
A preparation method of lepidolite slag concrete.
The preparation process of the modified lepidolite lithium extraction tailings comprises the following steps:
(1) Taking 13 parts of lepidolite extracted lithium tailings, and putting the 13 parts into a ball mill, wherein the specific surface area of the lepidolite extracted lithium tailings is 450m 2 Particles per kg for use;
(2) 21 parts of butyl acrylate, 5 parts of 1,4,7,10,13, 16-hexaoxacyclooctadecane, 18 parts of styrene, 15-crown ether-5 3 parts of hexafluoroisopropanol, 6 parts of pentenoate and 5 parts of polyvinyl alcohol fiber are taken, methyl acetate solution is added, the mixture is transferred into a reaction kettle, the temperature is raised to 275 ℃ at the speed of 5 ℃/min, the mixture is kept warm and stirred for 11 hours, and then the mixture is added into the lepidolite extracted lithium tailings obtained in the step (1) and is stirred uniformly, so that the product is obtained.
The procedure is as in example 1.
Comparative example 5
A preparation method of lepidolite slag concrete.
The preparation method of the air entraining agent comprises the following steps:
taking 4 parts of cyclopropylmethyl ketone, adding methyl acetate, heating to 325 ℃ at the speed of 4 ℃/min, preserving heat and stirring for 4.5 hours, controlling the temperature of the solution to 155 ℃, adding 7 parts of humic acid and 4.5 parts of hexahydrophthalic anhydride, heating to 213 ℃, preserving heat and stirring for 6.5 hours, adding 3.5 parts of methyltributyroxime silane and 5 parts of isooctyl hydroxystearate, pouring the mixture into a homogenizing and emulsifying reaction kettle, uniformly mixing, heating to 160 ℃, and homogenizing and emulsifying the mixture to obtain the product.
The procedure is as in example 1.
Comparative example 6
A preparation method of lepidolite slag concrete.
The preparation method of the air entraining agent comprises the following steps:
5 parts of dodecyl dimethyl amine ethyllactone, 4 parts of cyclopropylmethyl ketone and methyl acetate are taken, the temperature is raised to 325 ℃ at the speed of 4 ℃/min, the heat preservation and stirring are carried out for 4.5 hours, the solution temperature is controlled to 155 ℃, 4.5 parts of hexahydrophthalic anhydride is added, the temperature is raised to 213 ℃, 3.5 parts of methyltributyroxime silane is added after the heat preservation and stirring are carried out for 6.5 hours, 5 parts of isooctyl hydroxystearate is poured into a homogenizing and emulsifying reaction kettle, the mixture is uniformly mixed, the heating is carried out to 160 ℃, and the homogenizing and emulsifying are carried out, thus obtaining the product.
The procedure is as in example 1.
Comparative example 7
A preparation method of lepidolite slag concrete.
The preparation method of the air entraining agent comprises the following steps:
5 parts of dodecyl dimethyl amine ethyllactone, 4 parts of cyclopropylmethyl ketone, 7 parts of humic acid, 4.5 parts of hexahydrophthalic anhydride and 3.5 parts of methyltributyroziridosilane are taken, 5 parts of isooctyl hydroxystearate is added into methyl acetate, the temperature is raised to 325 ℃ at the speed of 4 ℃/min, the mixture is kept warm and stirred for 11 hours, and then the mixture is poured into a homogenizing and emulsifying reaction kettle to be uniformly mixed, the temperature is controlled to 160 ℃, and the mixture is homogenized and emulsified to obtain the product.
The procedure is as in example 1.
Comparative example 8
A preparation method of lepidolite slag concrete.
Wherein the air entraining agent is sodium alkyl benzene sulfonate.
The procedure is as in example 1.
Comparative example 9
A preparation method of lepidolite slag concrete.
The preparation method of the additive comprises the following steps:
adding 6 parts of sesbania gum, 5 parts of guar gum and 5 parts of alkylphenol polyoxyethylene ether into an ethanol solution, heating to 145 ℃ at the speed of 3 ℃/min, adding 3 parts of 3,3', 4' -biphenyl tetracarboxylic dianhydride after heat preservation and stirring for 4 hours, controlling the temperature of the solution to 235 ℃, adding 1.5 parts of polyoxyethylene sorbitan palmitate and 1.5 parts of 2' -hydroxy-3-phenylpropiophenone after heat preservation and stirring for 5 hours at the speed of 1.5 ℃/min, adding 5.5 parts of microcrystalline wax after heat preservation and stirring for 5 hours at the temperature of 65 ℃ to obtain the finished product.
The procedure is as in example 1.
Comparative example 10
A preparation method of lepidolite slag concrete.
The preparation method of the additive comprises the following steps:
adding 6 parts of sesbania gum, 5 parts of guar gum and 5 parts of alkylphenol polyoxyethylene ether into an ethanol solution, heating to 145 ℃ at the speed of 3 ℃/min, adding 5 parts of ethyl cyanoacrylate after heat preservation and stirring for 4 hours, controlling the temperature of the solution to 235 ℃, adding 3 parts of polyoxyethylene sorbitan palmitate and 1.5 parts of 2' -hydroxy-3-phenylpropiophenone after heat preservation and stirring for 5.5 hours, heating to 263 ℃ at the speed of 1.5 ℃/min, adding 5.5 parts of microcrystalline wax after heat preservation and stirring for 5 hours, controlling the temperature of the solution to 65 ℃, and obtaining the finished product after heat preservation and stirring for 5 hours.
The procedure is as in example 1.
Comparative example 11
A preparation method of lepidolite slag concrete.
The preparation method of the additive comprises the following steps:
adding 5 parts of alkylphenol ethoxylates into an ethanol solution, heating to 145 ℃ at a speed of 3 ℃/min, preserving heat and stirring for 4 hours, adding 5 parts of ethyl cyanoacrylate and 3,3', 4' -biphenyl tetracarboxylic dianhydride, controlling the temperature of the solution to 235 ℃, preserving heat and stirring for 5.5 hours, adding 3 parts of polyoxyethylene sorbitan palmitate and 1.5 parts of 2' -hydroxy-3-phenylpropionyl acetone, heating to 263 ℃ at a speed of 1.5 ℃/min, preserving heat and stirring for 5.5 hours, adding 5.5 parts of microcrystalline wax, controlling the temperature of the solution to 65 ℃, and preserving heat and stirring for 5 hours to obtain the modified polyoxyethylene sorbitan palmitate.
The procedure is as in example 1.
Comparative example 12
A preparation method of lepidolite slag concrete.
The preparation method of the additive comprises the following steps:
6 parts of sesbania gum, 5 parts of guar gum, 5 parts of alkylphenol polyoxyethylene ether, 5 parts of ethyl cyanoacrylate, 3 parts of 3,3', 4' -biphenyl tetracarboxylic dianhydride, 3 parts of polyoxyethylene sorbitan palmitate and 1.5 parts of 2' -hydroxy-3-phenylpropionyl ketone are taken, an ethanol solution is added, the temperature is raised to 263 ℃ at the speed of 3 ℃/min, after heat preservation and stirring for 15 hours, 5.5 parts of microcrystalline wax is added, the temperature of the solution is controlled to 65 ℃, and heat preservation and stirring for 5 hours are carried out, thus obtaining the finished product.
The procedure is as in example 1.
Comparative example 13
A preparation method of lepidolite slag concrete.
The concrete raw material formula comprises the following components: cement model P.042.5R13 parts, sand 33 parts, broken stone 43 parts, water 7 parts, mineral powder 2 parts, lepidolite lithium extraction tailings 2 parts, air entraining agent 0.15 parts and additive 0.15 parts;
the procedure is as in example 1.
Comparative example 14
A preparation method of lepidolite slag concrete.
The concrete raw material formula comprises the following components: cement model P.042.5R13 parts, sand 33 parts, broken stone 43 parts, water 7 parts, mineral powder 2 parts, modified lepidolite extracted lithium tailings 2 parts and additive 0.15 part;
the procedure is as in example 1.
Comparative example 15
A preparation method of lepidolite slag concrete.
The concrete raw material formula comprises the following components: cement model P.042.5R13 parts, sand 33 parts, broken stone 43 parts, water 7 parts, mineral powder 2 parts, modified lepidolite extracted lithium tailings 2 parts and air entraining agent 0.15 parts.
The procedure is as in example 1.
Experimental example 1 Strength of concrete
The concrete prepared in the examples and the comparative examples are tested for 7-day and 28-day compressive strength according to the national standard GB/T50107-2010 concrete strength test evaluation Standard, and specific results are recorded in Table 1;
table 1 compressive strength of concrete
As can be seen from table 1, the concrete prepared in the examples has excellent compressive strength compared with the comparative examples. Comparative examples 1-4 adjustments were made to the raw material formulation and steps in the process of preparing the modified lepidolite lithium extraction tailings, with a 28 day compressive strength of the final concrete of only 32.6-34.2 MPa. Comparative examples 5-7 the raw material formulation of the air entraining agent was changed, the preparation process of the admixture adjusted in comparative examples 9-12, but the properties of the final concrete were much lower than in examples. The lepidolite tailing added in comparative example 13 was not modified, so that the compressive strength of the concrete was only 12.4MPa for 7 days and only 20.9MPa for 28 days.
Experimental example 2 slump and expansion Property of concrete
The concrete prepared in the examples and the comparative examples were tested for slump and expansion according to the national standard GB/T50080-2016 Standard of the method for testing the Experimental Property of mixing Property of ordinary concrete, and specific results are recorded in Table 2;
TABLE 2 slump and expansion of concrete
Slump refers to the workability of concrete, and ensures normal progress of construction, including water retention, fluidity and cohesiveness of concrete. The slump is measured by a quantization index, and is used for judging whether the construction can be normally performed. Workability refers to whether concrete is easy to work and is uniformly dense, including fluidity, cohesiveness, and water retention. As can be seen from Table 2, the concrete prepared in examples 1-3 had slump of 193-205mm and expansion of 511-520mm, and was suitable for processing and stirring of concrete. And the fluidity and cohesiveness of the concrete prepared after the formula of the concrete is adjusted are not suitable for processing and stirring.

Claims (2)

1. The lepidolite slag concrete is characterized in that: the formula of the concrete raw materials is as follows: 10-15 parts of cement model P.042.5R10-35 parts of sand, 40-45 parts of broken stone, 6.5-7.5 parts of water, 1.5-2.5 parts of mineral powder, 1.5-2.5 parts of modified lepidolite lithium extraction tailings, 0.1-0.2 part of air entraining agent and 0.1-0.2 part of additive;
the preparation method of the concrete comprises the following steps:
1) Weighing broken stone and sand according to a proportion, putting the broken stone and the sand into a stirrer, mixing and stirring for 1 minute, adding cement and modified lepidolite to extract lithium tailings, and stirring for 1 minute for later use;
2) Adding the air entraining agent and the additive into water, controlling the temperature of the solution to be 60-70 ℃, stirring for 5-8min, adding the mixture in the step 1), and stirring for 3-5min together to obtain the air entraining agent;
wherein the crushed stone is 15-18mm in particle size and has a mud content of 0.3%;
the sand is natural sand, the fineness modulus range is 2.5-2.7, and the mud content is less than or equal to 0.45%;
the preparation process of the modified lepidolite lithium extraction tailings comprises the following steps:
(1) Taking 10-15 parts of lepidolite extracted lithium tailings, putting the lepidolite extracted lithium tailings into a ball mill for ball milling, wherein the specific surface area of the lepidolite extracted lithium tailings is not less than 400m 2 Particles per kg for use;
(2) Taking 18-25 parts of butyl acrylate, 4-6 parts of 1,4,7,10,13, 16-hexaoxacycle octadecane, 15-20 parts of styrene, adding methyl acetate solution, heating to 230-240 ℃ at the speed of 4-6 ℃/min, preserving heat and stirring for 5-7 hours, adding 15-crown ether-5 2-4 parts, 3-5 parts of hexafluoroisopropanol, 5-7 parts of pentenoate and 4-6 parts of polyvinyl alcohol fibers, transferring the polyvinyl alcohol fibers into a reaction kettle, controlling the temperature to 270-280 ℃, preserving heat and stirring for 4-6 hours, adding the mixture into the lepidolite extracted lithium tailings of the step (1), and stirring uniformly to obtain the product;
wherein, the preparation method of the additive comprises the following steps:
adding 5-7 parts of sesbania gum, 4-6 parts of guar gum and 4-6 parts of alkylphenol ethoxylates into ethanol solution, heating to 140-150 ℃ at the speed of 2-4 ℃/min, insulating and stirring for 3-5 hours, adding 4-6 parts of ethyl cyanoacrylate and 2-4 parts of 3,3', 4' -biphenyl tetracarboxylic dianhydride, controlling the temperature of the solution to 230-240 ℃, insulating and stirring for 5-6 hours, adding 2-4 parts of polyoxyethylene sorbitan palmitate and 1-2 parts of 2' -hydroxy-3-phenylpropionyl acetone, heating to 260-265 ℃ at the speed of 1-2 ℃/min, insulating and stirring for 5-6 hours, adding 5-6 parts of microcrystalline wax, controlling the temperature of the solution to 60-70 ℃, and insulating and stirring for 4-6 hours.
2. A lepidolite residue concrete according to claim 1, wherein: the preparation method of the air entraining agent comprises the following steps:
4-6 parts of dodecyl dimethyl amine ethyllactone, 3-5 parts of cyclopropylmethyl ketone and methyl acetate are taken, the temperature is raised to 320-330 ℃ at the speed of 3-5 ℃/min, the temperature of the solution is controlled to be 150-160 ℃ after heat preservation and stirring for 4-5 hours, 6-8 parts of humic acid and 4-5 parts of hexahydrophthalic anhydride are added, the temperature is raised to 210-215 ℃ after heat preservation and stirring for 6-7 hours, 3-4 parts of methyltributylketone oxime silane and 4-6 parts of isooctyl hydroxystearate are added, and the mixture is poured into a homogenizing and emulsifying reaction kettle to be uniformly mixed, heated to 160 ℃, and homogenized and emulsified to obtain the product.
CN202211307459.7A 2022-10-25 2022-10-25 Lepidolite slag concrete Active CN115872695B (en)

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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105503075A (en) * 2015-12-21 2016-04-20 乔俊擎 Scour-resistant and abrasion-resistant concrete for hydraulic engineering and preparation method thereof
CN111606614A (en) * 2020-05-06 2020-09-01 江西理工大学 Filling material containing lithium mica slag and preparation method and application thereof

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105503075A (en) * 2015-12-21 2016-04-20 乔俊擎 Scour-resistant and abrasion-resistant concrete for hydraulic engineering and preparation method thereof
CN107244860A (en) * 2015-12-21 2017-10-13 乔俊擎 A kind of hydraulic engineering scour and abrasion resistant concrete and preparation method thereof
CN111606614A (en) * 2020-05-06 2020-09-01 江西理工大学 Filling material containing lithium mica slag and preparation method and application thereof

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