CN111302708B - Comprehensive utilization technology of large-volume lithium slag waste and implementation method thereof - Google Patents
Comprehensive utilization technology of large-volume lithium slag waste and implementation method thereof Download PDFInfo
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- CN111302708B CN111302708B CN202010125483.3A CN202010125483A CN111302708B CN 111302708 B CN111302708 B CN 111302708B CN 202010125483 A CN202010125483 A CN 202010125483A CN 111302708 B CN111302708 B CN 111302708B
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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
- C04B28/006—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 mineral polymers, e.g. geopolymers of the Davidovits type
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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
- C04B2201/52—High compression strength concretes, i.e. with a compression strength higher than about 55 N/mm2, e.g. reactive powder concrete [RPC]
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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
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P40/00—Technologies relating to the processing of minerals
- Y02P40/10—Production of cement, e.g. improving or optimising the production methods; Cement grinding
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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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Abstract
The invention discloses a large-volume lithium slag waste comprehensive utilization technology and an implementation method thereof, wherein the prepared lithium slag geopolymer material comprises, by weight, 50-100 parts of lithium slag, 0-60 parts of admixture, 1-10 parts of activator, 0-5 parts of water reducing agent, 1-5 parts of chelating agent and 20-60 parts of water. The lithium slag geopolymer material prepared by the method has good working performance, mechanical strength and durability, can replace common cement-based cementing materials, and is widely applied to building materials.
Description
Technical Field
The invention relates to the field of comprehensive utilization of solid wastes, in particular to a comprehensive utilization technology of large-volume lithium slag wastes and an implementation method thereof.
Background
Lithium is called as energy metal of 21 st century, which has important significance in modern national economy and national defense construction, with the increase of consumption markets of electronic products, power batteries (field of new energy vehicles) and the like, the total lithium consumption of China will be further improved, especially, the realization of the scale application of new energy vehicles is required at the present stage, a power battery industrial chain with global competitiveness is built, the improvement project of new energy vehicle power batteries is promoted, the total lithium consumption is more and more large, and reportedly, the total lithium consumption of the domestic market in 2019 China is probably about 2000 tons, and the total lithium consumption of the global metal reaches about 30 million tons.
However, lithium or lithium salts can generate a large amount of lithium slag in the production process, 8-10 tons of lithium slag are generated in each 1 ton of lithium salts, waste slag generated by lithium or lithium salts prepared by different preparation methods accounts for more than 90% of the total amount of minerals, the yield of lithium slag in China at present is about 120 ten thousand tons every year, and the generation of a large amount of lithium slag always troubles lithium production enterprises.
At present, the method for treating the lithium slag basically adopts landfill and damming stockpiling, the treatment mode is not only wasteful and harmful to the environment and is easy to cause pollution to land, air and underground water, but also at present, much research is carried out on the lithium slag as an admixture for a cement concrete material, but the content of the lithium slag is low (generally within 30 wt%), along with the addition of the lithium slag, the mechanical property of the cement concrete material is obviously reduced, the comprehensive utilization effect of the lithium slag is not ideal, and millions of tons of lithium slag are reportedly stockpiled in a lithium salt field in Xinjiang.
Accordingly, the prior art is yet to be improved and developed.
Disclosure of Invention
In view of the above-mentioned shortcomings of the prior art, the present invention aims to provide a comprehensive utilization technology of large-volume lithium slag waste and a realization method thereof, and aims to solve the technical problems of low utilization rate of the conventional lithium slag waste and great influence on ecological environment.
The technical scheme of the invention is as follows:
the comprehensive utilization technology of the large-volume lithium slag waste is characterized in that the lithium slag waste is used for preparing a geopolymer material of the lithium slag, and the geopolymer material of the lithium slag comprises the following components in parts by weight:
50-100 parts of lithium slag;
0-60 parts of admixture;
1-10 parts of an excitant;
0-5 parts of a water reducing agent;
1-5 parts of a chelating agent;
20-60 parts of water.
The comprehensive utilization technology of the large-volume lithium slag waste is characterized in that the lithium slag is pretreated lithium slag, and the pretreatment process comprises the following steps:
and (3) drying the lithium slag in an oven, and then grinding the lithium slag by using a ball mill to prepare the lithium slag with the median diameter of 2-25 mu m.
The comprehensive utilization technology of the large-volume lithium slag waste comprises the following steps of mixing materials including fly ash, slag and silica fume.
The comprehensive utilization technology of the large-volume lithium slag waste is characterized in that the excitant is one or more of an acid excitant, an alkali excitant, a salt excitant and an organic metal compound excitant.
The comprehensive utilization technology of the large-volume lithium slag waste comprises the step of comprehensively utilizing the large-volume lithium slag waste, wherein the chelating agent is one or more of phosphoric acid and derivatives thereof, citric acid and derivatives thereof, oxalic acid and derivatives thereof, and ethylenediaminetetraacetic acid and derivatives thereof.
The comprehensive utilization technology of the large-volume lithium slag waste is characterized in that the water reducing agent is a polycarboxylic acid water reducing agent.
A method for realizing a large-volume lithium slag waste comprehensive utilization technology comprises the following steps:
mixing the lithium slag, the admixture, the activator, the water reducing agent, the chelating agent and the water, and uniformly mixing to obtain a mixture;
adding water into the mixture, uniformly stirring, and pouring and forming to obtain a young blank;
and curing the young blank to obtain the lithium slag geopolymer material.
The method for realizing the large-volume lithium slag waste comprehensive utilization technology comprises the following steps of mixing the lithium slag, the admixture, the activator, the water reducer, the chelating agent and water, and uniformly mixing the mixture to obtain a mixture, wherein the method comprises the following steps:
and (3) drying the lithium slag in an oven at the temperature of 60-105 ℃, and then, grinding for 0-3mins by using a ball mill to prepare the lithium slag with the median diameter of 2-25 mu m.
The implementation method of the large-volume lithium slag waste comprehensive utilization technology comprises the following steps of:
maintaining at 20 + -1 deg.C and 95 + -5% relative humidity for 7 days.
Has the advantages that: the invention provides a large-volume lithium slag waste comprehensive utilization technology and a realization method thereof, wherein a large amount of lithium slag waste is used in the prepared lithium slag geopolymer material, the utilization rate of lithium slag is improved, the ecological environment is protected, and meanwhile, the prepared lithium slag geopolymer has better working performance, mechanical strength and durability, can replace common cement-based cementing materials, and can be widely applied to building materials.
Drawings
FIG. 1 is a flow chart of a method for preparing a geopolymer material with a large amount of lithium slag according to a preferred embodiment of the present invention.
FIG. 2 is an SEM image of a lithium slag geopolymer material prepared in example 1 of the present invention.
FIG. 3 is an SEM image of a geopolymer material of lithium slag prepared in example 4 of the present invention.
Detailed Description
The invention provides a comprehensive utilization technology of large-volume lithium slag waste and an implementation method thereof, and the invention is further described in detail below in order to make the purpose, technical scheme and effect of the invention clearer and clearer. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
The invention provides a comprehensive utilization technology of a large amount of lithium slag waste, wherein the lithium slag waste is used for preparing a geopolymer material of lithium slag, and the geopolymer material of lithium slag comprises the following components in parts by weight: 50-100 parts of lithium slag, 0-60 parts of admixture, 1-10 parts of excitant, 0-5 parts of water reducing agent, 1-5 parts of chelating agent and 20-60 parts of water.
The large-doping-amount lithium slag geopolymer material provided by the invention has large doping amount of lithium slag, can quickly consume the existing lithium slag waste, reduces the influence on the ecological environment, simultaneously, the larger the doping amount of the lithium slag in the lithium slag geopolymer material is, the better the chlorine ion permeation resistance is, the electric flux of the common geopolymer material is 1500C, the electric flux of the lithium slag geopolymer material prepared by the invention can be reduced to 650C, and in addition, the drying shrinkage rate of the common geopolymer material is 800 to 10-6The drying shrinkage rate of the lithium slag geopolymer material prepared by the invention can be reduced to 300 x 10 to the minimum-6Compared with the common geopolymer material, the drying shrinkage performance of the geopolymer material of the lithium slag is improvedCompared with the common geopolymer material, the lithium slag geopolymer material provided by the invention has better durability, and the lithium slag geopolymer material with the compressive strength ranging from 1 MPa to 95MPa and the fluidity ranging from 8 cm to 20cm can be designed according to requirements.
Further, in the present invention, the lithium slag is pretreated lithium slag, and the pretreatment process includes:
and (3) drying the lithium slag in an oven, and then grinding the lithium slag by using a ball mill to prepare the lithium slag with the median diameter of 2-25 mu m.
According to the invention, the lithium slag is pretreated to be dried firstly, and then is ground by adopting a ball mill to form the lithium slag with the particle size range of 2-25 mu m, and when the lithium slag is subsequently mixed with the admixture, the excitant, the water reducing agent and the chelating agent, the lithium slag is uniformly dispersed, and the mechanical property and the durability of the prepared geopolymer material of the lithium slag are not influenced by the agglomeration or the nonuniform dispersion.
Further, in the present invention, the admixture includes fly ash, slag and silica fume. In the invention, the admixture is 0-60 parts by weight, wherein the fly ash is 0-20 parts by weight, the slag is 0-20 parts by weight, the silica fume is 0-20 parts by weight, and the fly ash, the slag and the silica fume can be the same or different in parts by weight.
Further, in the present invention, the activator is one or more of an acid activator, a base activator, a salt activator, and an organometallic compound activator. In the invention, the acid activator can be selected from sulfuric acid, carbonic acid, phosphoric acid and other substances, the alkali activator can be selected from sodium hydroxide, calcium hydroxide, potassium hydroxide and other substances, the salt activator can be selected from sodium chloride, calcium carbonate, sodium silicate and other substances, and the organic metal compound activator can be selected from sodium methoxide, sodium ethoxide and other substances.
Further, in the invention, the chelating agent is one or more of phosphoric acid and derivatives thereof, citric acid and derivatives thereof, oxalic acid and derivatives thereof, and ethylenediaminetetraacetic acid and derivatives thereof. In the invention, the chelating agent includes, but is not limited to, one or more of the above phosphoric acid and its derivatives, citric acid and its derivatives, oxalic acid and its derivatives, and ethylenediaminetetraacetic acid and its derivatives, wherein the added chelating agent has dual effects on heavy metal in the waste gas of the lithium slag, on one hand, the chelating agent can perform a complexing reaction with heavy metal ions, thereby reducing the heavy metal pollution degree of the prepared large-doped lithium slag geopolymer material, and preparing a more environment-friendly lithium slag geopolymer material, and on the other hand, the chelating agent can adjust the pH value of the lithium slag to a certain extent, thereby improving the pH value in the preparation process of the lithium slag geopolymer material, so that after the adjustment of the chelating agent, a pH environment suitable for synthesis of the lithium slag geopolymer material is achieved, and the lithium slag geopolymer material with better mechanical properties and durability is prepared.
Further, in the invention, the water reducing agent is a polycarboxylic acid water reducing agent.
The invention also provides a realization method of the comprehensive utilization technology of the large-volume lithium slag waste, which comprises the following steps:
s10, mixing the lithium slag, the admixture, the excitant, the water reducer, the chelating agent and water to obtain a mixture;
s20, adding water into the mixture, uniformly stirring, and pouring to obtain a young blank;
and S30, curing the young blank to obtain the lithium slag geopolymer material.
In the invention, in step S10, the activator may not be added to mix, and when water is added to the mixture and stirred in step S20, the activator is added to the water to prepare an aqueous solution of the activator, and the aqueous solution of the activator is added to the mixture and stirred uniformly, and then the mixture is poured to form a blank.
Further, in the present invention, the method for implementing the large-volume lithium slag waste comprehensive utilization technology, wherein the step of mixing the lithium slag, the admixture, the activator, the water reducing agent, the chelating agent and the water to uniformly mix them to obtain the mixture further comprises:
and (3) drying the lithium slag in an oven at the temperature of 60-105 ℃, and then, grinding for 0-3mins by using a ball mill to prepare the lithium slag with the median diameter of 2-25 mu m.
According to the invention, the lithium slag is pretreated, so that the lithium slag is easier to be uniformly mixed with the admixture, meanwhile, the lithium slag is ground by the ball mill to form the lithium slag powder with the median diameter of 2-25 μm, the contact area of the chelating agent and the lithium slag powder is increased, and the chelating agent is more fully subjected to a complexing reaction with the heavy metal in the lithium slag powder.
Furthermore, in the present invention, the method for implementing the large-volume comprehensive utilization technology of lithium slag waste comprises the following steps:
maintaining at 20 + -1 deg.C and 95 + -5% relative humidity for 7 days.
The invention is further illustrated by the following specific examples:
example 1
Preparing raw materials: 60 parts of lithium slag, 15 parts of slag, 5 parts of silica fume, 5 parts of activator sodium silicate (water glass with the modulus of 2M), 5 parts of chelating agent sodium ethylene diamine tetracetate and 28 parts of water.
Material synthesis: mixing the lithium slag, the slag and the silica fume which are subjected to the powder treatment by the ball mill by using a mixer, adding sodium silicate, sodium ethylene diamine tetracetate and water into the mixer for continuous mixing, setting the mixing time to be 10mins to obtain a mixture, adding water into the mixture, stirring, pouring and forming to obtain a young blank, and performing maintenance treatment on the young blank to obtain the lithium slag geopolymer material.
Example 2
Preparing raw materials: 100 parts of lithium slag, 5 parts of activator sodium silicate (powder anhydrous sodium silicate), 2 parts of water reducing agent, 1 part of chelating agent magnesium phosphate and 30 parts of water.
Material synthesis: mixing the lithium slag, sodium silicate and magnesium phosphate which are subjected to powder treatment by the ball mill by using a mixer, adding water into the mixer for continuously mixing, setting the mixing time to be 10min to obtain a mixture, adding water into the mixture, stirring, pouring and forming to obtain a young blank, and curing the young blank to obtain the lithium slag geopolymer material.
Example 3
Preparing raw materials: 60 parts of lithium slag, 15 parts of slag, 5 parts of silica fume, 8 parts of activator sodium silicate (water glass with the modulus of 2M), 1 part of water reducing agent, 4 parts of chelating agent ethylene diamine tetraacetic acid and 30 parts of water.
Material synthesis: mixing the lithium slag, the slag and the silica fume which are subjected to the powder treatment by the ball mill by using a mixer, adding sodium silicate, a water reducing agent, ethylene diamine tetraacetic acid and water into the mixer for continuous mixing, setting the mixing time to be 10min to obtain a mixture, adding water into the mixture, stirring, pouring and forming to obtain a young blank, and performing maintenance treatment on the young blank to obtain the lithium slag geopolymer material.
In the invention, the performance of the lithium slag geopolymer materials prepared in the three groups of examples is detected, and the experimental results shown in the following chart are obtained:
the electric flux and the fluidity of the common geopolymer material without the lithium slag are respectively 1200C (6h) and 80mm, and the data in the figure show that the electric flux and the fluidity of the geopolymer material without the lithium slag are respectively superior to those of the common geopolymer material without the lithium slag, the compressive strength is high, furthermore, the durability of the material can be judged by detecting the electric flux and the carbonization depth of the material, if the numerical values of the electric flux and the carbonization depth of the material are lower, the durability of the material is better, the data in the figure show that the electric flux and the 28d carbonization depth of the geopolymer material with the lithium slag prepared by the invention are lower, and the prepared geopolymer material with the lithium slag also has better durability, so the geopolymer material with the lithium slag prepared by the invention has better working performance, mechanical strength and durability, and can replace common cement-based gelled material, can be widely applied to building materials.
Further, in the present invention, the shape of the lithium slag geopolymer material prepared in example 1 is observed to obtain an SEM image of the material, as shown in fig. 2, and the shape of the lithium slag geopolymer material used as a reference is prepared by the same method except for the exciting agent used for the raw material in example 1, and the SEM image of the material is obtained by observing the shape of the lithium slag geopolymer material used as a reference, as shown in fig. 3, as can be seen from fig. 2 and 3, the structure of the lithium slag geopolymer material added with the exciting agent in fig. 2 is more dense, and obvious hydration products can be seen on the surface, while the structure of the lithium slag geopolymer material not added with the exciting agent in fig. 3 is loose, and no hydration products can be seen on the surface. Therefore, the invention can prepare the lithium slag geopolymer materials with different functions by adopting different raw material proportions according to different performance requirements.
In conclusion, the invention provides a comprehensive utilization technology of large-volume lithium slag waste and an implementation method thereof, the prepared lithium slag geopolymer material uses a large amount of lithium slag waste, the utilization rate of lithium slag is improved, the ecological environment is protected, and meanwhile, the working performance, the mechanical strength and the durability of the prepared large-volume lithium slag geopolymer material are adjusted by adjusting the types of the exciting agent and the chelating agent and the proportion of each component in the lithium slag geopolymer material, so that the large-volume lithium slag geopolymer material can adapt to different use occasions, replaces a common cement-based cementing material, and is widely applied to building materials.
It is to be understood that the invention is not limited to the examples described above, but that modifications and variations may be effected thereto by those of ordinary skill in the art in light of the foregoing description, and that all such modifications and variations are intended to be within the scope of the invention as defined by the appended claims.
Claims (7)
1. The comprehensive utilization technology of the large-volume lithium slag waste is characterized in that the lithium slag waste is used for preparing a geopolymer material of the lithium slag, and the geopolymer material of the lithium slag comprises the following components in parts by weight:
50-100 parts of lithium slag;
0-60 parts of admixture;
1-10 parts of an excitant;
0-5 parts of a water reducing agent;
1-5 parts of a chelating agent;
20-60 parts of water;
the method comprises the following steps of (1) pretreating lithium slag, wherein the lithium slag is pretreated lithium slag, and the pretreatment process comprises the following steps:
drying the lithium slag in an oven, and then grinding the lithium slag by using a ball mill to prepare the lithium slag with the median diameter of 2-25 mu m;
the chelating agent is one or more of phosphoric acid and derivatives thereof, citric acid and derivatives thereof, and ethylenediaminetetraacetic acid and derivatives thereof.
2. The large-volume lithium slag waste recycling technology as claimed in claim 1, wherein the admixture comprises fly ash, slag and silica fume.
3. The comprehensive utilization technology of the large-volume lithium slag waste according to claim 1, wherein the activator is one or more of an acid activator, a base activator, a salt activator and an organometallic compound activator.
4. The comprehensive utilization technology of the large-volume lithium slag waste according to claim 1, wherein the water reducing agent is a polycarboxylic acid water reducing agent.
5. A method for realizing the comprehensive utilization technology of the large-volume lithium slag waste as claimed in any one of claims 1 to 4, which is characterized by comprising the following steps:
mixing the lithium slag, the admixture, the activator, the water reducing agent, the chelating agent and the water, and uniformly mixing to obtain a mixture;
adding water into the mixture, uniformly stirring, and pouring and forming to obtain a young blank;
and curing the young blank to obtain the lithium slag geopolymer material.
6. The method for realizing the large-volume lithium slag waste comprehensive utilization technology according to claim 5, wherein the step of mixing the lithium slag, the admixture, the activator, the water reducer, the chelating agent and the water to uniformly mix the mixture is further performed before the step of obtaining the mixture, and the method further comprises the following steps:
and (3) drying the lithium slag in an oven at the temperature of 60-105 ℃, and then, grinding for 0-3mins by using a ball mill to prepare the lithium slag with the median diameter of 2-25 mu m.
7. The method for realizing the comprehensive utilization technology of the large-volume lithium slag waste as claimed in claim 5, wherein the step of maintaining the young blanks comprises the following steps:
maintaining at 20 + -1 deg.C and 95 + -5% relative humidity for 7 days.
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| CN114605113A (en) * | 2021-12-29 | 2022-06-10 | 成都宏基建材股份有限公司 | Lithium slag concrete prepared from pure industrial waste slag and preparation method thereof |
| CN114643271A (en) * | 2022-03-25 | 2022-06-21 | 珠海广隆新材料科技有限公司 | Solid waste lithium slag and treatment method and application thereof |
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| CN115893888A (en) * | 2023-02-03 | 2023-04-04 | 成都工业学院 | Lithium slag-based early-strength high-strength cementing material and preparation method thereof |
| CN117361917A (en) * | 2023-10-30 | 2024-01-09 | 石家庄市长安育才建材有限公司 | Lithium slag composite admixture, preparation method thereof and sprayed concrete |
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