CN107634221A - A kind of synthetic method for the ferrous silicate lithium anode material that bismuth doping is prepared using iron tailings as raw material - Google Patents
A kind of synthetic method for the ferrous silicate lithium anode material that bismuth doping is prepared using iron tailings as raw material Download PDFInfo
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Abstract
The present invention relates to a kind of synthetic method for the ferrous silicate lithium anode material that bismuth doping is prepared using iron tailings as raw material, first sodium silicate solution is prepared by raw material of iron tailings, then ferrous nitrate is added into sodium silicate solution and obtains ferrous metasilicate precipitation, lithia and di-iron trioxide are mixed into deposit again, finally calcines, cool down the ferrosilicon silicate of lithium sample for obtaining bismuth doping.Ferrosilicon silicate of lithium system material is a kind of important anode material of lithium battery, and comprehensive utilization, environmental protection and the development of promotion new and high technology of this method for iron tailings, which all have, to be of great significance.
Description
Technical field
The present invention relates to it is a kind of using iron tailings as raw material prepare bismuth doping ferrous silicate lithium anode material synthetic method,
Belong to field of inorganic nonmetallic material.
Background technology
Mineral Resources in China taste is relatively low, and using preceding needing by ore dressing, remaining solid waste is remained after ore dressing
Referred to as mine tailing.Iron ore remaining solid waste after the specific sorting process of Iron Works Plant is referred to as iron tailings.Iron ore
Masonry is the main source of steel, and with going from strength to strength for China's steel industry in recent decades, its demand is also continuously increased.Again
After the price increase of iron ore concentrate, putting more effort for iron ore is exploited, the stockpiling quantity of iron tailings drastically rises.China's iron tail
The stockpiling quantity of ore deposit once reached 1 year more than ten00000000 tons.Iron tailings is generally landfill placement, occupies substantial amounts of land resource.Its
Body exists and a kind of wasting of resources.Iron tailings granularity after sorting is smaller and long-term air storage, airborne dust of blowing, causes air
Pollution.Some iron tailings stack place close to river, cause water pollution.Iron tailings also can be to the soil reclamation dirt of its surrounding area
Dye, causes the harm of the farmland underproduction.Improvement and secondary use to iron tailings have become China's big problem urgently to be resolved hurrily.
The chemical composition of the iron tailings of table 1
Fe2O3 | SiO2 | Al2O3 | CaO | MgO | Na2O | K2O |
8.28 | 61.03 | 14.38 | 5.99 | 4.31 | 2.98 | 3.03 |
The content of iron tailings wherein metal after selected is very low, is mostly nonmetallic substance, main component SiO2, with
And a small amount of Fe2O3、MgO、Al2O3, CaO etc., wherein SiO2Content be generally higher than 50wt%, there are very big utilization
Value.Specific composition is as shown in table 1.According to the composition characteristic of iron tailings, researcher has carried out the recycling of iron tailings
Work, specific utilization power are as follows:
1st, iron tailings selects again.The resource utilization of part ore is low, and it is higher to handle later iron tailings iron content, can pass through correlation
Equipment carries out secondary sorting to iron tailings, obtains high-quality iron ore concentrate.
2nd, Applying Iron Tailings as Building Material.One of maximum building material product of Building Trade in China dosage is exactly building brick,
Iron tailings substitution clay is used as the primary raw material of production building brick, not only solves infringement problem of the clay reduction to cultivated land
The resource utilization issue of the iron tailings of solution.
3rd, mine worked-out section is filled.Its stockpiling problem that the goaf in mine solves, the soil avoided are filled with iron tailings
The waste of ground resource.Furthermore the mine worked-out section after being filled avoids the generation collapsed, so as to which win-win progress can be realized
Situation.
4th, soil conditioner and trace-element fertilizer are produced.The Zn usually contained in iron tailings, Mn, Cu, Mo, V, B, Fe, P
Deng trace element, we can also be produced by trace element necessary to adding N, P, K etc. plant soil conditioner and
Fertilizer.There is experiment to show to add the soil conditioner and trace-element fertilizer that iron tailings is produced, farming produce in soil
Amount greatly improves.
5th, re-vegetation.Iron tailings is discharged into the place of the unsuitable crop growth such as barren beach, one is covered on its surface
Various crops can be planted by determining the soil of thickness.The way built up fields of reclaiming solves the problems, such as airborne dust to the wind, increases cultivated land face
Product, there is very big benifit in terms of land resource.
6th, materialized application.By iron tailings and other raw material hybrid process, the material with certain application value is obtained.Mesh
The materialized application technology of preceding iron tailings, which is concentrated mainly on, prepares construction material aspect.Application No. 201310620026.1 it is special
Profit reports a kind of preparation method of Low-silica iron ore tailings expanded ceramsite, and the invention uses Low-silica iron ore tailings powder, coal dust, clay as original
Material has prepared expanded ceramsite by techniques such as drying, mixing, balling-up, calcinings.5~25mm of particle diameter haydite can be used as building
Light ceramsite concrete aggregate, heat preserving and insulating material or gardens haydite.The patent report of Application No. 201010569847.3
Iron tailings and blast furnace slag are mixed, are heated to melting by a kind of method that inorganic slag fibre is prepared using iron tailings, the invention
After state, inorganic slag fibre is prepared through being blown or getting rid of silk.This fiber can prepare building thermal insulation material, Industrial Stoves it is heat-insulated
Material, the selected superfine fibre in part can be additionally used in paper-making fibre, instead of trees fiber.Although iron tailings is in terms of construction material
Obtained certain practical application, the iron ore handled by this kind of method only account for the 12.4% of the processing of national year iron tailings,
But reach comprehensive utilization to iron tailings far away, it would be highly desirable to the new way that iron tailings utilizes is developed, additionally as construction material, its
Added value of product is low, and economic benefit is not high.
Lithium ion battery with its high-energy-density, high discharge voltage, specific capacity is big, self-discharge rate is low, memory-less effect and
The advantages that pollution-free the extensive concern by countries in the world.Ferrosilicon silicate of lithium is a kind of important anode material of lithium battery, is had
Raw material resources are abundant, no hygroscopicity, the advantages that nontoxic, environment-friendly, heat endurance is good, safe.It belongs to electric function
The category of material, there is higher technology content and added value compared to above-mentioned construction material.To sum up, due to bismuth of the present invention
The ferrous silicate lithium anode material of doping is different from the target product of the iron tailings material technology of preparing of existing report, therefore raw material
Formula, technique etc. are also entirely different.
Present invention is generally directed to the utilization present situation of China's iron tailings, it is proposed that one kind prepares bismuth by primary raw material of iron tailings
The ferrous silicate lithium anode material new method of doping.This method is suitable to industrialized production, comprehensive utilization, environment for iron tailings
Protection and the development of promotion new and high technology, which all have, to be of great significance.
The content of the invention
The invention mainly relates to a kind of synthesis for the ferrous silicate lithium anode material that bismuth doping is prepared using iron tailings as raw material
Method, the specific content of the invention are as follows:
1st, iron tailings is milled to below 400 mesh, in mass ratio iron tailings:Caustic soda=1:3~4 carry out dispensing, mixing, gained
Compound is placed in micro-wave oven heat-activated, after compound activation, compound in mass ratio:Water=1:20~30 pour into water rapidly
In, above-mentioned mixed liquor is placed in 150 ~ 180 DEG C of oil baths, 5~8h of stirring reaction, reaction is filtered after terminating, and gained filtrate is
Sodium silicate solution;SiO in molar ratio3 2-:Fe2+= 1:1, nitrous acid iron is added into sodium silicate solution, then at 100 ~ 130 DEG C of oil
1 ~ 5h of reaction is sufficiently stirred in bath;After reaction terminates, by filtering, washing, being dried to obtain sediment;Fe in molar ratio again2+:
Li+: Bi3+=1:2:0.01 ~ 0.03, lithia and bismuth oxide are mixed into sediment, is sufficiently mixed;Mixture is put
Calcined in Muffle furnace, the ferrosilicon silicate of lithium sample of bismuth doping is obtained after natural cooling.
2nd, during microwave heating activation compound, the power adjusting of micro-wave oven is 1000 ~ 3500MHz, and temperature is 800 ~ 900
DEG C, the heat time is 15 ~ 30min.
3rd, the heating medium of oil bath uses a kind of in silicone oil, methyl-silicone oil and polyethylene glycol.
4th, the method for deposit washing is washed 3 ~ 5 times using ethanol, then is washed with deionized 3 ~ 5 times.
5th, deposit drying temperature is 90 ~ 110 DEG C, and drying time is 5 ~ 10h.
6th, the temperature schedule of calcining is:Highest calcining heat is 600 ~ 800 DEG C, 2 ~ 5h of soaking time, 5 DEG C of heating rate/
min;Ar gas is protection gas, and it is 10 ~ 20m to be passed through speed3/min。
Brief description of the drawings
Fig. 1 is the XRD of the ferrous silicate lithium anode material adulterated with the bismuth prepared under the process conditions of example 1.
Embodiment
The present invention is described in detail with reference to embodiments, and the present invention is not limited by these manufacture embodiments.
Example 1
Iron tailings is milled to below 400 mesh, in mass ratio iron tailings:Caustic soda=1:4 carry out dispensing, mixing, gained compound
Micro-wave oven heat-activated is placed in, the power adjusting of micro-wave oven is 1500MHz, and temperature is 810 DEG C, heat time 30min;Mixing
Expect after activating, in mass ratio compound:Water=1:25 are poured into water rapidly, and above-mentioned mixed liquor is placed in into 160 DEG C of silicone oil oil baths
In, stirring reaction 6h, reaction is filtered after terminating, and gained filtrate is sodium silicate solution;SiO in molar ratio3 2-:Fe2+= 1:1,
Nitrous acid iron is added into sodium silicate solution, reaction 4h is sufficiently stirred in 120 DEG C of silicone oil oil baths;After reaction terminates, carry out
Filtering, then washed 5 times by ethanol washing 3 times, deionized water, and dry 8h at 100 DEG C and obtain sediment;Again in molar ratio
Fe2+:Li+: Bi3+=1:2:0.01, lithia and bismuth oxide are mixed into sediment, after being sufficiently mixed, mixture is put
Calcined in Muffle furnace, Ar gas is passed through during calcining as protection gas, it is 10m to be passed through speed3/ min, calcining heat are 600 DEG C, insulation
Time 5h, 5 DEG C/min of heating rate;The ferrosilicon silicate of lithium sample of bismuth doping is obtained after natural cooling.
Example 2
Iron tailings is milled to below 400 mesh, in mass ratio iron tailings:Caustic soda=1:3 carry out dispensing, mixing, gained compound
Micro-wave oven heat-activated is placed in, the power adjusting of micro-wave oven is 2000MHz, and temperature is 850 DEG C, heat time 20min;Mixing
Expect after activating, in mass ratio compound:Water=1:25 are poured into water rapidly, and above-mentioned mixed liquor is placed in into 160 DEG C of silicone oil oil baths
In, stirring reaction 6h, reaction is filtered after terminating, and gained filtrate is sodium silicate solution;SiO in molar ratio3 2-:Fe2+= 1:1,
Nitrous acid iron is added into sodium silicate solution, reaction 4h is sufficiently stirred in 120 DEG C of silicone oil oil baths;After reaction terminates, carry out
Filtering, then washed 5 times by ethanol washing 3 times, deionized water, and dry 8h at 100 DEG C and obtain sediment;Again in molar ratio
Fe2+:Li+: Bi3+=1:2:0.015, lithia and bismuth oxide are mixed into sediment, after being sufficiently mixed, by mixture
It is placed in Muffle furnace and calcines, Ar gas is passed through during calcining as protection gas, it is 15m to be passed through speed3/ min, calcining heat are 700 DEG C, are protected
Warm time 5h, 5 DEG C/min of heating rate;The ferrosilicon silicate of lithium sample of bismuth doping is obtained after natural cooling.
Example 3
Iron tailings is milled to below 400 mesh, in mass ratio iron tailings:Caustic soda=1:3 carry out dispensing, mixing, gained compound
Micro-wave oven heat-activated is placed in, the power adjusting of micro-wave oven is 2500MHz, and temperature is 850 DEG C, heat time 20min;Mixing
Expect after activating, in mass ratio compound:Water=1:25 are poured into water rapidly, and above-mentioned mixed liquor is placed in into 160 DEG C of methyl-silicone oil oil
In bath, stirring reaction 6h, reaction is filtered after terminating, and gained filtrate is sodium silicate solution;SiO in molar ratio3 2-:Fe2+= 1:
1, nitrous acid iron is added into sodium silicate solution, reaction 4h is sufficiently stirred in 120 DEG C of silicone oil oil baths;After reaction terminates, enter
Row filtering, then washed 5 times by ethanol washing 5 times, deionized water, and dry 7h at 100 DEG C and obtain sediment;Again by mole
Compare Fe2+:Li+: Bi3+=1:2:0.02, lithia and bismuth oxide are mixed into sediment, after being sufficiently mixed, by mixture
It is placed in Muffle furnace and calcines, Ar gas is passed through during calcining as protection gas, it is 15m to be passed through speed3/ min, calcining heat are 750 DEG C,
Soaking time 3h, 5 DEG C/min of heating rate;The ferrosilicon silicate of lithium sample of bismuth doping is obtained after natural cooling.
Example 4
Iron tailings is milled to below 400 mesh, in mass ratio iron tailings:Caustic soda=1:3 carry out dispensing, mixing, gained compound
Micro-wave oven heat-activated is placed in, the power adjusting of micro-wave oven is 2500MHz, and temperature is 900 DEG C, heat time 20min;Mixing
Expect after activating, in mass ratio compound:Water=1:25 are poured into water rapidly, and above-mentioned mixed liquor is placed in into 170 DEG C of silicone oil oil baths
In, stirring reaction 5h, reaction is filtered after terminating, and gained filtrate is sodium silicate solution;SiO in molar ratio3 2-:Fe2+= 1:1,
Nitrous acid iron is added into sodium silicate solution, reaction 3h is sufficiently stirred in 130 DEG C of silicone oil oil baths;After reaction terminates, carry out
Filtering, then washed 4 times by ethanol washing 4 times, deionized water, and dry 8h at 100 DEG C and obtain sediment;Again in molar ratio
Fe2+:Li+: Bi3+=1:2:0.025, lithia and bismuth oxide are mixed into sediment, after being sufficiently mixed, by mixture
It is placed in Muffle furnace and calcines, Ar gas is passed through during calcining as protection gas, it is 18m to be passed through speed3/ min, calcining heat are 800 DEG C, are protected
Warm time 5h, 5 DEG C/min of heating rate;The ferrosilicon silicate of lithium sample of bismuth doping is obtained after natural cooling.
Example 5
Iron tailings is milled to below 400 mesh, in mass ratio iron tailings:Caustic soda=1:3.5 carry out dispensing, mixing, gained mixing
Material is placed in micro-wave oven heat-activated, and the power adjusting of micro-wave oven is 3000MHz, and temperature is 900 DEG C, heat time 15min;It is mixed
Close after expecting activation, in mass ratio compound:Water=1:25 are poured into water rapidly, and above-mentioned mixed liquor is placed in into 180 DEG C of silicone oil oil baths
In, stirring reaction 5h, reaction is filtered after terminating, and gained filtrate is sodium silicate solution;SiO in molar ratio3 2-:Fe2+= 1:1,
Nitrous acid iron is added into sodium silicate solution, reaction 5h is sufficiently stirred in 130 DEG C of silicone oil oil baths;After reaction terminates, carry out
Filtering, then washed 3 times by ethanol washing 3 times, deionized water, and dry 6h at 110 DEG C and obtain sediment;Again in molar ratio
Fe2+:Li+: Bi3+=1:2:0.03, lithia and bismuth oxide are mixed into sediment, after being sufficiently mixed, mixture is put
Calcined in Muffle furnace, Ar gas is passed through during calcining as protection gas, it is 20m to be passed through speed3/ min, calcining heat are 800 DEG C, insulation
Time 2h, 5 DEG C/min of heating rate;The ferrosilicon silicate of lithium sample of bismuth doping is obtained after natural cooling.
Claims (6)
- A kind of 1. synthetic method for the ferrous silicate lithium anode material that bismuth doping is prepared using iron tailings as raw material, it is characterised in that: Iron tailings is milled to below 400 mesh, in mass ratio iron tailings:Caustic soda=1:3~4 carry out dispensing, mixing, gained compound It is placed in micro-wave oven heat-activated, after compound activation, compound in mass ratio:Water=1:20~30 are poured into water rapidly, will be upper State mixed liquor to be placed in 150 ~ 180 DEG C of oil baths, 5~8h of stirring reaction, reaction is filtered after terminating, and gained filtrate is that sodium metasilicate is molten Liquid;SiO in molar ratio3 2-:Fe2+= 1:1, nitrous acid iron is added into sodium silicate solution, in 100 ~ 130 DEG C of oil baths fully 1 ~ 5h of stirring reaction;After reaction terminates, by filtering, washing, being dried to obtain sediment;Fe in molar ratio again2+:Li+: Bi3+ =1:2:0.01 ~ 0.03, lithia and bismuth oxide are mixed into sediment, is sufficiently mixed;Mixture is placed in Muffle furnace Calcine, the ferrosilicon silicate of lithium sample of bismuth doping is obtained after natural cooling.
- A kind of 2. synthesis side for the ferrous silicate lithium anode material that bismuth doping is prepared using iron tailings as raw material as claimed in claim 1 Method, it is characterised in that during microwave heating activation compound, the power adjusting of micro-wave oven is 1000 ~ 3500MHz, temperature is 800 ~ 900 DEG C, the heat time is 15 ~ 30min.
- A kind of 3. synthesis side for the ferrous silicate lithium anode material that bismuth doping is prepared using iron tailings as raw material as claimed in claim 1 Method, it is characterised in that the heating medium of oil bath uses silicone oil, methyl-silicone oil and polyethylene glycol one of which.
- A kind of 4. synthesis side for the ferrous silicate lithium anode material that bismuth doping is prepared using iron tailings as raw material as claimed in claim 1 Method, it is characterised in that the method for deposit washing is washed 3 ~ 5 times using ethanol, then is washed with deionized 3 ~ 5 times.
- A kind of 5. synthesis side for the ferrous silicate lithium anode material that bismuth doping is prepared using iron tailings as raw material as claimed in claim 1 Method, it is characterised in that deposit drying temperature is 90 ~ 110 DEG C, and drying time is 5 ~ 10h.
- A kind of 6. synthesis side for the ferrous silicate lithium anode material that bismuth doping is prepared using iron tailings as raw material as claimed in claim 1 Method, it is characterised in that the temperature schedule of calcining is:Highest calcining heat is 600 ~ 800 DEG C, 2 ~ 5h of soaking time, heating rate 5 ℃/min;Ar gas is protection gas, and it is 10 ~ 20m to be passed through speed3/min。
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