CN105280908A - Method for preparing lithium titanate by utilizing sulfuric-acid-method titanium dioxide intermediate product metatitanic acid - Google Patents
Method for preparing lithium titanate by utilizing sulfuric-acid-method titanium dioxide intermediate product metatitanic acid Download PDFInfo
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- CN105280908A CN105280908A CN201510867163.4A CN201510867163A CN105280908A CN 105280908 A CN105280908 A CN 105280908A CN 201510867163 A CN201510867163 A CN 201510867163A CN 105280908 A CN105280908 A CN 105280908A
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- metatitanic acid
- titanium dioxide
- lithium titanate
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- acid
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/485—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of mixed oxides or hydroxides for inserting or intercalating light metals, e.g. LiTi2O4 or LiTi2OxFy
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G23/00—Compounds of titanium
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G23/00—Compounds of titanium
- C01G23/04—Oxides; Hydroxides
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/139—Processes of manufacture
- H01M4/1391—Processes of manufacture of electrodes based on mixed oxides or hydroxides, or on mixtures of oxides or hydroxides, e.g. LiCoOx
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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
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention relates to a method for preparing lithium titanate by utilizing sulfuric-acid-method titanium dioxide intermediate product metatitanic acid. The method comprises the following steps: preprocessing the intermediate product metatitanic acid in the production process of the sulfuric-acid-method titanium dioxide, removing impurities contained in the intermediate product metatitanic acid, dehydrating, drying, adding lithium salt, moisturizing, curing, heating, and finally forming lithium titanate uniform in particle size. The method is simple in process, low in price of raw materials and easy for controlling the production process, the prepared lithium titanate is stable in quality and uniform in appearance, the preparation method can reach the quality requirement, is easy to control and likely to form mass production, and the weaknesses of the traditional production method are overcome.
Description
Technical field
What the present invention relates to the middle product metatitanic acid of a kind of sulfuric acid method titanium pigment production utilizes field, particularly a kind of method utilizing the middle product metatitanic acid of sulfate process titanium dioxide to prepare lithium titanate.
Background technology
World today's energy crisis becomes increasingly conspicuous, and energy security is the grand strategy of various countries, for breaking away from energy crisis countries in the world all at the positive development of new energy.Lithium battery more and more demonstrates its advantage as a kind of novel energy, and the technology of preparing as the lithium titanate of negative pole material of lithium battery directly determines quality and the cost of lithium battery.The lithium titanate of spinel structure is because have useful structural stability and security performance is considered to a kind of well high power lithium ion cell and asymmetric hybrid battery negative material.Prepare lithium titanate precursor at present and mostly use chemical pure or analytically pure nanoscale titanium salt, titanium tetrachloride, organic titanium etc.These raw materials or value costliness, or there is certain security risk, especially environmental risk.The preparation method of lithium titanate mainly contains high temperature solid-state and sol-gel two kinds of methods.High temperature solid-state method has simple, is easy to suitability for industrialized production, but its reaction time is long, and product is uneven, and Grain growth is inconsistent causes the inconsistent and agglomeration of granular size etc.Lithium titanate prepared by sol-gel process has possessed the features such as particle is homogeneous, excellent performance, but controlled condition is harsh, complex technical process, can only complete the preparation of a small amount of sample in the lab, be difficult to realize industrialization, the raw material of employing is generally organic titanium, toxicity is large, cost is high, and operability is poor, is secondly that the whole sol-gel process time is long, a large amount of micropore is there is in gel, much gas and harmful substance will be overflowed in dry run, and produce contraction, have impact on application performance.How to adopt a kind of method of lithium titanate good quality that is cheap, that be easy to get and prepare unresolved so far.
Summary of the invention
The object of this invention is to provide a kind of method utilizing the middle product metatitanic acid of sulfate process titanium dioxide to prepare lithium titanate; technical process is simple, raw materials used cheap; production process is easy to control; gained lithium titanate steady quality, pattern are homogeneous; preparation method can reach quality requirement; and be easy to control and form large-scale production, the customer service deficiency of existing processing.
A kind of method utilizing the middle product metatitanic acid of sulfate process titanium dioxide to prepare lithium titanate of the present invention, product metatitanic acid in the middle of sulfate process titanium dioxide production process is carried out preliminary treatment, remove the impurity that middle product metatitanic acid is mingled with, carry out dewatered drying, then add lithium salts and carry out leaching pool, solidification, finally heat up, make the granule-morphology of the lithium titanate of formation even.
The impurity that middle product metatitanic acid is mingled with is metal impurities and the sulfate radicals such as iron, manganese, nickel, cobalt, magnesium.
The described product metatitanic acid in the middle of sulfate process titanium dioxide that utilizes prepares the method for lithium titanate, it is characterized in that, comprises the steps:
1) after product metatitanic acid in the middle of sulfate process titanium dioxide production process being carried out making beating washing, after further making beating evenly, add alkaline solution, make the mass ratio of ammonium and titanium be 1:2-3, after fully stirring, adjustment PH is 7-8, after squeeze and filter, washing is less than less than 0.05% to the sulfate radical mass content in filter cake, and wherein, sulfate radical measures with elemental sulfur;
2) dried by the metatitanic acid washed, temperature controls in the scope of 120-150 DEG C, dries 2-4 hour;
3) by the material grinding after oven dry, the metatitanic acid after grinding is for subsequent use;
4) dissolved by lithium hydroxide, concentration is 100-160g/L, is joined by lithium hydroxide solution in metatitanic acid dry powder and mixes;
5) by above-mentioned drying materials, cool, grind, obtain lithium titanate product.
Alkaline solution is one or more in ammonium carbonate, carbonic hydroammonium or ammoniacal liquor, the aqueous solution of ammonium carbonate, carbonic hydroammonium, ammoniacal liquor containing ammonium mass content be 6 ?10%.
The operating procedure that the middle product metatitanic acid of sulfate process titanium dioxide production process carries out making beating washing is: keep the slurry concentration of metatitanic acid at 200-300g/L, wherein, metatitanic acid measures with titanium dioxide, deionized water is adopted to wash, the temperature of deionized water remains on 40-60 DEG C, and the iron content detecting metatitanic acid filter cake is less than 10ppm and can stops washing.
During further making beating, keep the stock quality concentration of metatitanic acid at 200-300g/L, wherein, metatitanic acid measures with titanium dioxide.
Lithium salts adopts Li
2cO
3and LiOHH
2o.Preferred LiOHH
2o.
The dosage of lithium salts at the mass ratio of LI:Ti be 0.85-0.95:1 basis on excessive 8-10%.Wherein, metatitanic acid measures with TiO2, and metatitanic acid measures with titanium dioxide.The loss caused because lithium salts volatilizees to make up.
In step (5), drying materials heats up according to following heating curve:
Control room temperature to 400 DEG C of constant temperature 2 hours, by 400-500 DEG C of constant temperature 30min, 500-600 DEG C of constant temperature 30-50min, 600-700 DEG C of constant temperature 30-50min, 700-800 DEG C of constant temperature 60-80min, 800-900 DEG C of constant temperature 60-90min, after 900-1000 DEG C of constant temperature 300-500min, cut off the electricity supply, be cooled to room temperature and take out.
The present invention is according to principle:
5TiO
2+2Li
2CO
3——Li4Ti
5O
12+2CO
2
5TiO
2+4LiOH——Li
4Ti
5O1
2+2H
2O。
The present invention, by product metatitanic acid in the middle of sulfate process titanium dioxide production process is carried out preliminary treatment, after removing the impurity and sulfate radical that middle product metatitanic acid is mingled with, carries out dewatered drying.Then add lithium salts and carry out leaching pool, solidification.By progressively heating up, make the granule-morphology of the lithium titanate of formation even.
Compared with prior art, the present invention has following beneficial effect:
The present invention utilizes product metatitanic acid in the middle of sulfate process titanium dioxide to prepare the method for lithium titanate; technical process is simple, raw materials used cheap; production process is easy to control; gained lithium titanate steady quality, pattern are homogeneous; preparation method can reach quality requirement; and be easy to control and form large-scale production, the customer service deficiency of existing processing.
Embodiment
Below in conjunction with embodiment, the present invention is described further.
Embodiment 1
Product metatitanic acid in the middle of sulfate process titanium dioxide production process is carried out making beating washing, specifically keep the slurry concentration of metatitanic acid in 200g/L (with titanium dioxide metering), deionized water is adopted to wash, the temperature of deionized water remains on 40 DEG C, and the iron content detecting metatitanic acid filter cake is less than 10ppm (with fe metering) and can stops washing.
Metatitanic acid filter cake good for above-mentioned washing is pulled an oar further, the slurry concentration of concrete maintenance metatitanic acid is in 200g/L (with titanium dioxide metering), after making beating evenly, add the aqueous solution of ammoniacal liquor, its concentration requirement is 6% (measuring with the quality of ammoniacal liquor), count after fully stirring after the aqueous solution of ammoniacal liquor, use sheet frame squeeze and filter, adopt deionized water to carry out washing to the sulfate radical content in filter cake and be less than less than 0.05% (with elemental sulfur metering).Stop washing.The metatitanic acid washed is put into stainless pallet, puts into stainless baking oven and dry, temperature controls, at 120 DEG C, to dry 3 hours.Adopt gas grinding to grind the material after drying, the metatitanic acid after grinding is for subsequent use.
LiOHH is taken according to the ratio of LI:Ti=0.85:1
2o and the metatitanic acid after grinding are (with TiO
2metering).The lithium hydroxide measured is dissolved, concentration is 100g/L (with lithium hydroxide metering), is joined by lithium hydroxide solution in the metatitanic acid dry powder measured, adopts flour dough mixing machine or other powder siccative mixing apparatus, equipment material is stainless steel, product of preventing and remedying pollution.Stainless steel pallet is put into after fully mixing.
Material in above-mentioned stainless steel pallet is put into Muffle furnace, dry according to following heating curve: Muffle furnace controls room temperature to 400 DEG C of constant temperature 2 hours, by 400-500 DEG C of constant temperature 30min, 500-600 DEG C of constant temperature 30min, 600-700 DEG C of constant temperature 30min, 700-800 DEG C of constant temperature 60min, 800-900 DEG C of constant temperature 60min, after 900-1000 DEG C of constant temperature 300min, cut off the electricity supply, be cooled to room temperature and take out.The material of cooling is put into grinder grind, obtain lithium titanate product.
Embodiment 2
Product metatitanic acid in the middle of sulfate process titanium dioxide production process is carried out making beating washing, specific requirement keeps the slurry concentration of metatitanic acid in 240g/L (with titanium dioxide metering), deionized water is adopted to wash, the temperature of deionized water remains on 45 DEG C, and the iron content detecting metatitanic acid filter cake is less than 10ppm (with fe metering) and can stops washing.
Metatitanic acid filter cake good for above-mentioned washing is pulled an oar further, specific requirement keeps the slurry concentration of metatitanic acid in 240g/L (with titanium dioxide metering), after making beating evenly, add the aqueous solution of ammoniacal liquor, its concentration requirement is 7% (measuring with the quality of ammoniacal liquor), after fully stirring after counting the aqueous solution of ammoniacal liquor, use sheet frame squeeze and filter, adopt deionized water to carry out washing to the sulfate radical content in filter cake and be less than less than 0.05% (with elemental sulfur metering).Stop washing.The metatitanic acid washed is put into stainless pallet, puts into stainless baking oven and dry, temperature controls, at 130 DEG C, to dry 3 hours.Adopt gas grinding to grind the material after drying, the metatitanic acid after grinding is for subsequent use.
LiOHH is taken according to the ratio of LI:Ti=0.90:1
2o and the rear metatitanic acid for subsequent use of grinding are (with TiO
2metering).The lithium hydroxide measured is dissolved, concentration is 120g/L (with lithium hydroxide metering), is joined by lithium hydroxide solution in the metatitanic acid dry powder measured, adopts flour dough mixing machine or other powder siccative mixing apparatus, equipment material is stainless steel, product of preventing and remedying pollution.Stainless steel pallet is put into after fully mixing.
Material in above-mentioned stainless steel pallet is put into Muffle furnace, dry according to following heating curve: Muffle furnace controls room temperature to 400 DEG C of constant temperature 2 hours, by 400-500 DEG C of constant temperature 40min, 500-600 DEG C of constant temperature 40min, 600-700 DEG C of constant temperature 30min, 700-800 DEG C of constant temperature 70min, 800-900 DEG C of constant temperature 70min, after 900-1000 DEG C of constant temperature 400min, cut off the electricity supply, be cooled to room temperature and take out.The material of cooling is put into grinder grind, obtain lithium titanate product.
Embodiment 3
Product metatitanic acid in the middle of sulfate process titanium dioxide production process is carried out making beating washing, specific requirement keeps the slurry concentration of metatitanic acid in 260g/L (with titanium dioxide metering), deionized water is adopted to wash, the temperature of deionized water remains on 50 DEG C, and the iron content detecting metatitanic acid filter cake is less than 10ppm (with fe metering) and can stops washing.
Metatitanic acid filter cake good for above-mentioned washing is pulled an oar further, specific requirement keeps the slurry concentration of metatitanic acid in 260g/L (with titanium dioxide metering), after making beating evenly, add the aqueous solution of ammoniacal liquor, its concentration requirement is 8% (measuring with the quality of ammoniacal liquor), after fully stirring after counting the aqueous solution of ammoniacal liquor, use sheet frame squeeze and filter, adopt deionized water to carry out washing to the sulfate radical content in filter cake and be less than less than 0.05% (with elemental sulfur metering).Stop washing.The metatitanic acid washed is put into stainless pallet, puts into stainless baking oven and dry, temperature controls, at 140 DEG C, to dry 3 hours.Adopt electric coffee grinder to grind the material after drying, the metatitanic acid after grinding is for subsequent use.
LiOHH is taken according to the ratio of LI:Ti=0.95:1
2o and the rear metatitanic acid for subsequent use of grinding are (with TiO
2metering).The lithium hydroxide measured is dissolved, concentration is 140g/L (with lithium hydroxide metering), is joined by lithium hydroxide solution in the metatitanic acid dry powder measured, adopts flour dough mixing machine or other powder siccative mixing apparatus, equipment material is stainless steel, product of preventing and remedying pollution.Stainless steel pallet is put into after fully mixing.
Material in above-mentioned stainless steel pallet is put into Muffle furnace, dry according to following heating curve: Muffle furnace controls room temperature to 400 DEG C of constant temperature 2 hours, by 400-500 DEG C of constant temperature 50min, 500-600 DEG C of constant temperature 50min, 600-700 DEG C of constant temperature 30min, 700-800 DEG C of constant temperature 80min, 800-900 DEG C of constant temperature 80min, after 900-1000 DEG C of constant temperature 500min, cut off the electricity supply, be cooled to room temperature and take out.The material of cooling is put into grinder grind, obtain lithium titanate product.
Embodiment 4
Product metatitanic acid in the middle of sulfate process titanium dioxide production process is carried out making beating washing, specific requirement keeps the slurry concentration of metatitanic acid in 300g/L (with titanium dioxide metering), deionized water is adopted to wash, the temperature of deionized water remains on 60 DEG C, and the iron content detecting metatitanic acid filter cake is less than 10ppm (with fe metering) and can stops washing.
Metatitanic acid filter cake good for above-mentioned washing is pulled an oar further, specific requirement keeps the slurry concentration of metatitanic acid in 300g/L (with titanium dioxide metering), after making beating evenly, add the aqueous solution of ammoniacal liquor, its concentration requirement is 10% (measuring with the quality of ammoniacal liquor), after fully stirring after counting the aqueous solution of ammoniacal liquor, use sheet frame squeeze and filter, adopt deionized water to carry out washing to the sulfate radical content in filter cake and be less than less than 0.05% (with elemental sulfur metering).Stop washing.The metatitanic acid washed is put into stainless pallet, puts into stainless baking oven and dry, temperature controls, at 150 DEG C, to dry 3 hours.Adopt electric coffee grinder to grind the material after drying, the metatitanic acid after grinding is for subsequent use.
LiOHH is taken according to the ratio of LI:Ti=0.95:1
2o and the rear metatitanic acid for subsequent use of grinding are (with TiO
2metering).The lithium hydroxide measured is dissolved, concentration is 160g/L (with lithium hydroxide metering), is joined by lithium hydroxide solution in the metatitanic acid dry powder measured, adopts flour dough mixing machine or other powder siccative mixing apparatus, equipment material is stainless steel, product of preventing and remedying pollution.Stainless steel pallet is put into after fully mixing.
Material in above-mentioned stainless steel pallet is put into Muffle furnace, dry according to following heating curve: Muffle furnace controls room temperature to 400 DEG C of constant temperature 2 hours, by 400-500 DEG C of constant temperature 50min, 500-600 DEG C of constant temperature 50min, 600-700 DEG C of constant temperature 50min, 700-800 DEG C of constant temperature 80min, 800-900 DEG C of constant temperature 80min, after 900-1000 DEG C of constant temperature 500min, cut off the electricity supply, be cooled to room temperature and take out.The material of cooling is put into grinder grind, obtain lithium titanate product.
Claims (9)
1. one kind utilizes product metatitanic acid in the middle of sulfate process titanium dioxide to prepare the method for lithium titanate, it is characterized in that, product metatitanic acid in the middle of sulfate process titanium dioxide production process is carried out preliminary treatment, remove the impurity that middle product metatitanic acid is mingled with, carry out dewatered drying, then add lithium salts and carry out leaching pool, solidification, finally heat up, make the granule-morphology of the lithium titanate of formation even.
2. the method utilizing the middle product metatitanic acid of sulfate process titanium dioxide to prepare lithium titanate according to claim 1, it is characterized in that, the impurity that middle product metatitanic acid is mingled with is metal impurities and the sulfate radicals such as iron, manganese, nickel, cobalt, magnesium.
3. the method utilizing the middle product metatitanic acid of sulfate process titanium dioxide to prepare lithium titanate according to claim 1, is characterized in that, comprise the steps:
1) after product metatitanic acid in the middle of sulfate process titanium dioxide production process being carried out making beating washing, after further making beating evenly, add alkaline solution, make the mass ratio of ammonium and titanium be 1:2-3, after fully stirring, adjustment PH is 7-8, after squeeze and filter, washing is less than less than 0.05% to the sulfate radical mass content in filter cake, and wherein, sulfate radical measures with elemental sulfur;
2) dried by the metatitanic acid washed, temperature controls in the scope of 120-150 DEG C, dries 2-4 hour;
3) by the material grinding after oven dry, the metatitanic acid after grinding is for subsequent use;
4) dissolved by lithium hydroxide, concentration is 100-160g/L, is joined by lithium hydroxide solution in metatitanic acid dry powder and mixes;
5) by above-mentioned drying materials, cool, grind, obtain lithium titanate product.
4. the method utilizing the middle product metatitanic acid of sulfate process titanium dioxide to prepare lithium titanate according to claim 1, it is characterized in that, the operating procedure that the middle product metatitanic acid of sulfate process titanium dioxide production process carries out making beating washing is: keep the slurry concentration of metatitanic acid at 200-300g/L, wherein, metatitanic acid measures with titanium dioxide, adopt deionized water to wash, the temperature of deionized water remains on 40-60 DEG C, and the iron content detecting metatitanic acid filter cake is less than 10ppm and can stops washing.
5. the method utilizing the middle product metatitanic acid of sulfate process titanium dioxide to prepare lithium titanate according to claim 1, it is characterized in that, when pulling an oar further, keep the stock quality concentration of metatitanic acid at 200-300g/L, wherein, metatitanic acid measures with titanium dioxide.
6. the method utilizing the middle product metatitanic acid of sulfate process titanium dioxide to prepare lithium titanate according to claim 1, it is characterized in that, alkaline solution is one or more in ammonium carbonate, carbonic hydroammonium or ammoniacal liquor, the aqueous solution of ammonium carbonate, carbonic hydroammonium, ammoniacal liquor be 6-10% containing ammonium mass content.
7. the method utilizing the middle product metatitanic acid of sulfate process titanium dioxide to prepare lithium titanate according to claim 1, it is characterized in that, lithium salts adopts Li
2cO
3and LiOHH
2o.
8. according to claim 1ly utilize product metatitanic acid in the middle of sulfate process titanium dioxide to prepare the method for lithium titanate, it is characterized in that, the dosage of lithium salts at the mass ratio of LI:Ti be 0.85-0.95:1 basis on excessive 8-10%.
9. the method utilizing the middle product metatitanic acid of sulfate process titanium dioxide to prepare lithium titanate according to claim 1, it is characterized in that, in step (5), drying materials heats up according to following heating curve:
Control room temperature to 400 DEG C of constant temperature 2 hours, by 400-500 DEG C of constant temperature 30min, 500-600 DEG C of constant temperature 30-50min, 600-700 DEG C of constant temperature 30-50min, 700-800 DEG C of constant temperature 60-80min, 800-900 DEG C of constant temperature 60-90min, after 900-1000 DEG C of constant temperature 300-500min, cut off the electricity supply, be cooled to room temperature and take out.
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| CN110937586B (en) * | 2018-09-25 | 2023-09-22 | 杭州长凯能源科技有限公司 | Circular economic process for preparing material |
| CN110028099A (en) * | 2019-05-24 | 2019-07-19 | 江苏特丰新材料科技有限公司 | A kind of preparation method of powder-type high capacity titanium based lithium-ion exchanger |
| CN110102353A (en) * | 2019-05-24 | 2019-08-09 | 江苏特丰新材料科技有限公司 | A kind of preparation method of the highly selective titanium based lithium-ion exchanger of powder-type high capacity |
| CN110127756A (en) * | 2019-05-24 | 2019-08-16 | 江苏特丰新材料科技有限公司 | A kind of preparation method of titanium based lithium-ion exchanger, its presoma |
| CN110215935A (en) * | 2019-05-24 | 2019-09-10 | 江苏特丰新材料科技有限公司 | A kind of preparation method of powder-type high capacity titanium based lithium-ion exchanger |
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Denomination of invention: Method for preparing lithium titanate using metatitanic acid as intermediate in sulfuric acid method for titanium dioxide production Effective date of registration: 20230803 Granted publication date: 20181019 Pledgee: China Construction Bank Corporation Zibo Boshan sub branch Pledgor: SHANDONG DOGUIDE GROUP Co.,Ltd. Registration number: Y2023980050752 |