Method for producing high purity battery level iron oxalate from pickle liquor
What is Al technical title?
Al technical title is built by PatSnap Al team. It summarizes the technical point description of the patent document.
A technology of ferrous oxalate and pickling waste liquid, applied in the preparation of carboxylate, organic chemistry, etc., can solve the problems of waste of manpower and material resources, low content, environmental pollution, etc., and achieves improved reaction rate, small particle size, and sufficient reaction. Effect
Active Publication Date: 2009-06-24
HUBEI WANRUN NEW ENERGY TECH DEV
View PDF0 Cites 13 Cited by
Summary
Abstract
Description
Claims
Application Information
AI Technical Summary
This helps you quickly interpret patents by identifying the three key elements:
Problems solved by technology
Method used
Benefits of technology
Problems solved by technology
[0002] The molecular formula of ferrous oxalate is FeC 2 o 4 2H 2 O, the existing ferrous oxalate production method is to utilize ferrous sulfate heptahydrate particles produced in the titanium dioxide production process to make a solution, directly add ammonia or other reactants in the oxalic acid solution, make it react to generate ammonium oxalate solution, and then Then make the ammonium oxalate solution react with ferrous sulfate to produce ferrous oxalate. The shortcoming of the process is that the obtained ferrous oxalate particle size is relatively large, generally exceeding D 50 >15um. The particle size distribution is extremely uneven, and the particles are wrapped with other substances, so the content is low, usually FeC 2 o 4 2H 2 The total content of O is 98%-99%, generally about 98%
In addition, in the existing large-scale industrial production process, a large amount of pickling waste liquid will be produced, which must be neutralized before it can be discharged, resulting in a serious waste of manpower and material resources, and will bring serious environmental pollution
Method used
the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more
Examples
Experimental program
Comparison scheme
Effect test
Embodiment 1
[0029] Embodiment 1, the production method of ferrous oxalate:
[0030] (a), first add iron sheet or iron filings in the reaction tank, pour pickling waste liquid into, it is heated to 93 ℃, obtain ferrous salt solution, control the remaining acid amount=0.9% after its reaction, PH= 4; Ferrous salt solution includes ferrous sulfate, ferrous nitrate and ferrous oxide; the concentration of ferrous salt solution is 180mg / l
[0031] (b), the ferrous salt solution is passed through a group of Y-shaped filters to filter its metal impurities and non-metallic impurities, remove iron filings, and make it obtain a pure ferrous salt solution;
[0032] (c), add pure ferrous salt solution in the 2000L reactor with stirring, add industrial ammonia and stir the aqueous solution to make it react to generate ferrous hydroxide gel, and control the pH value=6.8 after adding ammonia, and the temperature is 72°C;
[0033] (d), in the dissolving reactor, dissolve oxidized oxalic acid to make oxal...
Embodiment 2
[0037] Embodiment 2, the production method of ferrous oxalate:
[0038] (a), first add iron flakes or iron filings in the reaction tank, pour pickling waste liquid into, it is heated to 93 ℃, obtain ferrous salt solution, control the remaining acid amount=0.8% after its reaction, PH= 5; Ferrous salt solution includes ferrous sulfate, ferrous nitrate and ferrous oxide; the concentration of ferrous salt solution is 200mg / l
[0039] (b), the ferrous salt solution is passed through a group of precision filter and magnetic filter, filter its metallic impurities and non-metallic impurities, remove iron filings, make it obtain pure ferrous salt solution;
[0040] (c), add pure ferrous salt solution in 2000L reactor with stirring, add industrial ammonia and stir the aqueous solution to make it react to generate ferrous hydroxide gel, and control the pH value=6.9 after adding ammonia, and the temperature is 78°C;
[0041] (d), in the dissolution reactor, dissolve the oxidized oxalic ...
the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more
PUM
Login to view more
Abstract
The invention relates to a method for producing high-purity battery grade iron oxalate by utilizing pickle liquor, comprising the following steps: the pickle liquor is pre-treated for lowering spent acid content, thus leading the pickle liquor to generate ferrite solution with a certain concentration; then after strict filtering and magnetic separation, the ferrite solution is transported into a reaction kettle, then industry ammonia is added and the solution is stirred for reaction to generate ferrous hydroxide gelatin; the soluble oxalic acid solution is slowly added in and stirred, and then the mixture is stirred by a conversion reaction kettle and heat preservation is carried out, thus obtaining iron oxalate slurry after reaction; iron oxalate mother solution is separated in the iron oxalate slurry, and the separated iron oxalate is washed, dried and crashed for obtaining high-purity superfine iron oxalate products. The method has the beneficial effects that: the pickle liquor in industrial production is fully utilized; a two-step liquid phase method of oxidation and conversion is adopted for leading the reaction to be more fully, so that the reaction rate is greatly improved, the grain diameter of the finished products iron oxalate is fine and uniform, D50 is less than or equal to 5mum, and the content of the iron oxalate is more than or equal to 95.5 percent; furthermore, the pickle liquor is used as raw material, and cyclic utilization and environmental protection of the industrial waste are utilized, thus changing waste into valuable and greatly lowering the production cost.
Description
technical field [0001] The invention relates to a method for producing ferrous oxalate, in particular to a method for producing high-purity battery-grade ferrous oxalate by utilizing pickling waste liquid. Background technique [0002] The molecular formula of ferrous oxalate is FeC 2 o 4 2H 2 O, the existing ferrous oxalate production method is to utilize ferrous sulfate heptahydrate particles produced in the titanium dioxide production process to make a solution, directly add ammonia or other reactants in the oxalic acid solution, make it react to generate ammonium oxalate solution, and then Then make the ammonium oxalate solution react with ferrous sulfate to produce ferrous oxalate. The shortcoming of the process is that the obtained ferrous oxalate particle size is relatively large, generally exceeding D 50 >15um. The particle size distribution is extremely uneven, and the particles are wrapped with other substances, so the content is low, usually FeC 2 o 4 2H ...
Claims
the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more
Application Information
Patent Timeline
Application Date:The date an application was filed.
Publication Date:The date a patent or application was officially published.
First Publication Date:The earliest publication date of a patent with the same application number.
Issue Date:Publication date of the patent grant document.
PCT Entry Date:The Entry date of PCT National Phase.
Estimated Expiry Date:The statutory expiry date of a patent right according to the Patent Law, and it is the longest term of protection that the patent right can achieve without the termination of the patent right due to other reasons(Term extension factor has been taken into account ).
Invalid Date:Actual expiry date is based on effective date or publication date of legal transaction data of invalid patent.
Login to view more 
Login to view more