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Method for preparing battery-grade manganese sulfate from alkylation waste sulfuric acid

A technology for alkylating waste sulfuric acid and battery grade, applied in manganese sulfate and other directions, can solve the problems of large energy consumption, large equipment corrosion, large consumption of sulfuric acid, etc., and achieve the effect of reducing pollution, reducing production cost and high purity

Active Publication Date: 2017-05-17
QINZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the method of manganese sulfate impurity removal mainly contains: 1) normal pressure steam concentration method, by heating solution, solvent is continuously evaporated to reach concentrated crystalline manganese sulfate, but this method is carried out under normal pressure, needs to steam a large amount of water, consumes A lot of energy; 2) concentrated sulfuric acid salting out method, in the presence of sulfuric acid, the solubility of manganese sulfate significantly decreased, mainly due to SO 4 2- The same ion effect will lead to the precipitation of manganese sulfate crystals in the solid phase, but the disadvantage of this method is mainly that it consumes a large amount of sulfuric acid, and it has a great corrosion on the equipment

Method used

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  • Method for preparing battery-grade manganese sulfate from alkylation waste sulfuric acid

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Experimental program
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Effect test

Embodiment 1

[0026] 1) Dilute the alkylated waste sulfuric acid with water to a volume concentration of 20%, let it stand for stratification, take the lower layer solution and pass it through a macroporous resin column filled with two types of resin, D315 and AB-8, and the flow rate of the upper column is 1BV / h , collect the effluent, which is sulfuric acid solution; the mass ratio of D315 and AB-8 resin is 3:1.

[0027] 2) Grind the manganese ore to 100 mesh, add the sulfuric acid solution in step 1) for leaching, the solid-to-liquid ratio of manganese ore and sulfuric acid solution is 1:5g / ml, the leaching time is 180min, the heating temperature is 75°C, and the stirring rate is 300r / min , to obtain leachate;

[0028] 3) Adjust the pH value of the leachate to 5.5, let it stand and filter, and take the filtrate A for later use;

[0029] 4) Add manganese fluoride to the filtrate A, adjust the pH value to 5.8, and when the temperature is 90°C, the stirring rate is 350r / min, the fluorinatio...

Embodiment 2

[0034] 1) Dilute the alkylated waste sulfuric acid with water to a volume concentration of 30%, let it stand for stratification, take the lower layer solution and pass it through a macroporous resin column filled with two types of resin, D315 and AB-8, and the flow rate of the upper column is 2BV / h , collect the effluent, which is sulfuric acid solution; the mass ratio of D315 and AB-8 resin is 6:1.

[0035] 2) Grind the manganese ore to 200 mesh, add the sulfuric acid solution in step 1) for leaching, the solid-to-liquid ratio of manganese ore and sulfuric acid solution is 1:10g / ml, the leaching time is 240min, the heating temperature is 85°C, and the stirring rate is 400r / min , to obtain leachate;

[0036] 3) Adjust the pH value of the leachate to 6.0, let it stand and filter, and take the filtrate A for later use;

[0037] 4) Add manganese fluoride to the filtrate A, adjust the pH value to 6.2, and when the temperature is 95°C, the stirring rate is 450r / min, the fluorinati...

Embodiment 3

[0042] 1) Dilute the alkylated waste sulfuric acid with water to a volume concentration of 25%, let it stand for stratification, take the lower layer solution and pass it through a macroporous resin column filled with two types of resins, D315 and AB-8, and the flow rate of the upper column is 1.5BV / h, collect the effluent, which is sulfuric acid solution; the mass ratio of D315 and AB-8 resin is 4:1.

[0043] 2) Grind the manganese ore to 150 mesh, add the sulfuric acid solution in step 1) for leaching, the solid-to-liquid ratio of manganese ore and sulfuric acid solution is 1:8g / ml, the leaching time is 200min, the heating temperature is 80°C, and the stirring rate is 350r / min , to obtain leachate;

[0044] 3) Adjust the pH value of the leachate to 5.8, let it stand and filter, and take the filtrate A for later use;

[0045] 4) Add manganese fluoride to the filtrate A, adjust the pH value to 6.0, and when the temperature is 92°C, the stirring rate is 400r / min, the fluorina...

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Abstract

The invention discloses a method for preparing battery-grade manganese sulfate from alkylation waste sulfuric acid. The method comprises the following steps: 1) purifying the alkylation waste sulfuric acid; 2) grinding manganese ore, adding sulfuric acid for leaching, and obtaining a leachate; 3) regulating pH of the leachate, leaving the leachate to stand and filtering the leachate, and taking a filtrate A for standby application; 4) adding manganese(II) fluoride to the filtrate A, leaving the solution to stand and filtering the solution, and taking a filtrate B for standby application; 5) adding sodium sulfide to the filtrate B, leaving the solution to stand and filtering the solution, and taking a filtrate C for standby application; 6) adding sodium carbonate to the filtrate C, leaving the solution to stand and filtering the solution, taking, washing and drying filter residues to obtain manganese carbonate powder; 7) dissolving the manganese carbonate powder in sulfuric acid, adding ethanol, radiating the solution with ultraviolet light of 315-400 nm and 0.5-0.8 wm<2>, filtering the solution, and washing and drying filter residues to obtain battery-grade manganese sulfate crystals. The produced manganese sulfate is high in purity, and the production cost and environmental pollution are reduced.

Description

technical field [0001] The invention relates to a method for preparing manganese sulfate, in particular to a method for producing battery-grade manganese sulfate by using alkylated waste sulfuric acid. Background technique [0002] Alkylated gasoline is a kind of alkane mixture without olefins and aromatics, low sulfur, high octane number, low vapor pressure and branched chain, and it is also an ideal gasoline blending component. At present, the large-scale production of alkylated gasoline mainly includes sulfuric acid method and hydrofluoric acid method. The production of alkylated gasoline by sulfuric acid method uses 98% concentrated sulfuric acid as an alkylation catalyst, and about 0.1T of waste sulfuric acid is produced for every 1T of light hydrocarbonated oil produced. During the reaction process, when the acid concentration drops to about 80%-85%, the catalyst is discharged as waste acid, and the acid contains 5%-15% organic matter. The organic matter is mainly po...

Claims

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Application Information

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IPC IPC(8): C01G45/10
CPCC01G45/10C01P2006/80
Inventor 廖日权于汉玉张艳军尹艳镇杨斌焦淑菲林美芳黄海方
Owner QINZHOU UNIV