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Preparation method of electronic grade high-purity manganese sulfate monohydrate

A technology of monohydrate sulfuric acid and manganese sulfate, applied in manganese sulfate and other directions, can solve the problems of low utilization rate of manganese, strong corrosion of equipment, long process, etc., and achieve the effect of simple production process, low equipment requirements and complete crystal form

Active Publication Date: 2010-04-28
GUANGDONG GUANGHUA SCI TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The manufacturing process of manganese sulfate includes: (1) high temperature roasting method, using pyrolusite as raw material. Although this method is mature, it has long process, high labor intensity, serious environmental pollution, high energy consumption, low utilization rate of manganese, waste of resources, etc. Shortcoming; (2) acid leaching method, with rhodochrosite as raw material, this method needs to consume a large amount of sulfuric acid, is strong to equipment corrosion, and filtrate needs to remove the accompanying alkaline earth metal impurity in the ore, has increased production cost; (3 ) Other methods, such as sulfur dioxide method, ferrous sulfate method, manganese monoxide method, hydrocarbon method, methods such as using biogas, rice husk, sugarcane molasses alcohol waste liquid, etc. are still in theoretical discussion and small-scale experimental exploration. Not mature yet; (4) two ore acid leaching method, this method is adopted by manganese sulfate producer gradually at present, and its advantage is to have saved high-temperature reducing roasting process, has improved operating environment, has reduced the consumption of raw material and fuel, leaching, Neutralization and iron removal and heavy metal removal are all completed in the same reaction tank at one time, and solid-liquid separation is easy
However, in actual production, especially when low-lean pyrolusite is selected as raw material, it is difficult to produce qualified manganese sulfate monohydrate simply by two-mine acid leaching
In the actual production of the existing two-mine acid leaching method, manganese ore with high manganese content is added to the low-poor pyrolusite raw material to supplement the manganese content of the raw material, otherwise qualified manganese sulfate monohydrate cannot be produced

Method used

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  • Preparation method of electronic grade high-purity manganese sulfate monohydrate

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Effect test

Embodiment 1

[0021] (1) Grind the electrolytic manganese and pass through a 300-mesh sieve to obtain manganese powder; add the manganese powder to industrial sulfuric acid, heat to 80°C under stirring conditions and continue to react for 12 hours to obtain a manganese sulfate suspension, which is analyzed by atomic absorption The content of the heavy metal salt in the manganese sulfate suspension is determined by spectrum; the mass ratio of the industrial sulfuric acid and manganese powder is 5:1;

[0022] (2) adjust pH to 3 with limestone, add barium sulfide to filter, after reaction 1h, obtain filtrate 1; The quality of described barium sulfide is 2 times of lead salt quality in heavy metal salt;

[0023] (3) add limestone to filtrate 1, adjust the pH value to 6, filter after leaving standstill 1h, obtain filtrate 2;

[0024] (4) Add sodium fluoride to the filtrate 2, filter after reacting for 24 hours, and obtain a manganese sulfate solution; the addition of the sodium fluoride is twice...

Embodiment 2

[0028] (1) Grind the electrolytic manganese and pass through a 350-mesh sieve to obtain manganese powder; add the manganese powder to industrial sulfuric acid, heat it to 90°C under stirring conditions and continue to react for 4 hours to obtain a manganese sulfate suspension, which is analyzed by atomic absorption The content of the heavy metal salt in the manganese sulfate suspension is determined by spectrum; the mass ratio of the industrial sulfuric acid and manganese powder is 4:1;

[0029] (2) adjust pH to 4 with limestone, add barium sulfide to filter, after reacting for 0.5h, obtain filtrate 1; The quality of described barium sulfide is 2 times of lead salt quality in the heavy metal salt;

[0030] (3) add limestone to filtrate 1, adjust the pH value to 6, filter after leaving standstill 1h, obtain filtrate 2;

[0031] (4) Add sodium fluoride to the filtrate 2, filter after reacting for 20 hours, and obtain a manganese sulfate solution; the addition of the sodium fluor...

Embodiment 3

[0035] (1) Grind the electrolytic manganese and pass through a 320-mesh sieve to obtain manganese powder; add the manganese powder to industrial sulfuric acid, heat it to 80°C under stirring conditions and continue to react for 10 hours to obtain a manganese sulfate suspension, which is analyzed by atomic absorption The content of the heavy metal salt in the manganese sulfate suspension is determined by spectrum; the mass ratio of the industrial sulfuric acid and manganese powder is 6:1;

[0036] (2) adjust pH to 3 with limestone, add barium sulfide to filter, after reacting for 0.8h, obtain filtrate 1; The quality of described barium sulfide is 2 times of lead salt quality in heavy metal salt;

[0037] (3) add limestone to filtrate 1, adjust the pH value to 6, filter after leaving standstill 1h, obtain filtrate 2;

[0038] (4) Add sodium fluoride to the filtrate 2, filter after reacting for 20 hours, and obtain a manganese sulfate solution; the addition of the sodium fluoride...

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Abstract

The invention discloses a method for preparing manganese sulfate monohydrate by taking electrolytic manganese and industrial sulphuric acid as raw material; the method comprises the following steps: (1) the electrolytic manganese is ground and sieved to obtain manganese powder; the manganese powder is added in the industrial sulphuric acid and is heated to 80-90 DEG C and reacts for 4-12h continuously under the stirring condition, so as to obtain manganese sulphate suspension; the heavy metallic salt content in the manganese sulphate suspension is measured by atomic absorption spectroscopy; (2) the pH of the suspension is adjusted to 3-4, barium sulphide is added and filtration is carried out, so as to obtain filtrate 1; (3) lime stone is added in the filtrate 1, after the pH value is adjusted to be 5-6 and is placed still, so as to obtain the filtrate 2; (4) sodium fluoride is added in the filtrate 2 for reacting 20-26 hours and then is filtered, so as to obtain manganese sulphate solution; (5) after the manganese sulphate solution is concentrated and recrystallized, centrifugal separation, washing, drying and crashing are carried out, thereby obtaining the manganese sulfate monohydrate; the method has simple production process, easy operation, no pollution and low equipment requirements.

Description

technical field [0001] The invention belongs to the field of chemical production, in particular to a preparation method of electronic-grade high-purity manganese sulfate monohydrate. Background technique [0002] Manganese sulfate is an important chemical product and an important raw material for chemical industry and metallurgy. It can be used in the production of medicine, papermaking, ceramics, electrolytic manganese and other manganese salts. The manufacturing process of manganese sulfate includes: (1) high temperature roasting method, using pyrolusite as raw material. Although this method is mature, it has long process, high labor intensity, serious environmental pollution, high energy consumption, low utilization rate of manganese, waste of resources, etc. Shortcoming; (2) acid leaching method, with rhodochrosite as raw material, this method needs to consume a large amount of sulfuric acid, is strong to equipment corrosion, and filtrate needs to remove the accompanying...

Claims

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Application Information

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IPC IPC(8): C01G45/10
Inventor 谭泽詹和孙张志斌周一朗
Owner GUANGDONG GUANGHUA SCI TECH
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