CN104495949A - Method for preparing iron oxide red and manganese carbonate by using titanium white waste acid - Google Patents

Method for preparing iron oxide red and manganese carbonate by using titanium white waste acid Download PDF

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CN104495949A
CN104495949A CN201510002913.1A CN201510002913A CN104495949A CN 104495949 A CN104495949 A CN 104495949A CN 201510002913 A CN201510002913 A CN 201510002913A CN 104495949 A CN104495949 A CN 104495949A
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iron oxide
titanium white
waste acid
white waste
filter
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CN104495949B (en
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朱军
邓勇
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Fiedler Environmental Ecology Engineering (suzhou) Co Ltd
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Fiedler Environmental Ecology Engineering (suzhou) Co Ltd
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Abstract

The invention discloses a method for preparing iron oxide red and manganese carbonate by using titanium white waste acid. The method comprises the following steps: enabling ferrous sulfate and pyrolusite powder to react with the titanium white waste acid; adding soluble carbonate to obtain a powdery middle intermediate after reaction; and reacting once, so as to obtain the iron oxide red, manganese carbonate and sulfate. The iron oxide red product prepared by the method is high in chemical grade, and good in physical property. The method is economic, and environmentally friendly; industrial by-products are fully utilized; meanwhile, the iron oxide red, the manganese carbonate and the sulfate are prepared; three products can be obtained by production once, and therefore, the method can be applied to large-scale production; the product is stable in quality, and has the advantages of being short in reaction time, high in iron recovery rate and the like; and the titanium white waste acid, the ferrous sulfate and the low-grade pyrolusite are changed into treasures, thus, repeated utilization of resources is achieved.

Description

A kind of method utilizing titanium white waste acid to produce red iron oxide and manganous carbonate
Technical field
The present invention relates to a kind of method of comprehensive utilization of industrial waste, be specifically related to a kind of method utilizing titanium white waste acid to produce red iron oxide and manganous carbonate.
Background technology
Ferrite magnetic material is as the important branch of magneticsubstance, be widely used in the various fields such as cableless communication, control automatically, metrical instrument, aerospace, household electrical appliances and medical science, obtain great development in China in recent years, the ferrite output of China with annual more than 20% speed rapid growth.But the ferrite class that China produces is not high, and its very large reason is exactly, produce indispensable material oxidation iron oxide red (the ferric oxide Fe of ferrite magnetic material 2o 3) quality not high, and the price of external high-quality red iron oxide is very expensive.Therefore along with the sustainable development of China's ferrite industry, day by day strong to the requirement of the high-quality red iron oxide of par again.
Meanwhile, in sulfate process titanium dioxide is produced, a large amount of spent acid and ferrous sulfate can be produced, not only wasted a large amount of available resource, and caused serious environmental pollution.
Chinese patent 200710202616.7 discloses a kind of method of ferrous sulfate production red iron oxide, adopts ammoniacal liquor, iron powder and ferrous sulfate to react.Chinese patent 102649588 discloses a kind of method of titanium white by product thing ferrous sulfate production red iron oxide, is also to use ammoniacal liquor and ferrous sulfate to react.But these patents still have following weak point: 1) fail a large amount of waste acid reuse; 2) product quality can't reach external high-quality requirement, and can not stablize and scale operation.
Summary of the invention
For solving the problems of the technologies described above, the invention provides a kind of method utilizing titanium white waste acid and ferrous sulfate and low-grade pyrolusite thereof to produce red iron oxide and manganous carbonate, titanium white waste acid and by-product ferrous sulfate during thereof and low-grade pyrolusite all can be made full use of, achieve the recycling of resource, and can extensive stably manufactured high-quality product.
For achieving the above object, technical scheme of the present invention is as follows: a kind of method utilizing titanium white waste acid to produce red iron oxide and manganous carbonate, comprises the following steps:
1) by FeSO 47H 2o adds dissolving in titanium white waste acid (sulfuric acid 100-300g/l), and add pyrolusite powder (total Fe content 10%-35%) reaction, the pH value to solution is 1 ~ 1.5, filters;
2) by step 1) gained filtrate adds calcium carbonate adjust pH to 1.5 ~ 2, filters, and filter residue adds lime slurry neutralization outward transport to be disposed;
3) by step 2) filter gained filtrate (iron ion 150-250g/l) add soluble carbonate salt adjust pH to 2 ~ 2.5, reacting by heating;
4) still aging 12 hours, filter;
5) by step 4) gained residue washing, oven dry, then calcine, washing, dry, grinding, to get product red iron oxide after packaging;
6) by step 4) add calcium carbonate adjust pH to 5 ~ 6 in gained filtrate, then filter, remove the impurity such as iron, aluminium, gained filtrate adds soluble carbonate salt carbonization adjust pH to 6.5 ~ 7.5, thick product through washing, dry, get product after packaging manganous carbonate;
7) by step 6) after the remaining mother liquor removal of impurities of institute is separated, to get product vitriol through evaporation concentration, crystallization, separation, oven dry.
Wherein, step 3) add soluble carbonate salt after, in reaction process, temperature remains on 75 ~ 95 DEG C, is incubated 2 ~ 4 hours.
Wherein, described soluble carbonate salt is volatile salt, bicarbonate of ammonia, sodium carbonate, salt of wormwood.
Wherein, step 5) middle filter residue washes 1 ~ 5 time with water, and oven dry at 100 ~ 125 DEG C.
Wherein, step 5) in filter residue dry after in 600 ~ 800 DEG C of calcinings.
Wherein, step 5) in the washing water of filter residue add soluble carbonate salt adjust pH to 6.5 ~ 7.5, then thick product is filtered, washing, dry, after packaging manganous carbonate.
Wherein, step 6) in thick product wash 1 ~ 5 time with water, and to dry at 95 ~ 105 DEG C.
Wherein, step 7) in dry be at 95 ~ 105 DEG C dry.
Wherein, step 7) gained sulfate product is ammonium sulfate, sodium sulfate, potassium sulfate.
The ferrous sulfate that the present invention uses is the by product producing titanium dioxide, and containing a lot of impurity, but the present invention does not need to purify to it, directly uses.Pyrolusite powder can be low-grade pyrolusite, total Fe content 12-15%.Titanium white waste acid main component is sulfuric acid, content 10-30%.
Step 2) filter in gained filtrate and contain ferric sulphate, manganous sulfate and other various metals impurity, after adding soluble carbonate salt to pH 2 ~ 2.5, generate Powdered intermediate product.Then filtered by this intermediate product, wash, calcine, only remaining ferric oxide, obtains finished product red iron oxide.The granularity of finished product can reach 0.2 micron.
The inventive method iron recovery > 85%, the red iron oxide finished product purity > 99% obtained, granularity reaches 0.2 micron.
The inventive method manganese recovery ratio > 95%, the total manganese purity > 43.0% of the manganous carbonate finished product obtained.
Red iron oxide finished chemical grade prepared by the inventive method is high, good physical performance, can meet the requirement of market to high-quality iron oxide red; The economic environmental protection of present method, makes full use of industrial by-products, prepares red iron oxide, manganous carbonate and vitriol simultaneously, once production acquisition three kinds of products.The present invention can be used in large-scale commercial production, constant product quality; There is reaction times short, iron recovery advantages of higher, titanium white waste acid, ferrous sulfate and low-grade pyrolusite can also be used in a large number, achieve the recycling of resource.
Accompanying drawing explanation
Fig. 1 is present invention process schematic flow sheet
Embodiment
Be clearly and completely described to the technical scheme in the embodiment of the present invention below, obviously, described embodiment is only the present invention's part embodiment, instead of whole embodiments.Based on the embodiment in the present invention, those of ordinary skill in the art, not making the every other embodiment obtained under creative work prerequisite, belong to the scope of protection of the invention.
Embodiment 1
Utilize titanium white waste acid to produce a method for red iron oxide and manganous carbonate, comprise the following steps:
1) by 25kg FeSO 47H 2o adds titanium white waste acid 43L (H 2sO 4concentration 20%) in dissolve, add the pyrolusite 25.5kg of Fe content 12%, the pH value of reacting to solution is 1 ~ 1.5, filters;
2) by step 1) gained filtrate adds calcium carbonate adjust pH to 1.5 ~ 2, and filter, filter residue adds lime slurry neutralization and goes to abandon;
3) by step 2) to filter gained filtrate and add bicarbonate of ammonia adjust pH to 2 ~ 2.5, in reaction process, temperature remains on 75 ~ 95 DEG C, is incubated 2 ~ 4 hours;
4) step 3) still aging 12 hours, there is a large amount of iron content intermediate product to precipitate, filter;
5) by step 4) gained filter residue washes 1 ~ 5 time with water, at 100 ~ 125 DEG C dry, obtain Powdered intermediate product, then by this Powdered intermediate product in 600 ~ 800 DEG C of calcinings, washing and drying obtains product ferric oxide 7.8kg, and get product after grinding, packaging red iron oxide;
6) step 4) add calcium carbonate adjust pH to 5 ~ 6 in gained filtrate, to remove the impurity such as de-iron, aluminium, then filter, leave standstill, filtrate adds bicarbonate of ammonia adjust pH to 6.5 ~ 7.5 again, thick product washes 1 ~ 5 time with water, at 95 ~ 105 DEG C, dry to obtain product 6.2kg, get product after packaging manganous carbonate;
7) step 6) after the remaining mother liquor removal of impurities of institute is separated, through evaporation concentration, crystallization, separation, dries at 95 ~ 105 DEG C, obtain 7kg finished product sulfuric acid ammonium.
Step 5) in, filter residue obtains Powdered intermediate product after drying at 100 ~ 125 DEG C, instead of lenticular intermediate product of the prior art, Powdered intermediate product of the present invention directly becomes nano-scale particle after 600 ~ 800 DEG C of calcinings, only need grind to destroy its coagulated state when calcining a little, just can reach the standard-required of ferrite magnetic material, thus provide the red iron oxide raw material of high-quality par again for China's ferrite industry.
Embodiment 2
1) by 25kgFeSO 4.7H 2o adds titanium white waste acid 43L (H 25O 4concentration 20%) middle dissolving, add the pyrolusite 20kg of Fe content 15%, react the pH value 1 ~ 1.5 to solution, obtain ferric iron and bivalent manganese, filter;
2) by step 1) gained filtrate adds calcium carbonate adjust pH to 1.5 ~ 2, filters, and filter residue adds lime slurry neutralization outward transport to be disposed;
3) by step 2) to filter gained filtrate and add volatile salt adjust pH to 2 ~ 2.5, in reaction process, temperature remains on 75 ~ 95 DEG C, is incubated 2 ~ 4 hours;
4) step 3) still aging 12 hours, there is a large amount of iron content intermediate product to precipitate, filter;
5) by step 4) gained filter residue washes 1 ~ 5 time with water, dry at 100 ~ 125 DEG C, obtain Powdered intermediate product, then by this Powdered intermediate product in 600 ~ 800 DEG C of calcinings, obtain product ferric oxide 7.9kg after washing and drying, get product after grinding, packaging red iron oxide.
6) step 4) add calcium carbonate adjust pH 5 ~ 6 in gained filtrate, with except the impurity such as de-iron, aluminium, then filter, leave standstill, add volatile salt adjust pH 6.5 ~ 7.5 again, thick product washes 1 ~ 5 time with water, dries to obtain product 6kg at 95 ~ 105 DEG C, and get product after packaging manganous carbonate.
7) step 6) after the remaining mother liquor removal of impurities of institute is separated, through evaporation concentration, crystallization, separation, dries at 95 ~ 105 DEG C, obtain 6.5kg finished product sulfuric acid ammonium packaging.
Embodiment 3
1) by 20kg FeSO 47H 2o adds titanium white waste acid 35L (H 2sO 4concentration 20%) middle dissolving, add the pyrolusite 20.5kg of Fe content 12%, react the pH value 1 ~ 1.5 to solution, filter;
2) by step 1) gained filtrate adds calcium carbonate adjust pH 1.5 ~ 2, filters, and filter residue adds lime slurry neutralization outward transport to be disposed;
3) by step 2) to filter gained filtrate and add sodium carbonate adjust pH 2 ~ 2.5, in reaction process, temperature remains on 75 ~ 95 DEG C, is incubated 2 ~ 4 hours;
4) step 3) within still aging 12 hours, there is a large amount of iron content intermediate product to precipitate, filter;
5) by step 4) gained filter residue washes 1 ~ 5 time with water, dry at 100 ~ 125 DEG C, obtain Powdered intermediate product 13kg, then by this Powdered intermediate product in 600 ~ 800 DEG C of calcinings, washing and drying obtains product ferric oxide 5.8kg, and get product after grinding, packaging red iron oxide.
6) step 4) add calcium carbonate adjust pH 5 ~ 6 in gained filtrate, with except the impurity such as de-iron, aluminium, then filter, leave standstill, add sodium carbonate adjust pH 6.5 ~ 7.5 again, thick product washes 1 ~ 5 time with water, dries to obtain product 5.1kg at 95 ~ 105 DEG C, and get product after packaging manganous carbonate.
7) step 6) after the remaining mother liquor removal of impurities of institute is separated, through evaporation concentration, crystallization, separation, dries at 95 ~ 105 DEG C, obtain 6kg finished product sulfuric acid sodium packaging.
Embodiment 4
1) by 20kg FeSO 47H 2o adds titanium white waste acid 35L (H 28O 4concentration 20%) middle dissolving, add the pyrolusite 16.4kg of Fe content 15%, react the pH value 1 ~ 1.5 to solution, filter;
2) by step 1) gained filtrate adds calcium carbonate adjust pH 1.5 ~ 2, filters, and filter residue adds lime slurry neutralization outward transport to be disposed;
3) by step 2) to filter gained filtrate and add salt of wormwood adjust pH 2 ~ 2.5, in reaction process, temperature remains on 75 ~ 95 DEG C, is incubated 2 ~ 4 hours;
4) by step 3) within still aging 12 hours, there is a large amount of iron content intermediate product to precipitate, filter;
5) by step 4) gained filter residue washes 1 ~ 5 time with water, dry at 100 ~ 125 DEG C, obtain Powdered intermediate product 13kg, then by this Powdered intermediate product in 600 ~ 800 DEG C of calcinings, obtain product ferric oxide 5.8kg after washing and drying, get product after grinding, packaging red iron oxide.
6) by step 4) add calcium carbonate adjust pH 5 ~ 6 in gained filtrate, with except the impurity such as de-iron, aluminium, then filter, leave standstill, add salt of wormwood adjust pH 6.5 ~ 7.5 again, thick product washes 1 ~ 5 time with water, dries to obtain product 5kg at 95 ~ 105 DEG C, and get product after packaging manganous carbonate.
7) by step 6) after the remaining mother liquor removal of impurities of institute is separated, through evaporation concentration, crystallization, separation, dries at 95 ~ 105 DEG C, obtain 7.2kg finished product sulfuric acid potassium packaging.
Product quality is through inspection, and properties is in table 1.
Red iron oxide finished chemical grade prepared by the inventive method is high, good physical performance, can meet the requirement of market to high-quality iron oxide red; The economic environmental protection of present method, makes full use of industrial by-products, prepares red iron oxide, manganous carbonate and vitriol simultaneously, once production acquisition three kinds of products.The present invention can be used in large-scale commercial production, constant product quality; There is reaction times short, iron recovery advantages of higher, titanium white waste acid, ferrous sulfate and low-grade pyrolusite can also be used in a large number, achieve the recycling of resource.
To the above-mentioned explanation of the disclosed embodiments, professional and technical personnel in the field are realized or uses the present invention.To be apparent for those skilled in the art to the multiple amendment of these embodiments, General Principle as defined herein can without departing from the spirit or scope of the present invention, realize in other embodiments.Therefore, the present invention can not be restricted to these embodiments shown in this article, but will meet the widest scope consistent with principle disclosed herein and features of novelty.

Claims (8)

1. utilize titanium white waste acid to produce a method for red iron oxide and manganous carbonate, it is characterized in that, comprise the following steps:
1) by FeSO 47H 2o adds in titanium white waste acid and dissolves, and add pyrolusite powder reaction, the pH value to solution is 1 ~ 1.5, filters;
2) by step 1) filter gained filtrate and add calcium carbonate adjust pH to 1.5 ~ 2, filter;
3) by step 2) filter gained filtrate and add soluble carbonate salt adjust pH to 2 ~ 2.5, reacting by heating;
4) still aging 12 hours, filter;
5) by step 4) filter gained residue washing, oven dry, then calcine, get product after washing, oven dry, grinding, packaging red iron oxide;
6) by step 4) filter in gained filtrate and add calcium carbonate adjust pH to 5 ~ 6, then filter, gained filtrate adds soluble carbonate salt carbonization adjust pH to 6.5 ~ 7.5, thick product through washing, dry, get product after packaging manganous carbonate;
7) by step 6) after the remaining mother liquor removal of impurities of institute is separated, evaporation concentration, crystallization, separation, oven dry get product vitriol.
2. the method utilizing titanium white waste acid to produce red iron oxide and manganous carbonate according to claim 1, is characterized in that, described step 3) add soluble carbonate salt after, in reaction process, temperature remains on 75 ~ 95 DEG C, is incubated 2 ~ 4 hours.
3. the method utilizing titanium white waste acid to produce red iron oxide and manganous carbonate according to claim 1, is characterized in that, described step 3) and step 6) in soluble carbonate salt be volatile salt, bicarbonate of ammonia, sodium carbonate, salt of wormwood.
4. the method utilizing titanium white waste acid to produce red iron oxide and manganous carbonate according to claim 1, is characterized in that, described step 5) middle filter residue washes 1 ~ 5 time with water, and oven dry at 100 ~ 125 DEG C.
5. the method utilizing titanium white waste acid to produce red iron oxide and manganous carbonate according to claim 1, is characterized in that, described step 5) in filter residue dry after in 600 ~ 800 DEG C of calcinings.
6. the method utilizing titanium white waste acid to produce red iron oxide and manganous carbonate according to claim 1, it is characterized in that, described step 5) in the washing water of filter residue add soluble carbonate salt adjust pH 6.5 ~ 7.5, then thick product is filtered, washing, dry, after packaging manganous carbonate.
7. the method utilizing titanium white waste acid to produce red iron oxide and manganous carbonate according to claim 1, is characterized in that, described step 6) in thick product wash 1 ~ 5 time with water, and to dry at 95 ~ 105 DEG C.
8. the method utilizing titanium white waste acid to produce red iron oxide and manganous carbonate according to claim 1, is characterized in that, described step 7) in dry refer at 95 ~ 105 DEG C dry.
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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109354071A (en) * 2018-11-21 2019-02-19 安徽工业大学 A method of LITHIUM BATTERY manganese sulfate is produced using manganese tailing and Titanium white waste sulfuric acid
CN109399723A (en) * 2018-12-03 2019-03-01 安徽工业大学 A method of electrolytic manganese dioxide is produced using manganese tailing and Titanium white waste sulfuric acid
CN110157911A (en) * 2019-04-03 2019-08-23 张响 A kind of technique of comprehensive reutilization electrolytic manganese residues and manganese tailing
CN110229961A (en) * 2019-04-03 2019-09-13 张响 A kind of technique leaching electrolytic manganese residues and manganese tailing using titanium white waste acid

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101920998A (en) * 2010-08-05 2010-12-22 蓝星化工新材料股份有限公司广西分公司 Method for preparing manganese sulfate from waste byproducts obtained in the production of titanium white and low-grade pyrolusite

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101920998A (en) * 2010-08-05 2010-12-22 蓝星化工新材料股份有限公司广西分公司 Method for preparing manganese sulfate from waste byproducts obtained in the production of titanium white and low-grade pyrolusite

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109354071A (en) * 2018-11-21 2019-02-19 安徽工业大学 A method of LITHIUM BATTERY manganese sulfate is produced using manganese tailing and Titanium white waste sulfuric acid
CN109354071B (en) * 2018-11-21 2020-11-24 安徽工业大学 Method for producing battery-grade manganese sulfate by using manganese tailings and waste sulfuric acid of titanium white
CN109399723A (en) * 2018-12-03 2019-03-01 安徽工业大学 A method of electrolytic manganese dioxide is produced using manganese tailing and Titanium white waste sulfuric acid
CN109399723B (en) * 2018-12-03 2020-11-24 安徽工业大学 Method for producing electrolytic manganese dioxide by using manganese tailings and titanium dioxide waste sulfuric acid
CN110157911A (en) * 2019-04-03 2019-08-23 张响 A kind of technique of comprehensive reutilization electrolytic manganese residues and manganese tailing
CN110229961A (en) * 2019-04-03 2019-09-13 张响 A kind of technique leaching electrolytic manganese residues and manganese tailing using titanium white waste acid

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