CN109205638A - A method of analcime is prepared using electrolytic manganese residues - Google Patents
A method of analcime is prepared using electrolytic manganese residues Download PDFInfo
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- CN109205638A CN109205638A CN201811318932.5A CN201811318932A CN109205638A CN 109205638 A CN109205638 A CN 109205638A CN 201811318932 A CN201811318932 A CN 201811318932A CN 109205638 A CN109205638 A CN 109205638A
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- C01B39/02—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof; Direct preparation thereof; Preparation thereof starting from a reaction mixture containing a crystalline zeolite of another type, or from preformed reactants; After-treatment thereof
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Abstract
The invention discloses a kind of methods for preparing analcime using electrolytic manganese residues, this method is by electrolytic manganese residues powder by aoxidizing and being complexed efficient removal iron, after realizing that the recycling of iron, removing of iron and manganese slag pass through calcining and activating, it is reacted with aluminum oxide, sodium hydroxide and water, crystallization obtains high pure phase analcime.This method step is simple, mild condition, at low cost, and while preparing high pure phase analcime using electrolytic manganese residues, can also recycle iron, be truly realized the resource utilization of electrolytic manganese residues, solve electrolytic manganese residues bring environmental issue.
Description
Technical field
The present invention relates to a kind of electrolytic manganese residues processing method, in particular to a kind of electrolytic manganese residues recycling recycles production high
Added value zeolite, while the method for efficiently separating recycling iron, belong to reclamation of solid wastes technical field.
Background technique
Electrolytic manganese residues refer to the acid slag that sulfuric acid solution production of manganese dioxide by electrolysis is added in manganese carbonate miberal powder,
Discharge amount is huge, stacks the dedicated place for being also required to requisition large area, and waste particle is small, long-term stacking can make therein
Harmful substance infiltrates underground water or contaminated soil, pollutes to water and soil and ecological environment.Therefore, fast with electrolytic manganese industry
Speed development, harmless treatment and resource utilization to manganese slag have become environmental protection and environmental project industry urgent problem to be solved.
The related report of country's electrolytic manganese residues processing, which has focused largely on, at present prepares building materials, solidification, stabilisation, preparation pottery
Porcelain, active composite material, porous material, modified micro mist etc., these preparation methods exist in varying degrees processing cost it is high,
Complex process, energy consumption is high and it is complicated for operation the disadvantages of, and be not related to pre-processing except iron, the methods of grading extraction has recycling
Not equal enough the series of problems of purpose product purity afterwards.
Zeolite is a kind of inorganic skeleton type alumino-silicate crystalline microporous material, former as important mineral resources and chemical industry
Material has unique internal structure, because of its unique ion exchangeable, shape-selective adsorptivity, composition and property mutability tonality, numerous
The high activity and selectivity of small molecule catalysis reaction, are widely used in many fields such as industrial process and hitech materials, special
It not can use the absorption and improvement etc. of its catalysis, ion exchange and ion adsorbing for polluted water body.
Chinese patent (CN108203097A) discloses a kind of method of electrolytic manganese residues high-efficiency resource recycling, and this method is
The activation of electrolytic manganese residues, separation, hydrated calcium silicate and zeolitic material technology of preparing are organically combined, it is high that added value is prepared
The qualified products of hydrated calcium silicate and zeolitic material realize the comprehensive utilization of useful component in electrolytic manganese residues.But this method
For the useful component for making full use of electrolytic manganese residues, it is activated using nitric acid solution；Then using sodium hydroxide as alkali
Property medium alkali fusion-hydrothermal synthesis method carried out to electrolytic manganese residues prepare zeolite, soda acid consumption is big at high cost, corrosion-resistant to equipment
Performance requirement is high.
Summary of the invention
In view of the defects existing in the prior art, simple, mild condition that the purpose of the invention is to provide a kind of steps, at
This low method for preparing high pure phase analcime using electrolytic manganese residues, this method can also recycle iron, be truly realized electrolytic manganese
The resource utilization of slag solves electrolytic manganese residues bring environmental issue.
In order to achieve the above technical purposes, the present invention provides a kind of methods for preparing analcime using electrolytic manganese residues, should
Method the following steps are included:
1) electrolytic manganese residues powder is mixed with water after sizing mixing, oxidant progress oxidation reaction is added in the slurry to be made in slurry
Low price iron be converted to ferric iron, add oxalic acid solution complexing slurry in ferric iron, be separated by solid-liquid separation, solid phase is removing of iron and manganese
Slag；
2) removing of iron and manganese slag and sodium carbonate mixed calcining are activated, obtains refined manganese dioxide slag；
3) after refined manganese dioxide slag being mixed with aluminum oxide, sodium hydroxide and water, ageing, crystallization to get.
The solid-to-liquid ratio of preferred scheme, electrolytic manganese residues powder and water is 1g/1.5mL~1g/1.8mL.
Preferred scheme, the condition of the oxidation reaction are as follows: temperature is 85~95 DEG C, and the time is 1~3h, using 20~
The hydrogen peroxide of 35wt% is 1mL/8g~1mL/10g with the liquid-solid ratio of reacting of electrolytic manganese residues as oxidant, the oxidant.
The Efficient Conversion that iron in electrolytic manganese residues may be implemented under preferred reaction condition is conducive to subsequent deferrization process.
Preferred scheme, oxalic acid and electrolytic manganese residues mass ratio are 1/1.2~1/1.6.By using the oxalic acid of appropriate amount,
Efficiently separating for iron can be not only may be implemented into ferric iron selective complexation, and the higher iron of purity can be separated and recovered.
The mass ratio of preferred scheme, removing of iron and manganese slag and sodium carbonate is 1:0.5~1.5.By using suitable sodium carbonate
High temperature solid state reaction is carried out with removing of iron and manganese slag, mainly by the lower quartzy phase SiO of removing of iron and manganese slag activity2It has been converted to reactivity
The Na of energy2SiO3。
Preferred scheme, the temperature of the calcining are 750 DEG C~800 DEG C, and the time is 2~3h.If temperature is lower than the section,
The purpose of inertia silicon source in activation electrolytic manganese slag is not achieved, the crystallization key of quartzy phase in electrolytic manganese residues can not be broken；If temperature is high
In the section, activation effect is not obviously improved, but can improve processing cost.
Preferred scheme, refined manganese dioxide slag and aluminum oxide, sodium hydroxide and water are according to molar ratio Si:Al:Na:H2O=
1:0.034:0.15:30 mixing.
Preferred scheme, the aging condition are as follows: the pH of control system between 9~10, at room temperature be aged 1~
3h。
Preferred scheme, the crystallization condition are as follows: under conditions of 175~185 DEG C keep the temperature 16~for 24 hours.
Preferred scheme is separated by solid-liquid separation gained liquid phase and ethyl alcohol is added, stand still for crystals, obtains three oxalic acid and close iron (III) hydrochlorate
Crystal.
The present invention is by obtaining electrolytic manganese residues powder for electrolytic manganese residues drying and ball milling.
Clear liquid obtained by separation of solid and liquid of the invention is placed in dark place crystallization, filters after being fully crystallized after ethyl alcohol is added,
With 50% ethanol washing crystal, drying is filtered, three oxalic acid is obtained and closes iron (III) sour potassium crystal.
The method for preparing analcime using electrolytic manganese residues of the invention, including implementation steps in detail below:
(1) the electrolytic manganese residues of certain mass are taken, dries, is milled to path grain powder with ball mill；
(2) by step, (1) powdered manganese slag obtained is dissolved in the distilled water of certain volume, and water after a certain amount of hydrogen peroxide is added
Bath heating, adds the distilled water of certain volume and suitable two oxalic acid hydrate is added, after reacting completely under magnet rotor stirring
Filtering retains solid residue；
(3) the mass mixings such as manganese slag and powdered sodium carbonate (2) step to be removed to iron after, subsequent calcination；
(4) the supernatant (2) step to be removed to iron after is added appropriate dehydrated alcohol and is placed on dark place crystallization, takes out after crystallizing completely
Filter filters drying with 50% ethanol washing crystal, obtains three oxalic acid and closes iron (III) sour potassium crystal；
(5) by step, (3) alkali melts manganese slag and Al after activation2O3、NaOH、H2O according to certain mol proportion example (Si:Al:Na:
H2O=1:0.034:0.15:30) proportion obtains mixed solution, and pH is to alkalescent for adjusting, subsequent to be aged at room temperature；
(6) the mixture after (4) is step being aged put into baking oven, and crystallization is crystallized under conditions of 180 DEG C, washed after taking-up to
Neutrality obtains pure phase analcime product after drying.
Compared with the prior art, the invention has the advantages that and effect:
1. the present invention obtains high pure phase analcime using electrolytic manganese waste residue solid waste, while having recycled iron, really real
The resource utilization for having showed electrolytic manganese residues solves the problems, such as solid waste environmental pollution；
2. technical solution of the present invention removes iron by the complexing of hydrogen peroxide oxidation combination oxalic acid, to the selectively removing efficiency of iron
Height, and be conducive to recycle ferro element therein；
3. technical solution of the present invention, which takes full advantage of electrolytic manganese residues itself, has the characteristics that faintly acid, without additional addition medicament
PH is adjusted, most suitable reaction environment is provided for hydrogen peroxide；Compared with the method for tradition strong acid, with weak acid (oxalic acid) solution network
The iron ion filtered out in manganese slag is closed, does not have to the strong reductants such as selection sodium thiosulfate, and can reacted at room temperature, improves
Process conditions, it is energy saving；
4. technical solution of the present invention under conditions of no organic formwork agent, is aged at room temperature and lower temperature
Lower crystallization can the high pure phase of rapid synthesis micron order analcime, reaction condition is mild, and external need not introduce and add reagent.
5, technical solution of the present invention is reduced using oxalic acid and sodium carbonate as reaction addition medicament to reaction vessel corrosion resistant
The requirement of corrosion, and the cost of adding of agent is significantly reduced, milder reaction condition is created for engineer application in the future.
Detailed description of the invention
Fig. 1 is the SEM figure of analcime prepared by embodiment 1；
Fig. 2 is the EDS figure of analcime prepared by embodiment 1；
Fig. 3 is the XRD of analcime prepared by embodiment 1.
Fig. 4 is the XRD of analcime prepared by comparative example 1.
Specific embodiment
Following embodiment is intended to further illustrate the content of present invention, rather than limits the protection model of the claims in the present invention
It encloses.
Embodiment 1:
Electrolytic manganese residues in following instance are both from two factory of Zhongxin Dameng Mining Industry Co., Ltd.'s manganese metal, technique
It is to roast manganese dioxide original ore powder and coal in rotary kiln high temperature, is converted to bivalent manganese, then with sulfuric acid to leach, utilizes sheet frame
Filters pressing obtains electrolytic manganese residues.
(1) electrolytic manganese residues are dried under the conditions of 105 DEG C, be broken into powder with 3000r/min ball mill ball milling 5min；
(2) take the powdered manganese slag of 100g to be dissolved in the distilled water of 150mL, it is pure that the analysis that 12mL mass fraction is 30% is added
Hydrogen peroxide under the conditions of 90 DEG C after stirring in water bath 2 hours, adds the bis- oxalic acid hydrate crystal of distilled water and 80g of 200mL,
The lower reaction of magnet rotor stirring is filtered afterwards for 24 hours, retains solid residue and supernatant respectively；
(3) it will be mixed except the manganese slag after iron with quality (7g:7g) such as powdered sodium carbonates, calcine 3h under conditions of 750 DEG C；
(4) the supernatant (2) step to be removed to iron after is added the appropriate dehydrated alcohol of 100mL and is placed on dark place crystallization, and crystallization is complete
After filter, with 50% ethanol washing crystal, drying obtains three oxalic acid and closes iron (III) sour potassium after dry under conditions of 60 DEG C
Crystal；
(5) alkali is melted into the 10g manganese slag after activation and 0.2049gAl is added2O3、0.48g NaOH、40ml H2O obtains mixing molten
Liquid is aged 2h after adjusting between pH to 9~10 at room temperature；
(6) baking oven is put into after the gelatinous mixture after ageing being transferred to stainless steel cauldron, it is brilliant under conditions of 180 DEG C
Change for 24 hours, washing obtains pure phase zeolite product 29g to neutrality after taking-up after drying.
The SEM figure of the analcime of preparation is as shown in Figure 1；, it is clear that zeolite product is clear in structure from SEM figure
Uniformly, miscellaneous few, the purity of product is higher.
The EDS figure of the analcime of preparation is as shown in Figure 2；The silica alumina ratio for the zeolite surface that EDS result obtains is higher than 2.5.Boiling
The silica alumina ratio of stone can consumingly influence its Acidity, that is acid amount and acid strength.In general, silica alumina ratio raising can reduce
The total acid content of zeolite, but can improve the acid strength of strong acid point achievees the purpose that improve zeolite absorption property with this.
The XRD of the analcime of preparation is as shown in Figure 3.XRD spectra can be seen that product peak and standard card degree of fitting are high, nothing
Miscellaneous peak occurs, and illustrates that crystallinity and purity are all in higher level in zeolite product.
The BET of the analcime of preparation such as table 1.
Table 1 is the BET of the analcime of preparation
Embodiment 2:
(1) electrolytic manganese residues are dried under the conditions of 105 DEG C, be broken into powder with 3000r/min ball mill ball milling 5min；
(2) take the powdered manganese slag of 100g to be dissolved in the distilled water of 150mL, it is pure that the analysis that 12mL mass fraction is 30% is added
Hydrogen peroxide under the conditions of 90 DEG C after stirring in water bath 2 hours, adds the bis- oxalic acid hydrate crystal of distilled water and 80g of 200mL,
The lower reaction of magnet rotor stirring is filtered afterwards for 24 hours, retains solid residue and supernatant respectively；
(3) mixing will be mixed with powdered sodium carbonate (mass ratio 8g:6.4g) except the manganese slag after iron, forged under conditions of 800 DEG C
Burn 2h；
(4) the supernatant (2) step to be removed to iron after is added 100mL dehydrated alcohol and is placed on dark place crystallization, takes out after crystallizing completely
Filter, it with 50% ethanol washing crystal, drains, three oxalic acid is obtained after dry under conditions of 60 DEG C and close iron (III) sour potassium crystal；
(5) alkali is melted into the 10g manganese slag after activation and 0.2049gAl is added2O3、0.48g NaOH、40ml H2O obtains mixing molten
Liquid is aged 2h at room temperature；
(6) baking oven is put into after the gelatinous mixture after ageing being transferred to stainless steel cauldron, it is brilliant under conditions of 180 DEG C
Change 16h, washing obtains pure phase zeolite product 35g to neutrality after taking-up after drying.
The BET of the analcime of preparation such as table 2.
Table 2 is the BET of the analcime of preparation
Comparative example 1:
(1) electrolytic manganese residues are dried under the conditions of 105 DEG C, be broken into powder with 3000r/min ball mill ball milling 5min；
(2) take the powdered manganese slag of 100g to be dissolved in the distilled water of 150mL, it is pure that the analysis that 10mL mass fraction is 30% is added
Hydrogen peroxide under the conditions of 90 DEG C after stirring in water bath 2 hours, adds the bis- oxalic acid hydrate crystal of distilled water and 80g of 200mL,
The lower reaction of magnet rotor stirring is filtered afterwards for 24 hours, retains solid residue and supernatant respectively.
(3) mixing will be mixed with powdered sodium carbonate (mass ratio 8g:6.4g) except the manganese slag after iron, under conditions of 600 DEG C
Calcine 2h；
(4) slag after alkali fusion calcining and activating is subjected to XRD detection, obtains Fig. 4 testing result.In XRD result, calcining
Still for inert quartzy phase in slag, the purpose not up to activated can not continue the zeolite synthesis step of next step.
The foregoing is merely preferred embodiment, all equivalent changes done according to scope of the present invention patent with repair
Decorations, are covering scope of the invention.
Claims (10)
1. a kind of method for preparing analcime using electrolytic manganese residues, it is characterised in that: the following steps are included:
1) electrolytic manganese residues powder is mixed with water after sizing mixing, addition oxidant progress oxidation reaction makes low in slurry in the slurry
Valence iron is converted to ferric iron, adds the ferric iron in oxalic acid solution complexing slurry, is separated by solid-liquid separation, solid phase is removing of iron and manganese slag；
2) removing of iron and manganese slag and sodium carbonate mixed calcining are activated, obtains refined manganese dioxide slag；
3) after refined manganese dioxide slag being mixed with aluminum oxide, sodium hydroxide and water, ageing, crystallization to get.
2. a kind of method for preparing analcime using electrolytic manganese residues according to claim 1, it is characterised in that: electrolytic manganese residues
The solid-to-liquid ratio of powder and water is 1g/1.5mL~1g/1.8mL.
3. a kind of method for preparing analcime using electrolytic manganese residues according to claim 1, it is characterised in that: the oxidation
The condition of reaction are as follows: temperature is 85~95 DEG C, and the time is 1~3h, described using the hydrogen peroxide of 20~35wt% as oxidant
Oxidant is 1mL/8g~1mL/10g with the liquid-solid ratio of reacting of electrolytic manganese residues.
4. a kind of method for preparing analcime using electrolytic manganese residues according to claim 1, it is characterised in that: oxalic acid and electricity
Solving manganese slag mass ratio is 1/1.2~1/1.6.
5. a kind of method for preparing analcime using electrolytic manganese residues according to claim 1, it is characterised in that: removing of iron and manganese slag
Mass ratio with sodium carbonate is 1:0.5~1.5.
6. a kind of method for preparing analcime using electrolytic manganese residues according to claim 1 or 5, it is characterised in that: described
The temperature of calcining is 750 DEG C~800 DEG C, and the time is 2~3h.
7. a kind of method for preparing analcime using electrolytic manganese residues according to claim 1, it is characterised in that: refined manganese dioxide slag
With aluminum oxide, sodium hydroxide and water according to molar ratio Si:Al:Na:H2O=1:0.034:0.15:30 mixing.
8. a kind of method for preparing analcime using electrolytic manganese residues according to claim 1, it is characterised in that: the ageing
Condition are as follows: the pH of control system is aged 1~3h between 9~10 at room temperature.
9. a kind of method for preparing analcime using electrolytic manganese residues according to claim 1, it is characterised in that: the crystallization
Change condition are as follows: under conditions of 175~185 DEG C keep the temperature 16~for 24 hours.
10. a kind of method for preparing analcime using electrolytic manganese residues according to claim 1, it is characterised in that: solid-liquid point
Ethyl alcohol is added from gained liquid phase, stands still for crystals, obtains three oxalic acid and closes iron (III) hydrochlorate crystal.
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Cited By (5)
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| CN110479207A (en) * | 2019-07-26 | 2019-11-22 | 铜仁学院 | A kind of method that the alkali fusion activation of electrolytic manganese residues microwave prepares high adsorption value fluorite |
| CN111715193A (en) * | 2020-07-02 | 2020-09-29 | 武汉大学 | Analcime/chitosan composite material, preparation method thereof and application of analcime/chitosan composite material as heavy metal adsorption material |
| CN112941328A (en) * | 2019-12-11 | 2021-06-11 | 内蒙古蒙泰集团有限公司 | Treatment method for recycling fly ash |
| CN114394771A (en) * | 2022-01-04 | 2022-04-26 | 广西大学 | Method for resource utilization of manganese ore slag generated in manganese sulfate production process |
| CN114644343A (en) * | 2022-04-13 | 2022-06-21 | 贵州大学 | Method for preparing pure-phase X-type zeolite by electrolytic manganese slag |
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| CN101831544A (en) * | 2010-05-18 | 2010-09-15 | 中国地质科学院郑州矿产综合利用研究所 | Method for separating manganese and silver from manganese-silver ore and purifying manganese leaching solution to extract manganese sulfate |
| CN108203097A (en) * | 2016-12-19 | 2018-06-26 | 南京工业大学 | A kind of method of electrolytic manganese residues high-efficiency resource recycling |
| CN108273516A (en) * | 2017-10-12 | 2018-07-13 | 北京森泉伟业科技有限公司 | A kind of method that electrolytic manganese residues prepare effective catalyst and catalyzing hydrogen peroxide oxidative degradation methylene blue |
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| WO2010024545A3 (en) * | 2008-08-26 | 2010-07-01 | 한국지질자원연구원 | A method for the autothermal manufacture of fired material using a vertical furnace |
| CN101831544A (en) * | 2010-05-18 | 2010-09-15 | 中国地质科学院郑州矿产综合利用研究所 | Method for separating manganese and silver from manganese-silver ore and purifying manganese leaching solution to extract manganese sulfate |
| CN108203097A (en) * | 2016-12-19 | 2018-06-26 | 南京工业大学 | A kind of method of electrolytic manganese residues high-efficiency resource recycling |
| CN108273516A (en) * | 2017-10-12 | 2018-07-13 | 北京森泉伟业科技有限公司 | A kind of method that electrolytic manganese residues prepare effective catalyst and catalyzing hydrogen peroxide oxidative degradation methylene blue |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110479207A (en) * | 2019-07-26 | 2019-11-22 | 铜仁学院 | A kind of method that the alkali fusion activation of electrolytic manganese residues microwave prepares high adsorption value fluorite |
| CN112941328A (en) * | 2019-12-11 | 2021-06-11 | 内蒙古蒙泰集团有限公司 | Treatment method for recycling fly ash |
| CN111715193A (en) * | 2020-07-02 | 2020-09-29 | 武汉大学 | Analcime/chitosan composite material, preparation method thereof and application of analcime/chitosan composite material as heavy metal adsorption material |
| CN114394771A (en) * | 2022-01-04 | 2022-04-26 | 广西大学 | Method for resource utilization of manganese ore slag generated in manganese sulfate production process |
| CN114644343A (en) * | 2022-04-13 | 2022-06-21 | 贵州大学 | Method for preparing pure-phase X-type zeolite by electrolytic manganese slag |
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