CN104591224A - Treatment method for producing sodium permanganate waste residues - Google Patents
Treatment method for producing sodium permanganate waste residues Download PDFInfo
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- CN104591224A CN104591224A CN201510056030.9A CN201510056030A CN104591224A CN 104591224 A CN104591224 A CN 104591224A CN 201510056030 A CN201510056030 A CN 201510056030A CN 104591224 A CN104591224 A CN 104591224A
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Abstract
The invention discloses a treatment method for producing sodium permanganate waste residues. The method comprises the following steps: determining total content of fluosilicate in the waste residues to determine the amount of potassium hydroxide required for reaction with the fluosilicate; mixing, heating and reacting the waste residues, a potassium hydroxide solution and water; removing manganese ions and permanganate ions in the reacted solution; filtering the obtained solution for the first time to obtain first filtrate and filter residues; concentrating and crystallizing the first filtrate, and filtering for the second time to obtain a sodium fluoride solution and second filtrate; concentrating and crystallizing the second filtrate, and filtering for the third time to obtain a potassium fluoride crude product and third filtrate; carrying out recrystallizing operation on the obtained potassium fluoride crude product; separating and drying to obtain a potassium fluoride product; and separating to obtain fourth filtrate. The invention aims at providing a method for treating and utilizing the waste residues generated by sodium permanganate production employing potassium permanganate and sodium fluosilicate as raw materials.
Description
Technical field
The present invention relates to the disposal and utilization technical field of industrial residue, particularly produce the treatment process of sodium permanganate waste residue.
Background technology
A kind of sodium permanganate production new technology of Guangdong Hangxin Technology Co., Ltd.'s independent research, has obtained national inventing patent (patent No. 201010231951.1).This technology is with potassium permanganate and Sodium Silicofluoride for raw material, adopts to exempt from chlorination single stage method and prepare sodium permanganate product, and technical process is simple and practical, and whole process is without toxic harmful exhaust gas, discharge of wastewater, and good quality of product, chloride content is low.Produce the technology ratio of sodium permanganate with other, it be efficient, safety, environmental protection, good quality of product.Although have above-mentioned lot of advantages with the method that potassium permanganate and Sodium Silicofluoride are raw material production sodium permanganate, but yet there are some problems in it: a large amount of waste residue will be produced in production, at present waste residue is transported to cinder yard by this enterprise, carries out sealing up for safekeeping process and carrys out meet the requirement of environmental protection.By current processing mode, not only to expend the cost of relatively large manpower, land resources, increase product, but also be the great wasting of resources.Analysis shows, the main component of this waste residue is K
2siF
6, another containing a small amount of Na
2siF
6, MnSiF
6, KMnO
4, NaMnO
4, MnO
2, SiO
2, NaF, KF etc.Silicofluoride content is up to 85% ~ 95%, if its waste residue can be reclaimed comprehensive utilization, both the place needed for waste residue stacking, expense can have been reduced, reduce the pollution to environment, also can turn waste into wealth, carry out effective utilization of resource, bring good economic benefit to enterprise, for Sustainable Development of Enterprises is expanded space.
Because this waste residue is a kind of novel waste residue, through literature survey, there is no people at present and relate to its process and comprehensive utilization.Contriver is successfully extracted Na from waste residue
2siF
6reuse in the production of sodium permanganate, and eliminates MnO
2, MnO
4 -pure K is obtained Deng impurity
2siF
6product (applying for a patent separately).But this technique employs special ultrasonic device, noise is large, it is high to consume energy, and the more important thing is that the market demand of potassium silicofluoride is less; If by obtained K
2siF
6it is long then to there is operational path for the production of KF in product, the problem that production cost is relatively high.
Summary of the invention
The object of this invention is to provide a kind of method of disposal and utilization of the waste residue for producing for raw material production sodium permanganate with potassium permanganate and Sodium Silicofluoride.
K with the waste residue main component that potassium permanganate and Sodium Silicofluoride produce for raw material production sodium permanganate
2siF
6, in anhydrous dry slag K
2siF
6content is 48 ~ 65w%; The another Na containing 20 ~ 47w%
2siF
6; Also containing a small amount of KMnO
4, NaMnO
4, MnO
2, MnSiF
6, SiO
2, the plurality of impurities such as NaF, KF.With potassium permanganate and Sodium Silicofluoride in raw material production sodium permanganate technique, the waste residue of generation often water content is greater than 10w%, and after for some time is stacked in stockyard, moisture can evaporate gradually, and water content can reduce.W% refers to mass percent.
Technical scheme of the present invention is: the treatment process of producing sodium permanganate waste residue, comprises the following steps:
Step 1: the total content determining silicofluoric acid root in waste residue, the potassium hydroxide consumption needed for determining to react with silicofluoric acid root with this;
Step 2: waste residue, potassium hydroxide solution, water mixing are heated up, reaction;
Step 3: remove the mn ion in the solution be obtained by reacting through step 2 and high manganese ion;
Step 4: solution step 3 obtained filters through first time and obtains the first filtrate and filter residue;
Step 5: after the first concentrating filter liquor, crystallization, carries out second time and filters, obtain Sodium Fluoride solid and the second filtrate;
Step 6: by the second filtrate after concentrated, crystallization, carry out third time filtration, obtain Potassium monofluoride crude product and the 3rd filtrate;
Step 7: obtained Potassium monofluoride crude product is carried out recrystallization operation, obtains Potassium monofluoride finished product, also obtains the 4th filtrate after separation after separation, drying.
In step 2, the chemical reaction of existence is as follows:
K
2SiF
6+4KOH＝6KF+SiO
2+2H
2O
Na
2SiF
6+4KOH＝4KF+2NaF+SiO
2+2H
2O
MnSiF
6+4KOH＝4KF+MnF
2+SiO
2+2H
2O
In the treatment process of above-mentioned production sodium permanganate waste residue, in described step 1, potassium hydroxide consumption is 0.91 ~ 1.08 times of the amount with potassium hydroxide needed for silicofluoric acid root reaction theory, is preferably 1.01 ~ 1.08 times.Wherein, namely, the mol ratio according to potassium hydroxide and silicofluoric acid root is the theoretical amount that 4:1 determines to the amount of potassium hydroxide needed for silicofluoric acid root reaction theory.
In the treatment process of above-mentioned production sodium permanganate waste residue, after described waste residue first fully mixes with water, and then add potassium hydroxide solution.Its mode that dropping or segmentation can be adopted to add adds, and also can disposablely add.Certainly, in the present invention, potassium hydroxide can also be adopted to be dissolved in water in advance to be formed, then add waste residue.
In the treatment process of above-mentioned production sodium permanganate waste residue, in described step 2, the mass ratio of waste residue and water is 1:10 ~ 1:20.
In the treatment process of above-mentioned production sodium permanganate waste residue, the temperature of reaction of described step 2 is 70 DEG C ~ 90 DEG C.
In the treatment process of above-mentioned production sodium permanganate waste residue, in described step 2, fully the rear pH value of solution of reaction is 7 ~ 10.
In the treatment process of above-mentioned production sodium permanganate waste residue, in described step 3, when there is mn ion in solution, adding excessive potassium permanganate or sodium permanganate reaction, then adding oxalic acid solution and remove excessive MnO4.
Concrete chemical equation is as follows:
3MnF
2+2KMnO
4+4KOH＝6KF+5MnO
2+2H
2O
3MnF
2+2NaMnO
4+4KOH＝4KF+2NaF+5MnO
2+2H
2O
Now, mn ion changes manganese dioxide precipitate in the basic conditions completely.
In the treatment process of above-mentioned production sodium permanganate waste residue, in described step 3, when there is high manganese ion in solution, adding oxalic acid solution and removing excessive MnO4.
Specifically, drip in filter paper with the take a morsel solution of step 2 of dropper, if the liquid circle diffused out is red-purple, for remaining MnO4, the dilute solution that need add oxalic acid potassium permanganate remaining in the solution of step 2 is become Manganse Dioxide (potassium permanganate this spontaneous for indicator can directing terminal).Dripping in filter paper with the take a morsel solution of step 2 of dropper, if the liquid circle diffused out is colourless, is remaining divalent manganesetion.Add Mn remaining in the solution of step 2 little over the potassium permanganate (or sodium permanganate) measured
2+, oxidation Manganse Dioxide, and then the dilute solution of the rare oxalic acid of addition excessive potassium permanganate is also become Manganse Dioxide (potassium permanganate this spontaneous for indicator can directing terminal).Aforesaid method is fairly simple, but in laboratory and Industrial processes, detect whether excessive aforesaid method is not unique method, as can also adopt titrimetry, ion chromatography which kind of ion of methods analyst excessive.
As follows by the concrete chemical equation of oxalic acid removing high manganese ion:
3H
2C
2O
4+2KMnO
4+6KOH＝2MnO
2+2CO
2+4K
2CO
3+6H
2O
3H
2C
2O
4+2NaMnO
4+6KOH＝2MnO
2+2CO
2+Na
2CO
3+3K
2CO
3+6H
2O
Na
2CO
3+2HF＝H
2O+CO
2+2NaF
K
2CO
3+2HF＝H
2O+CO
2+2KF
In the process, MnO4, under the oxalic acid existent condition of q.s, changes carbon dioxide, manganese dioxide precipitate removing into completely.
In the treatment process of above-mentioned production sodium permanganate waste residue, in the concentration operation of described step 5, the solution quality after concentrated is 1/10 ~ 1/15 of concentrated front solution quality.
In the treatment process of above-mentioned production sodium permanganate waste residue, in the crystallization operation of described step 5, Tc is room temperature.
In the treatment process of above-mentioned production sodium permanganate waste residue, described step 6 also comprises: by obtained Sodium Fluoride solid water or the washing of saturated Fluorinse, dry, obtain Sodium Fluoride finished product.
In the treatment process of above-mentioned production sodium permanganate waste residue, in the concentration operation of described step 6, the solution quality after concentrated is 1/2 ~ 1/5 of concentrated front solution quality.
In the treatment process of above-mentioned production sodium permanganate waste residue, in the crystallization operation of described step, Tc is greater than 45 DEG C.
In the treatment process of above-mentioned production sodium permanganate waste residue,
Also comprise step 8: the 3rd filtrate and/or the 4th filtrate are joined in the first filtrate and recycled.
The present invention's potassium hydroxide directly processes the technique that KF produced by waste residue.Original K in waste residue in treating processes
2siF
6, Na
2siF
6, MnSiF
6react with KOH and generate KF, NaF, MnO
2, SiO
2; MnO
2, SiO
2can with original MnO in waste residue
2, SiO
2filter and remove in the lump.In waste residue, original NaF, KF are water-soluble merges with product.Make use of contained Mn in waste residue especially cleverly
2+, MnO
4 -self react in the basic conditions and generate MnO
2eliminate most Mn.The removal of remaining Mn, the present invention processes in two kinds of situation and has dissolved this difficult problem.(1) for Mn
2+excessive, after waste residue and potassium hydroxide react completely, add a certain amount of oxygenant KMnO
4allow its solution be red-purple, be transformed to MnO by problem
4 -excessively to process.(2) for MnO
4 -excessive, MnO
4 -indivisible problem, after waste residue and potassium hydroxide react completely, adds a certain amount of oxalic acid to MnO
4 -red-purple just take off, generate MnO
2, remove excessive MnO
4 -.Present invention process route is brief, and without the need to specific installation, production cost significantly reduces.
Can realize waste residue to be converted to completely solvable Potassium monofluoride and Sodium Fluoride and insoluble Manganse Dioxide and silicon-dioxide by scheme provided by the present invention, wherein, the main component that this programme reclaims is Potassium monofluoride, Potassium monofluoride can be realized by filtering separation and condensing crystal to be separated with the effective of Sodium Fluoride, the purity of Potassium monofluoride and Sodium Fluoride is all greater than 98%, and wherein the mass percentage content of manganese element is all less than 0.001%.
In the present invention, in order to solve the problem of manganese element too high levels in product, this programme judges to react the mn ion in middle and later periods solution or MnO4 remaining quantity by experiment, when mn ion remaining quantity is large, adding MnO4 makes mn ion be converted into manganese dioxide precipitate, and then adopts oxalic acid treatment, when MnO4 remaining quantity is large, adopt oxalic acid removing to make it to be converted into manganese dioxide precipitate, prevent manganese element in Sodium Fluoride and Potassium monofluoride from exceeding standard.Meanwhile, manganese element recovery and reuse in throw out are conducive to after manganese element being all converted into Manganse Dioxide.
In the present invention, the selection of potassium hydroxide consumption is particularly important, crosses and can cause reaction not exclusively at least, still containing silicofluoride in the waste residue produced after treatment, cause waste residue utilization rate to reduce, make troubles to subsequent production white carbon black simultaneously, also may produce fluoride waste and cause environmental pollution; Too much easily cause silicate floss, or even jelly, also can cause reaction not exclusively waste residue parcel; The problem that precipitate and separate difficulty, product conglomeration, crystallisate foreign matter content also to be made many etc. serious simultaneously.
In addition, in the present invention, adopt such scheme, in 3rd filtrate and the 4th filtrate, the ion content of the contaminate environment such as mn ion, high manganese ion, silicofluoric acid radical ion is very low, the advantage of such result is, 3rd filtrate and the 4th filtrate of last generation of the present invention can return recycling in the first filtrate, which save with water, have effectively saved cost.
Embodiment
Below in conjunction with embodiment, the invention will be further described, but the present invention is not limited only to this.
Embodiment 1
Analyze waste residue containing SiF
6 2-total content be 57%, get 1 ton, waste residue, after being mixed in the ratio of 1:10 with water by waste residue, stir and be warming up to 100 DEG C, (coefficient ratio is 0.91 to add 0.818 ton of potassium hydroxide, be made into about 4 tons of aqueous solution), stirring reaction, to react completely (pH is 7), takes a morsel reaction drop on filter paper, colourless, add concentration be 1% potassium permanganate solution to reaction solution just in red-purple.Again in reaction solution, adding concentration is that the oxalic acid of 10% is to MnO
4 -red-purple just take off.
First time filters.By the filtrate evaporation concentration 10 times that first time filters, cooling, crystallizing at room temperature, second time is filtered.The filter cake saturated sodium fluoride aqueous solution washing that second time is filtered, dry, obtain byproduct Sodium Fluoride 0.173 ton.The filtrate that second time is filtered continues evaporation concentration 2 times, cooling, crystallization at 45 DEG C, and third time filters, filter cake water recrystallization, dry, obtains Potassium monofluoride product.It is product 0.816 ton that waste residue per ton obtains Potassium monofluoride content; Filtrate (filtrate of filtering with the first time merges) reuse of the filtrate that third time filters, recrystallization.The filter cake that first time filters can produce white carbon black and Manganse Dioxide separately.
Embodiment 2
Analyze waste residue containing SiF
6 2-total content be 62%, get 1 ton, waste residue, after waste residue is mixed in the ratio of 1:15 with water, stir and be warming up to 75 DEG C, (excess coefficient ratio is 1.08 to add 1.056 tons of potassium hydroxide, be made into about 4 tons of aqueous solution), stirring reaction, to react completely (pH is 10), take a morsel reaction drop on filter paper, red-purple, in reaction solution, adding concentration is that the oxalic acid of 10% is to MnO
4 -red-purple just take off.First time filters.By the filtrate evaporation concentration 12 times that first time filters, cooling, crystallizing at room temperature, second time is filtered.The filter cake saturated sodium fluoride aqueous solution washing that second time is filtered, dry, obtain byproduct Sodium Fluoride 0.190 ton.The filtrate that second time is filtered continues evaporation concentration 3.5 times, cooling, crystallization at 48 DEG C, and third time filters, filter cake water recrystallization, dry, obtains Potassium monofluoride product.It is product 0.854 ton that waste residue per ton obtains Potassium monofluoride content; Filtrate (filtrate of filtering with the first time merges) reuse of the filtrate that third time filters, recrystallization.The filter cake that first time filters can produce white carbon black and Manganse Dioxide separately.
Embodiment 3
Analyze waste residue containing SiF
6 2-total content be 66%, get 1 ton, waste residue, after waste residue is mixed in the ratio of 1:20 with water, stir and be warming up to 85 DEG C, (excess coefficient ratio is 1.04 to add 1.083 tons of potassium hydroxide, be made into about 4 tons of aqueous solution), stirring reaction, to react completely (pH is 9), take a morsel reaction drop on filter paper, red-purple, in reaction solution, adding concentration is that the oxalic acid of 10% is to MnO
4 -red-purple just take off.First time filters.By the filtrate evaporation concentration 15 times that first time filters, cooling, crystallizing at room temperature, second time is filtered.The filter cake saturated sodium fluoride aqueous solution washing that second time is filtered, dry, obtain byproduct Sodium Fluoride 0.251 ton.The filtrate that second time is filtered continues evaporation concentration 3.5 times, cooling, crystallization at 46 DEG C, and third time filters, filter cake water recrystallization, dry, obtains Potassium monofluoride product.It is product 1.124 tons that waste residue per ton obtains Potassium monofluoride content; Filtrate (filtrate of filtering with the first time merges) reuse of the filtrate that third time filters, recrystallization.The filter cake that first time filters can produce white carbon black and Manganse Dioxide separately.
In embodiment 1-3, % all refers to mass percent.
Three gained KF, the NaF Product checking results such as embodiment 1, embodiment 2, embodiment 3:
KF, various index all reaches GB/T 1271-2011 chemical pure standard.Potassium monofluoride (KF) ω/%>=98, clarity test≤5, free acid (HF) ω/%≤0.1, free alkali (KOH) ω/%≤0.1, muriate (Cl) ω/%≤0.005, vitriol (SO
4 2-) ω/%≤0.02, silicofluoride (SiF
6) ω/%≤0.1, iron (Fe) ω/%≤0.005, heavy metal (Pb) ω/%≤0.005, heavy metal (Mn) ω/%≤0.001.
NaF, various index all reaches GB/T 1264-1997 chemical pure standard.Sodium Fluoride (NaF) ω/%>=98, clarity test≤5, free acid (H
+) mmol/100g≤10, free alkali (OH
-) mmol/100g≤4, muriate (Cl) ω/%≤0.01, vitriol (SO
4 2-) ω/%≤0.05, silicofluoride (SiF
6) ω/%≤1.2, iron (Fe) ω/%≤0.005, heavy metal (Pb) ω/%≤0.005, heavy metal (Mn) ω/%≤0.001.
Claims (14)
1. produce a treatment process for sodium permanganate waste residue, it is characterized in that, comprise the following steps:
Step 1: the total content determining silicofluoric acid root in waste residue, the potassium hydroxide consumption needed for determining to react with silicofluoric acid root with this;
Step 2: waste residue, potassium hydroxide solution, water mixing are heated up, reaction;
Step 3: remove the mn ion in the solution be obtained by reacting through step 2 and high manganese ion;
Step 4: solution step 3 obtained filters through first time and obtains the first filtrate and filter residue;
Step 5: after the first concentrating filter liquor, crystallization, carries out second time and filters, obtain Sodium Fluoride solid and the second filtrate;
Step 6: by the second filtrate after concentrated, crystallization, carry out third time filtration, obtain Potassium monofluoride crude product and the 3rd filtrate;
Step 7: obtained Potassium monofluoride crude product is carried out recrystallization operation, obtains Potassium monofluoride finished product, also obtains the 4th filtrate after separation after separation, drying.
2. the treatment process of production sodium permanganate waste residue according to claim 1, is characterized in that, in described step 1, potassium hydroxide consumption is 0.91 ~ 1.08 times of the amount with potassium hydroxide needed for silicofluoric acid root reaction theory.
3. the treatment process of production sodium permanganate waste residue according to claim 1, is characterized in that, in step 2, after described waste residue first mixes with water, and then adds potassium hydroxide solution.
4. the treatment process of the production sodium permanganate waste residue according to claim 1 or 3, is characterized in that, in described step 2, the mass ratio of waste residue and water is 1:10 ~ 1:20.
5. the treatment process of production sodium permanganate waste residue according to claim 4, is characterized in that, the temperature of reaction of described step 2 is 70 DEG C ~ 100 DEG C.
6. the treatment process of production sodium permanganate waste residue according to claim 5, is characterized in that, in described step 2, fully the rear pH value of solution of reaction is 7 ~ 10.
7. the treatment process of production sodium permanganate waste residue according to claim 1, it is characterized in that, in described step 3, when there is mn ion in solution, add excessive potassium permanganate or sodium permanganate reaction, then add oxalic acid and remove excessive MnO4.
8. the treatment process of production sodium permanganate waste residue according to claim 1, is characterized in that, in described step 3, when there is high manganese ion in solution, adding oxalic acid and removing excessive MnO4.
9. the treatment process of production sodium permanganate waste residue according to claim 1, is characterized in that, in the concentration operation of described step 5, the solution quality after concentrated is 1/10 ~ 1/15 of concentrated front solution quality.
10. the treatment process of production sodium permanganate waste residue according to claim 9, is characterized in that, in the crystallization operation of described step 5, Tc is room temperature.
The treatment process of 11. production sodium permanganate waste residues according to claim 1, it is characterized in that, described step 6 also comprises: by obtained Sodium Fluoride solid water or the washing of saturated Fluorinse, dry, obtain Sodium Fluoride finished product.
The treatment process of 12. production sodium permanganate waste residues according to claim 1, is characterized in that, in the concentration operation of described step 6, the solution quality after concentrated is 1/2 ~ 1/5 of concentrated front solution quality.
The treatment process of 13. production sodium permanganate waste residues according to claim 12, it is characterized in that, in the crystallization operation of described step 6, Tc is greater than 45 DEG C.
The treatment process of 14. production sodium permanganate waste residues according to claim 1, is characterized in that, also comprise step 8: the 3rd filtrate and/or the 4th filtrate are joined in the first filtrate and recycled.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110589854A (en) * | 2019-10-24 | 2019-12-20 | 徐小岗 | Method for producing electronic-grade fluoride salt by using fluosilicic acid and fluosilicate |
| CN115676894A (en) * | 2022-11-23 | 2023-02-03 | 嘉应学院 | Resource utilization method of waste residues generated by treating organic wastewater with sodium permanganate |
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| CN102001688A (en) * | 2010-12-01 | 2011-04-06 | 陈锋 | Process for producing potassium sulfate by decomposing potassium feldspar at low temperature with fluorine-containing acid |
| CN102001686A (en) * | 2010-12-01 | 2011-04-06 | 陈锋 | Process for producing potassium fluoride and white carbon black by decomposing potassium feldspar with fluorine-containing acid at low temperature |
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| WO2009113088A2 (en) * | 2008-01-14 | 2009-09-17 | Aditya Birla Science & Technology Co. Limited | A process for manufacturing of potassium fluoride |
| CN101717097A (en) * | 2009-11-11 | 2010-06-02 | 云南云天化国际化工股份有限公司 | Method for separating sodium fluoride crystals from silicon dioxide |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110589854A (en) * | 2019-10-24 | 2019-12-20 | 徐小岗 | Method for producing electronic-grade fluoride salt by using fluosilicic acid and fluosilicate |
| CN115676894A (en) * | 2022-11-23 | 2023-02-03 | 嘉应学院 | Resource utilization method of waste residues generated by treating organic wastewater with sodium permanganate |
| CN115676894B (en) * | 2022-11-23 | 2024-01-12 | 嘉应学院 | Resource utilization method for waste residues generated by treating organic wastewater with sodium permanganate |
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| CN104591224B (en) | 2016-05-04 |
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