CN104591223A - Method for treating fluosilicate waste residues - Google Patents
Method for treating fluosilicate waste residues Download PDFInfo
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- CN104591223A CN104591223A CN201510053855.5A CN201510053855A CN104591223A CN 104591223 A CN104591223 A CN 104591223A CN 201510053855 A CN201510053855 A CN 201510053855A CN 104591223 A CN104591223 A CN 104591223A
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- silicofluoride
- filtrate
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Abstract
The invention discloses a method for treating fluosilicate waste residues. The method comprises the following steps: determining the total content of fluosilicate in the waste residues, so as to determine the usage amount of sodium hydroxide required to react with fluosilicate; mixing the waste residues and water according to the mass ratio of (1:30) to (1:40), heating up, then, adding a sodium hydroxide solution, stirring and reacting; removing manganese ions and permanganate ions from the solution obtained through reaction in the step (2); carrying out first-time filtration on the solution obtained in the step (3) so as to obtain a first filtrate and filtrated residue; concentrating and crystallizing the first filtrate, and then, carrying out second-time filtration so as to obtain sodium fluoride solid and a second filtrate; concentrating and crystallizing the second filtrate, then, carrying out third-time filtration so as to obtain a crude product potassium fluoride solid and a third filtrate, and recrystallizing the crude product potassium fluoride solid, so as to obtain a product potassium fluoride and a fourth filtrate. The method disclosed by the invention is aimed at treating and utilizing the fluosilicate waste residues generated from potassium permanganate and sodium fluosilicate which serve as raw materials.
Description
Technical field
The present invention relates to the disposal and utilization technical field of industrial residue, particularly a kind for the treatment of process of silicofluoride 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 KMnO
4, NaMnO
4, MnO
2, Na
2siF
6, MnSiF
6, SiO
2, NaF 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, in the process of attempting this waste residue of process, find that mn ion is difficult to removing, easily be blended in Potassium monofluoride and Sodium Fluoride, in addition, the problem that Sodium Fluoride is separated out too early is easily there is after adding sodium hydroxide in the water solution system of waste residue, silicofluoric acid root is difficult to complete reaction simultaneously, or easily react rear generation silicate flocculent gel with excessive sodium hydroxide, reaction is hindered to carry out further or reduce reaction carrying out degree, also can make precipitate and separate difficulty simultaneously, product conglomeration, the problems such as crystallisate foreign matter content is many.
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: a kind for the treatment of process of silicofluoride waste residue comprises the following steps:
A treatment process for silicofluoride waste residue, comprises the following steps:
Step 1: the total content determining silicofluoric acid root in waste residue, the sodium hydroxide concentration needed for determining to react with silicofluoric acid root with this;
Step 2: be, after 1:30 ~ 1:40 mixes and heats up, add sodium hydroxide solution and stir, reaction with mass ratio by waste residue and water;
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 carries out first time and filters, and first time filters 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 thick product Potassium monofluoride solid and the 3rd filtrate.
Step 7: thick product Potassium monofluoride solid, after recrystallization, obtains product Potassium monofluoride and the 4th filtrate.
In step 2, the chemical reaction of generation is as follows:
K
2SiF
6+4NaOH＝4NaF+2KF+SiO
2+2H
2O
Na
2SiF
6+4NaOH＝6NaF+SiO
2+2H
2O
MnSiF
6+4NaOH＝4NaF+MnF
2+SiO
2+2H
2O
In the treatment process of above-mentioned silicofluoride waste residue, in described step 1, sodium hydroxide concentration is 0.90 ~ 1.09 times of the amount with sodium hydroxide needed for silicofluoric acid root reaction theory, is preferably 1.03 ~ 1.09 times.The concentration of sodium hydroxide solution is preferably 3 ~ 5mol/L, and wherein, namely, the mol ratio according to sodium hydroxide and silicofluoric acid root is the theoretical amount that 4:1 determines to the amount of theoretical required sodium hydroxide.
In the treatment process of above-mentioned silicofluoride waste residue, in described step 2, temperature of reaction is 80 DEG C ~ 100 DEG C.
In the treatment process of above-mentioned silicofluoride waste residue, in described step 2, fully after reaction, pH value of solution is 7 ~ 10.
In the treatment process of above-mentioned silicofluoride 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 high manganese ion.
In the process, the chemical reaction of generation is as follows:
3MnF
2+2KMnO
4+4NaOH＝5MnO
2+2KF+4NaF+2H
2O
3MnF
2+2NaMnO
4+4NaOH＝5MnO
2+6NaF+2H
2O
3H
2C
2O
4+2KMnO
4+6NaOH＝2MnO
2+2CO
2+K
2CO
3+3Na
2CO
3+6H
2O
3H
2C
2O
4+2NaMnO
4+6NaOH＝2MnO
2+2CO
2+4Na
2CO
3+6H
2O
Na
2CO
3+2HF＝H
2O+CO
2+2NaF
K
2CO
3+2HF＝H
2O+CO
2+2KF
Mn ion is converted into manganese dioxide precipitate completely, and high manganese ion transformation is called manganese dioxide precipitate and carbon dioxide.
In the treatment process of above-mentioned silicofluoride waste residue, in described step 3, when high manganese ion is excessive, adds oxalic acid solution and remove excessive high manganese ion.
Its reaction equation is above-mentioned chemical equation mesoxalic acid and high manganese ion reaction equation, and high manganese ion is transformed into completely in order to manganese dioxide precipitate and carbon dioxide.
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 Mn2+ remaining in the solution of step 2 little over the potassium permanganate (or sodium permanganate) measured, oxidation generates 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.
In the treatment process of above-mentioned silicofluoride waste residue, described first time is filtered into heat filtering, and the temperature of described heat filtering is 90 DEG C ~ 100 DEG C.
In the treatment process of above-mentioned silicofluoride waste residue, in the concentration operation of described step 5, the solution quality after concentrated is 1/20 ~ 1/30 of concentrated front solution quality.
In the treatment process of above-mentioned silicofluoride waste residue, in the crystallization operation of described step 5, Tc is room temperature.
In the treatment process of above-mentioned silicofluoride waste residue, in described step 5, also comprise: Sodium Fluoride solid adopts saturated Sodium Fluoride washing.
In the treatment process of above-mentioned silicofluoride waste residue, described step 6 also comprises: after third time filters, and the solid water obtain filtration or saturated potassium fluoride solution wash, drying, obtain thick product Potassium monofluoride.
In the treatment process of above-mentioned silicofluoride waste residue, in the concentration operation of described step 6, the solution quality after concentrated is 1/10 ~ 1/15 of concentrated front solution quality.
In the treatment process of above-mentioned silicofluoride waste residue, in the crystallization operation of described step 6, Tc is greater than 45 DEG C.If Tc is lower than 45 DEG C, then Potassium monofluoride is separated out with the form of two hydration Potassium monofluorides.
In the treatment process of above-mentioned silicofluoride waste residue, also comprise step 8: the 3rd filtrate and/or the 4th filtrate are joined in the first filtrate and recycled.
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 Sodium Fluoride, 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 traditional method, 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, employing sodium hydroxide is raw material, generates a large amount of Sodium Fluorides, and Potassium monofluoride is 150g 80 DEG C of solubleness; And the solubleness of Sodium Fluoride in water is very little, be only 4.89g 80 DEG C of solubleness.Easily occur that concentration of sodium fluoride is large, the problem separated out in reaction solution.Such product Sodium Fluoride will with SiO
2, MnO
2mix and lose, giving SiO simultaneously
2, MnO
2process bring difficulty.(because Sodium Fluoride solubleness in water is much lower compared with Potassium monofluoride), therefore this programme solves this problem by following measures:
1, significantly improve the consumption of water, allow the Sodium Fluoride generated be in undersaturated condition in reaction solution.
2, improve temperature of reaction, allow the Sodium Fluoride meltage in reaction solution generated increase.
3, changing filter type, original room temperature is filtered, has made filtered while hot into, preventing Sodium Fluoride from separating out and SiO when filtering
2, MnO
2mix.
In the present invention, the selection of sodium hydroxide concentration is particularly important, and cross and can cause reaction not exclusively at least, the fluorine in wastewater silicate content produced after treatment is high, easily causes environmental pollution; Too much easily cause silicate floss, cause precipitate and separate difficulty, the crystallisate foreign matter content serious problem such as many.
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, the 3rd filtrate and the 4th filtrate of last generation of the present invention can return recycling in the first filtrate, and it can circulate at least thousand times, which save with water, 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 1:30 with water by waste residue, stir and be warming up to 90 DEG C, (excess coefficient ratio is 0.90 to add 0.578 ton of sodium hydroxide, be made into about 4 tons of aqueous solution), stirring reaction, to react completely (pH is 7.1), 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.Maintain the temperature at 90 ~ 100 DEG C, for the first time heat filtering.By the filtrate evaporation concentration 20 times of first time heat filtering, 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 product Sodium Fluoride 0.817 ton.The filtrate that second time is filtered continues evaporation concentration 10 times, cooling, crystallization at 45 DEG C, and third time filters, filter cake water recrystallization, dry, obtains Potassium monofluoride product.It is product 0.161 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 1:35 with water, stir and be warming up to 95 DEG C, (excess coefficient ratio is 1.09 to add 0.761 ton of sodium hydroxide, be made into about 4 tons of aqueous solution), stirring reaction, to react completely (pH is 9.8), 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.Maintain the temperature at 90 ~ 100 DEG C, for the first time heat filtering.By the filtrate evaporation concentration 25 times of first time heat filtering, 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 product Sodium Fluoride 0.932 ton.The filtrate that second time is filtered continues evaporation concentration 12 times, cooling, crystallization at 48 DEG C, and third time filters, filter cake water recrystallization, dry, obtains Potassium monofluoride product.It is product 0.183 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 1:40 with water, stir and be warming up to 100 DEG C, (excess coefficient ratio is 1.08 to add 0.803 ton of sodium hydroxide, be made into about 4 tons of aqueous solution), stirring reaction, to react completely (pH is 8.5), 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.Maintain the temperature at 90 ~ 100 DEG C, for the first time heat filtering.By the filtrate evaporation concentration 30 times of first time heat filtering, 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 product Sodium Fluoride 0.975 ton.The filtrate that second time is filtered continues evaporation concentration 15 times, and cooling, at 46 DEG C, third time filters, filter cake water recrystallization, dry, obtains Potassium monofluoride product.It is product 0.195 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.
In embodiment 1-3, % all refers to mass percent.
Three gained NaF, KF Product checking results such as embodiment 1, embodiment 2, embodiment 3:
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.
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.
Claims (14)
1. a treatment process for silicofluoride waste residue, is characterized in that, comprises the following steps:
Step 1: the total content determining silicofluoric acid root in waste residue, the sodium hydroxide concentration needed for determining to react with silicofluoric acid root with this;
Step 2: be, after 1:30 ~ 1:40 mixes and heats up, add sodium hydroxide solution and stir, reaction with mass ratio by waste residue and water;
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 carries out first time and filters, and first time filters 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 thick product Potassium monofluoride solid and the 3rd filtrate;
Step 7: thick product Potassium monofluoride solid, after recrystallization, obtains product Potassium monofluoride and the 4th filtrate.
2. the treatment process of silicofluoride waste residue according to claim 1, is characterized in that, in described step 1, sodium hydroxide concentration is 0.90 ~ 1.09 times of the amount with sodium hydroxide needed for silicofluoric acid root reaction theory.
3. the treatment process of silicofluoride waste residue according to claim 1, is characterized in that, in described step 2, temperature of reaction is 80 DEG C ~ 100 DEG C.
4. the treatment process of silicofluoride waste residue according to claim 3, is characterized in that, in described step 2, fully after reaction, pH value of solution is 7 ~ 10.
5. the treatment process of silicofluoride 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 solution and remove excessive high manganese ion.
6. the treatment process of silicofluoride waste residue according to claim 1, is characterized in that, in described step 3, under there is high manganese ion situation in solution, adds oxalic acid solution and removes excessive high manganese ion.
7. the treatment process of silicofluoride waste residue according to claim 1, is characterized in that, described first time is filtered into heat filtering, and the temperature of described heat filtering is 90 DEG C ~ 100 DEG C.
8. the treatment process of silicofluoride waste residue according to claim 1, is characterized in that, in the concentration operation of described step 5, the solution quality after concentrated is 1/20 ~ 1/30 of concentrated front solution quality.
9. the treatment process of silicofluoride waste residue according to claim 8, is characterized in that, in the crystallization operation of described step 5, Tc is room temperature.
10. the treatment process of silicofluoride waste residue according to claim 9, is characterized in that, in described step 5, also comprises: Sodium Fluoride solid adopts saturated Sodium Fluoride washing.
The treatment process of 11. silicofluoride waste residues according to claim 1, it is characterized in that, described step 6 also comprises: after third time filters, and the solid water obtain filtration or saturated potassium fluoride solution wash, drying, obtain thick product Potassium monofluoride.
The treatment process of 12. silicofluoride waste residues according to claim 1, is characterized in that, in the concentration operation of described step 6, the solution quality after concentrated is 1/10 ~ 1/15 of concentrated front solution quality.
The treatment process of 13. silicofluoride waste residues according to claim 12, is characterized in that, in the crystallization operation of described step 6, Tc is greater than 45 DEG C.
The treatment process of 14. silicofluoride 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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| CN110589854A (en) * | 2019-10-24 | 2019-12-20 | 徐小岗 | Method for producing electronic-grade fluoride salt by using fluosilicic acid and fluosilicate |
| CN113369289A (en) * | 2021-07-28 | 2021-09-10 | 嘉应学院 | Treatment method for dangerous solid waste containing fluorine silicate |
| CN117247024A (en) * | 2023-09-12 | 2023-12-19 | 内蒙古星汉新材料有限公司 | Method for extracting byproduct potassium silicate |
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| CN110589854A (en) * | 2019-10-24 | 2019-12-20 | 徐小岗 | Method for producing electronic-grade fluoride salt by using fluosilicic acid and fluosilicate |
| CN113369289A (en) * | 2021-07-28 | 2021-09-10 | 嘉应学院 | Treatment method for dangerous solid waste containing fluorine silicate |
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| CN117247024B (en) * | 2023-09-12 | 2024-09-20 | 内蒙古星汉新材料有限公司 | Method for extracting byproduct potassium silicate |
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|---|---|
| CN104591223B (en) | 2016-05-04 |
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