CN210559435U - Device for separating and preparing manganese carbonate from manganese-containing wastewater - Google Patents
Device for separating and preparing manganese carbonate from manganese-containing wastewater Download PDFInfo
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- CN210559435U CN210559435U CN201921471571.8U CN201921471571U CN210559435U CN 210559435 U CN210559435 U CN 210559435U CN 201921471571 U CN201921471571 U CN 201921471571U CN 210559435 U CN210559435 U CN 210559435U
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Abstract
The utility model relates to a device for separating and preparing manganese carbonate from manganese-containing wastewater, which comprises a first impurity removal tank, the first impurity removing tank is communicated with a first filter material inlet through a pipeline, a first filter material outlet of the first filter is communicated with a first filter material collecting tank, the first filtrate collecting tank is communicated with the second impurity removing tank and the second filter in sequence through pipelines, a filtrate discharge port of the second filter is communicated with the second filtrate collecting tank, the second filtrate collecting tank is communicated with a third impurity removing tank and a third filter in sequence through pipelines, a filtrate discharge port of the third filter is communicated with the third filtrate collecting tank, the third filtrate collecting tank is communicated with a fourth impurity removing tank and a fourth filter in sequence through pipelines, a filtrate discharge port of the fourth filter is communicated with the fourth filtrate collecting tank, and the fourth filtrate collecting tank is sequentially communicated with the fifth impurity removing tank and the fifth filter through pipelines. The utility model discloses carry out edulcoration purification treatment to titanium dioxide production manganese-containing waste water, carry out resource utilization.
Description
Technical Field
The utility model belongs to the technical field of manganese chloride production, a separate preparation manganese carbonate device from manganese-containing waste water is related to.
Background
With the development of new energy automobiles, the anode material of the manganese lithium ion battery provides higher requirements for manganese sources such as manganese sulfate and the like. Certain impurities in the manganese source can affect the morphology of the battery material and the performance of the battery, so the battery-grade manganese sulfate industry standard (HG/T4823-2015) puts higher requirements on the content of each impurity.
The production of titanium dioxide by adopting a sulfuric acid method is accompanied with the production of manganese-containing inorganic salt wastewater, and the wastewater has high contents of manganese ions, ammonium ions, calcium ions, magnesium ions and other ions. It needs to be recycled by waste water.
Disclosure of Invention
In order to solve the technical problem, the utility model provides a separate preparation manganese carbonate device from manganese-containing waste water, realize resource utilization to waste water edulcoration processing.
The utility model discloses a scheme:
the device for separating and preparing manganese carbonate from manganese-containing wastewater comprises a first impurity removal tank, wherein the first impurity removal tank is communicated with a feeding port of a first filter through a pipeline, the filtrate discharge port of the first filter is communicated with a first filtrate collecting tank, the first filtrate collecting tank is communicated with a second impurity removing tank and a second filter in sequence through pipelines, the filtrate discharge port of the second filter is communicated with a second filtrate collecting tank, the second filtrate collecting tank is communicated with a third impurity removing tank and a third filter in sequence through pipelines, the filtrate discharge port of the third filter is communicated with a third filtrate collecting tank, the third filtrate collecting tank is communicated with a fourth impurity removing tank and a fourth filter in sequence through pipelines, and the filtrate discharge port of the fourth filter is communicated with a fourth filtrate collecting tank, and the fourth filtrate collecting tank is sequentially communicated with the fifth impurity removing tank and the fifth filter through pipelines.
Preferably, the first filter, the second filter, the third filter, the fourth filter and the fifth filter are belt vacuum filters.
Further preferably, the filter residue discharge port of the first filter is communicated with the hydroxide recovery tank, the filter residue discharge port of the second filter is communicated with the heavy metal recovery tank, the filter residue discharge port of the third filter is communicated with the first insoluble calcium and magnesium precipitation recovery tank, the filter residue discharge port of the fourth filter is communicated with the second insoluble calcium and magnesium precipitation recovery tank, and the filter residue discharge port of the fifth filter is communicated with the manganese carbonate recovery tank.
Further preferably, a washing water feeding pipe of the fifth filter is respectively communicated with the deionized water pipeline and the absolute ethyl alcohol pipe.
Preferably, first edulcoration jar pan feeding mouth communicates respectively with hydrogen peroxide jar and aqueous ammonia jar through the pipeline, second edulcoration jar pan feeding mouth communicates with ammonium sulfate solution jar through the pipeline, fourth edulcoration jar pan feeding mouth communicates with ammonium fluoride solution jar through the pipeline, fifth edulcoration jar pan feeding mouth communicates with ammonium bicarbonate solution jar through the pipeline.
Preferably, the second impurity removing tank tail gas discharge pipe is communicated with the alkali liquor absorption tank.
The utility model discloses beneficial effect:
1. the utility model discloses carry out edulcoration purification treatment to the manganese-containing waste water that produces in the titanium dioxide production process, carry out resource utilization.
2. The utility model discloses an iron, aluminium ion are got rid of in hydrolysis method precipitation, and heavy metal ion, heating concentration and ammonium fluoride combination precipitation are got rid of calcium magnesium ion to the ammonium sulfide, and the later stage adopts and adds surfactant dodecyl benzene sulfonic acid sodium, and the manganese carbonate of purification is spherical, the surface is smooth and dispersion effect is good. Wherein the precipitation rate of iron and aluminum in the wastewater is 99.56-99.87%, the precipitation rate of calcium and magnesium ions is 99.87%, and the precipitation rate of manganese is 99.89%. The manganese content in the final product is 52.5%, the calcium content and the magnesium content are 0.21% and 0.01% respectively, and the quality standard of industrial manganese carbonate is achieved.
3. First washing water collecting vat, second washing water collecting vat and third washing water collecting vat are equipped with a plurality of from top to bottom respectively, and below washing water collecting vat size is greater than top washing water collecting vat size, spills over through stewing and retrieves the washing water, also retrieves again after carrying out purification treatment to the washing water simultaneously.
4. The first filter, the second filter, the third filter, the fourth filter and the fifth filter are belt vacuum filters, filtrate and filter residues are separated, and meanwhile, the filter residues can be cleaned and recovered.
5. And a washing water feeding pipe of the fifth filter is respectively communicated with the deionized water pipeline and the absolute ethyl alcohol pipe, and the final product of manganese carbonate is washed and recovered.
6. And the tail gas discharge pipe of the second impurity removal tank is communicated with the alkali liquor absorption tank, so that the generated tail gas is recycled and discharged, and the pollution to the environment is reduced.
7. Washing the filter residue on the first filter with washing water, and recycling ferric hydroxide and aluminum hydroxide from the filter residue in a hydroxide recycling tank; washing the filter residue filtered by the second filter with washing water, and recycling Ni from the filter residue in a heavy metal recycling tank2+、Cr3+、Cu2+Heavy metal ions of equal weight; washing the filter residue of the third filter, and feeding the filter residue into a first insoluble calcium and magnesium precipitate recovery tank to recover insoluble calcium and magnesium precipitates and the like; washing the filter residue of the fourth filter, and feeding the filter residue into a second insoluble calcium and magnesium precipitate recovery tank to further recover insoluble calcium and magnesium precipitate; and washing filter residues of the fifth filter, and feeding the filter residues into a manganese carbonate tank to recover manganese carbonate.
Drawings
FIG. 1 is a schematic view of the system of the present invention;
wherein: the device comprises a first impurity removing tank 1, a first filter 2, a first filtrate collecting tank 3, a second impurity removing tank 4, a second filter 5, a second filtrate collecting tank 6, a third impurity removing tank 7, a third filter 8, a third filtrate collecting tank 9, a fourth impurity removing tank 10, a fourth filter 11, a fourth filtrate collecting tank 12, a fifth impurity removing tank 13, a fifth filter 14, a deionized water pipeline 1401, an anhydrous ethanol pipe 1402, a hydroxide recovering tank 15, a heavy metal recovering tank 16, a first insoluble calcium and magnesium precipitate recovering tank 17, a second insoluble calcium and magnesium precipitate recovering tank 18, a manganese carbonate tank recovering tank 19, a hydrogen peroxide tank 20, an ammonia tank 21, an ammonium sulfate solution tank 22, an ammonium fluoride solution tank 23, an ammonium bicarbonate solution tank 24 and an alkali solution absorption tank 25.
Detailed Description
The invention is further described with reference to the following examples, but the scope of the invention as claimed is not limited to the scope of the examples.
Example 1
As shown in figure 1, the device for separating and preparing manganese carbonate from manganese-containing wastewater comprises a first impurity removal tank 1, wherein the first impurity removal tank 1 is communicated with a feeding port of a first pipeline filter 2, the filtrate discharge port of the first filter 2 is communicated with a first filtrate collecting tank 3, the first filtrate collecting tank 3 is communicated with a second impurity removing tank 4 and a second filter 5 in sequence through pipelines, the filtrate discharge port of the second filter 5 is communicated with a second filtrate collecting tank 6, the second filtrate collecting tank 6 is communicated with a third impurity removing tank 7 and a third filter 8 in sequence through pipelines, the filtrate discharge port of the third filter 8 is communicated with a third filtrate collecting tank 9, the third filtrate collecting tank 9 is communicated with a fourth impurity removing tank 10 and a fourth filter 11 in sequence through pipelines, and a filtrate discharge port of the fourth filter 11 is communicated with a fourth filtrate collecting tank 12, and the fourth filtrate collecting tank 12 is sequentially communicated with a fifth impurity removing tank 13 and a fifth filter 14 through pipelines.
Preferably, the first filter 2, the second filter 5, the third filter 8, the fourth filter 11 and the fifth filter 14 are belt vacuum filters.
Further preferably, the filter residue discharge port of the first filter 2 is communicated with the hydroxide recovery tank 15, the filter residue discharge port of the second filter 5 is communicated with the heavy metal recovery tank 16, the filter residue discharge port of the third filter 8 is communicated with the first insoluble calcium and magnesium precipitation recovery tank 17, the filter residue discharge port of the fourth filter 11 is communicated with the second insoluble calcium and magnesium precipitation recovery tank 18, and the filter residue discharge port of the fifth filter 14 is communicated with the manganese carbonate recovery tank 19.
Further preferably, the washing water inlet pipe of the fifth filter 14 is respectively communicated with the deionized water pipe 1401 and the anhydrous ethanol pipe 1402.
Preferably, the pan feeding mouth of the first impurity removing tank 1 is respectively communicated with the hydrogen peroxide tank 20 and the ammonia tank 21 through pipelines, the pan feeding mouth of the second impurity removing tank 4 is communicated with the ammonium sulfate solution tank 22 through a pipeline, the pan feeding mouth of the fourth impurity removing tank 10 is communicated with the ammonium fluoride solution tank 23 through a pipeline, and the pan feeding mouth of the fifth impurity removing tank 13 is communicated with the ammonium hydrogen carbonate solution tank 24 through a pipeline.
Preferably, the tail gas discharge pipe of the second impurity removing tank 4 is communicated with the alkali liquor absorption tank 25.
The utility model discloses during the use:
1) titanium dioxide wastewater is added into a first impurity removal tank 1 according to n (Fe)2+): n (hydrogen peroxide) = (2-3): 1, adding hydrogen peroxide to ensure that ferrous ions in the wastewater are completely oxidized into ferric ions, then adding ammonia water to adjust the pH value to 5-6, and reacting for 0.8-1.2h at 85-95 ℃ until Fe3+、Al3+Completely forming precipitate, and filtering the mixture in a first filter 2 to obtain filtrate and filter residue;
2) filtering in a first filter 2 to obtain filtrate, adding into a second impurity removing tank 4, adding (NH)4)2S solution, reacting for 2h at 60 ℃ to enable Ni in wastewater2+、Cr3+、Cu2+Precipitating the heavy metal ions completely in the form of sulfide, and filtering in a second filter 5 to obtain filtrate and filter residue, wherein the tail gas generated in the second impurity removal tank 4 is absorbed by sodium hydroxide lye;
3) filtering with the second filter 5 to obtain filtrate, feeding into a third impurity removing tank 7, heating until flocculent substance is separated out, stopping heating, cooling to room temperature, feeding into a third filter 8, and filtering to obtain filtrate and filter residue;
4) filtering with a third filter 8 to obtain filtrate, feeding into a fourth impurity removing tank 10, placing at 85-95 deg.C and pH =5-6, adding ammonium fluoride to precipitate Ca2+，Mg2+Filtering in a fourth filter 11 to obtain filtrate and filter residue, and filtering in the fourth filter 11 to obtain filtrate which is crude manganese sulfate concentrated mother liquor;
5) the crude manganese sulfate concentrated mother liquor obtained by filtering with the fourth filter 11 enters a fifth impurity removing tank 13 according to the proportion of n (SDS): n (Mn)2+) Adding a surfactant SDS into the manganese-rich mother liquor in a ratio of =0.043-0.046:1, heating in a water bath to 25-35 ℃, adding 1mol/L ammonium bicarbonate solution, stirring for 20min, aging the whole system in a water bath at 45 ℃ for 1.5-2.5h, and filtering in a fifth filter 14 to obtain filtrate and filter residue; fifth filteringAnd washing filter residue of the machine 14 for several times by using deionized water until no turbidity appears after a barium chloride solution with the mass fraction of 5% is added into the washing liquid. Washing the filter cake with absolute ethyl alcohol for 3-4 times to obtain the product of manganese carbonate.
Wherein, the filter residue on the first filter 2 is washed by washing water, and the filter residue enters a hydroxide recovery tank 15 to recover ferric hydroxide and aluminum hydroxide; washing the filter residue filtered by the second filter 5 with washing water, and recycling Ni from the filter residue in a heavy metal recycling tank 162+、Cr3+、Cu2+Heavy metal ions of equal weight; washing the filter residue of the third filter 8, and feeding the filter residue into a first insoluble calcium and magnesium precipitate recovery tank 17 to recover insoluble calcium and magnesium precipitates and the like; washing the filter residue of the fourth filter 11, and further recovering insoluble calcium and magnesium precipitates in a second insoluble calcium and magnesium precipitate recovery tank 18; and washing filter residues of the fifth filter 14, and feeding the filter residues into a manganese carbonate tank recovery tank 19 to recover manganese carbonate.
Claims (6)
1. From containing manganese waste water separation preparation manganese carbonate device, including first edulcoration jar (1), its characterized in that: the first impurity removing tank (1) is communicated with a feeding port of the first filter (2) through a pipeline, a filtrate discharging port of the first filter (2) is communicated with a first filtrate collecting tank (3), the first filtrate collecting tank (3) is sequentially communicated with a second impurity removing tank (4) and a second filter (5) through pipelines, a filtrate discharging port of the second filter (5) is communicated with a second filtrate collecting tank (6), the second filtrate collecting tank (6) is sequentially communicated with a third impurity removing tank (7) and a third filter (8) through pipelines, a filtrate discharging port of the third filter (8) is communicated with a third filtrate collecting tank (9), the third filtrate collecting tank (9) is sequentially communicated with a fourth impurity removing tank (10) and a fourth filter (11) through pipelines, a filtrate discharging port of the fourth filter (11) is communicated with a fourth filtrate collecting tank (12), and the fourth filtrate collecting tank (12) is sequentially communicated with the fifth impurity removing tank (13) and the fifth filter (14) through pipelines.
2. The apparatus for separating and preparing manganese carbonate from manganese-containing wastewater according to claim 1, wherein: the first filter (2), the second filter (5), the third filter (8), the fourth filter (11) and the fifth filter (14) are belt type vacuum filters.
3. The apparatus for separating and preparing manganese carbonate from manganese-containing wastewater according to claim 2, wherein: the filter residue discharge gate and the hydroxide recovery jar (15) of first filter (2) communicate, the filter residue discharge gate and the heavy metal recovery jar (16) intercommunication of second filter (5), the filter residue discharge gate and the first insoluble calcium magnesium of third filter (8) deposit recovery jar (17) intercommunication, the filter residue discharge gate and the second insoluble calcium magnesium of fourth filter (11) deposit recovery jar (18) intercommunication, and the filter residue discharge gate and the manganese carbonate jar recovery jar (19) intercommunication of fifth filter (14).
4. The apparatus for separating and preparing manganese carbonate from manganese-containing wastewater according to claim 2, wherein: and a washing water feeding pipe of the fifth filter (14) is respectively communicated with a deionized water pipeline (1401) and an absolute ethyl alcohol pipe (1402).
5. The apparatus for separating and preparing manganese carbonate from manganese-containing wastewater according to claim 1, wherein: first edulcoration jar (1) pan feeding mouth communicates respectively through pipeline and hydrogen peroxide jar (20) and aqueous ammonia jar (21), second edulcoration jar (4) pan feeding mouth communicates through pipeline and ammonium sulfate solution jar (22), fourth edulcoration jar (10) pan feeding mouth communicates through pipeline and ammonium fluoride solution jar (23), fifth edulcoration jar (13) pan feeding mouth communicates through pipeline and ammonium hydrogen carbonate solution jar (24).
6. The apparatus for separating and preparing manganese carbonate from manganese-containing wastewater according to claim 1, wherein: and the tail gas discharge pipe of the second impurity removal tank (4) is communicated with the alkali liquor absorption tank (25).
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201921471571.8U CN210559435U (en) | 2019-09-05 | 2019-09-05 | Device for separating and preparing manganese carbonate from manganese-containing wastewater |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201921471571.8U CN210559435U (en) | 2019-09-05 | 2019-09-05 | Device for separating and preparing manganese carbonate from manganese-containing wastewater |
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| CN210559435U true CN210559435U (en) | 2020-05-19 |
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| CN201921471571.8U Active CN210559435U (en) | 2019-09-05 | 2019-09-05 | Device for separating and preparing manganese carbonate from manganese-containing wastewater |
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