CN115231647A - Recovery method of back extraction waste acid - Google Patents
Recovery method of back extraction waste acid Download PDFInfo
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- CN115231647A CN115231647A CN202210889130.XA CN202210889130A CN115231647A CN 115231647 A CN115231647 A CN 115231647A CN 202210889130 A CN202210889130 A CN 202210889130A CN 115231647 A CN115231647 A CN 115231647A
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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/26—Treatment of water, waste water, or sewage by extraction
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2303/00—Specific treatment goals
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Abstract
The invention provides a method for recovering back extraction waste acid, and relates to the technical field of wastewater treatment. The invention uses trioctyl decyl tertiary amine and sulfonated kerosene as extracting agents (namely organic phase) to carry out countercurrent extraction on the iron-containing back extraction waste acid, and the concentration of iron in the recovered back extraction acid<0.01g/L, the removal rate of iron impurities is more than 99.5 percent, the iron content is low, the recovered strip acid can be recycled, and the back-extraction section of hydrometallurgy, especially P, is reduced 507 The consumption of acid in the back extraction section of the extraction system greatly reduces the production cost. Moreover, the recovery method provided by the invention is simple to operate, low in cost, safe and environment-friendly. Furthermore, the regenerated extractant obtained after the back extraction of the iron-containing extractant by the back extractant can be recycled, so that the continuous treatment of the iron-containing back extraction waste acid can be realized, and the treatment cost of the iron-containing back extraction waste acid is low.
Description
Technical Field
The invention relates to the technical field of wastewater treatment, in particular to a method for recovering back extraction waste acid.
Background
The vast majority of high-purity single rare earth elements are separated and prepared by a solvent extraction method, and the raw material source of the rare earth elements mainly comprises bastnaesite-monazite mixtureRaw ores such as composite rare earth ore, ionic rare earth ore and bastnaesite, and secondary resource rare earth ores such as neodymium iron boron waste, fluorescent powder waste, catalyst waste and smelting slag. In hydrometallurgy, where the metal mineral is leached with an acidic solution, the iron is usually in the form of Fe 2+ And Fe 3+ The form and the valuable metal enter the solution together, and the iron ions have strong hydrolysis tendency and are easy to form complexes with other ions, so that the existing form of the iron in an aqueous solution or a solvent extraction system is very complicated, the iron impurities are difficult to remove when the valuable metal is separated, and the iron inevitably enters the rare earth feed liquid.
In the process of separating rare earth elements by a solvent extraction method, thousands of stages of extraction tanks are generally adopted to realize rare earth element separation by a fuzzy extraction process. When extracting rare earth feed liquid containing iron impurities, the equilibrium acidity of the extraction system is low (pH value is 1-3), and iron is Fe 3+ Form and RE 3+ Is covered with P together 507 Extracting into organic phase, and back extracting rare earth with high acid due to iron ion and extractant P 507 The larger affinity between the iron ions and the rare earth ions leads to that the iron ions are easier to extract and harder to reverse than the rare earth ions, so that the rare earth is reversely extracted into the water phase in the reverse extraction stage, the iron ions can be reversely extracted into the water phase by high acid after the iron ions are more than the rare earth ions, and the iron ions are continuously enriched before the reverse extraction, thus leading to P in the organic phase 507 The extractant loses the extraction capability, and meanwhile, the system is easy to have emulsification phenomenon, thereby influencing the phase splitting effect of the extraction system, causing resource waste and increasing the production cost.
At present, aiming at the phenomenon of iron element enrichment in the process of rare earth extraction and separation, in order to avoid organic phase emulsification without influencing the quality of back extraction products, a 'back ferrite' discharge port is usually arranged at a back extraction section to discharge the iron element enriched in a system, but a large amount of back extraction waste acid is discharged at the same time, so that the consumption of back extraction hydrochloric acid is greatly increased, and no report about a recovery method of the discharged iron-containing back extraction waste acid exists at present.
Disclosure of Invention
In view of the above, the present invention aims to provide a method for recovering spent acid from stripping, wherein the recovered stripping acid obtained by the recovery method provided by the present invention has low iron impurity content, and the recovered stripping acid can be recycled in the stripping section.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a method for recovering back extraction waste acid, which comprises the following steps:
carrying out countercurrent extraction on the iron-containing back extraction waste acid by using an extracting agent to obtain recovered back extraction acid and an iron-containing extracting agent; the extracting agent is trioctyl decyl tertiary amine and sulfonated kerosene.
Preferably, the flow ratio of the iron-containing stripping waste acid to the extractant is 1: (5-10).
Preferably, the volume fraction of the trioctyl decyl tertiary amine in the extractant is 20 to 30 percent.
Preferably, the iron-containing spent acid comprises spent acid from the hydrometallurgical industry.
Preferably, the extraction stage number of the countercurrent extraction is 6 to 10.
Preferably, in the countercurrent extraction process, the iron-containing back extraction waste acid and the extractant have the same sample injection level, and the sample injection level is 2 nd to 4 th.
Preferably, the countercurrent extraction comprises mixing and standing clarification in sequence;
the mixing time is 1-8 min;
the standing and clarifying time is 3-20 min.
Preferably, the countercurrent extraction is followed by extractant regeneration, which comprises the following steps: and performing back extraction on the iron-containing extractant by using a back extractant to obtain a regenerated extractant and iron-containing wastewater.
Preferably, the stripping agent is water.
Preferably, the sample injection level of the stripping agent is 7 th to 9 th.
The invention provides a method for recovering back extraction waste acid, which comprises the following steps: carrying out countercurrent extraction on the iron-containing back extraction waste acid by using an extracting agent to obtain recovered back extraction acid and an iron-containing extracting agent; the extracting agent is trioctyl decyl tertiary amine and sulfonated kerosene. The invention uses trioctyl decyl tertiary amine and sulfonationThe kerosene is used as an extracting agent (namely an organic phase) to carry out countercurrent extraction on the iron-containing back extraction waste acid, and the concentration of iron in the obtained recovered back extraction acid (namely the raffinate)<0.01g/L, the removal rate of iron impurities is more than 99.5 percent, the iron content is low, the recovered back extraction acid can be recycled, and the back extraction section of hydrometallurgy, especially P, is reduced 507 The consumption of acid in the back extraction section of the extraction system greatly reduces the production cost. Moreover, the recovery method provided by the invention is simple to operate, low in cost, safe and environment-friendly.
Furthermore, the regenerated extractant obtained after the back extraction of the iron-containing extractant by the back extractant can be recycled, so that the continuous treatment of the iron-containing back extraction waste acid can be realized, and the treatment cost of the iron-containing back extraction waste acid is low.
Drawings
FIG. 1 is a schematic diagram of a counter-current extraction flow.
Detailed Description
The invention provides a method for recovering back extraction waste acid, which comprises the following steps:
carrying out countercurrent extraction on the iron-containing back extraction waste acid by using an extracting agent to obtain recovered back extraction acid and an iron-containing extracting agent; the extracting agent is trioctyl decyl tertiary amine and sulfonated kerosene. The concentration of iron in the recovered stripping acid is less than 0.01g/L.
In the present invention, all the raw material components are commercially available products well known to those skilled in the art unless otherwise specified.
In the present invention, the iron-containing spent acid preferably comprises spent acid from the hydrometallurgical industry, more preferably comprises P 507 And (4) back extracting the iron-containing waste acid. In the invention, the concentration of acid in the back-extraction iron-containing waste acid generated by the hydrometallurgy industry is preferably 5-6 mol/L; the content of iron in the back extraction iron-containing waste acid generated by the hydrometallurgical industry is preferably 2-10 g/L, and more preferably 4-8 g/L.
In the present invention, trioctyl decyl tertiary amine (N) is contained in the extractant 235 ) The volume fraction (b) is preferably 20 to 30%, more preferably 25 to 30%.
In the present invention, the flow ratio of the iron-containing spent stripping acid to the extractant is preferably 1: (5 to 10), more preferably 1: (6 to 9), more preferably 1: (7 to 8).
In the present invention, the number of extraction stages of the countercurrent extraction is preferably 6 to 10, more preferably 7 to 9, and still more preferably 8; the countercurrent extraction is preferably carried out using a countercurrent extraction tank. In the invention, in the countercurrent extraction process, the sample injection stages of the iron-containing back extraction waste acid and the extractant are preferably the same, and the sample injection stage is preferably the 2 nd to 4 th stage, and more preferably the 3 rd stage. In the present invention, each stage of the countercurrent extraction tank is preferably provided with a mixing chamber and a clarification chamber.
In the present invention, the countercurrent extraction preferably comprises mixing and standing clarification in this order. In the present invention, the temperature of the mixing is preferably room temperature, and the time of the mixing is preferably 1 to 8min, more preferably 2 to 7min, and further preferably 3 to 6min. In the present invention, the temperature of the standing clarification is preferably room temperature, and the time of the standing clarification is preferably 3 to 20min, more preferably 5 to 18min, and further preferably 8 to 15min. In the invention, the affinity of the extractant for iron ions is greater than that for hydrogen ions in the countercurrent extraction process, so that the iron ions enter an extraction organic phase, and the hydrogen ions enter a water phase to realize the effective separation of the iron ions and the hydrogen ions.
In the invention, the recovered strip acid flows out from the 1 st stage of the countercurrent extraction box, and the obtained recovered strip acid can be reused in the strip process of hydrometallurgy.
In the present invention, the countercurrent extraction preferably further comprises an extractant regeneration, and the extractant regeneration comprises the following steps: and performing back extraction on the iron-containing extractant by using a back extractant to obtain a regenerated extractant and iron-containing wastewater. In the present invention, the stripping agent is preferably water. In the invention, the sample injection level of the stripping agent is preferably 7 to 9 levels, and more preferably 7 to 8 levels; the iron-containing wastewater obtained by the back extraction preferably flows out from the 5 th to the 7 th stages of the countercurrent extraction box; the regenerated extractant is preferably returned from the uppermost stage of the countercurrent extraction tank for use in the countercurrent extraction process. In the present invention, the flow ratio of the iron-containing stripping waste acid to the stripping agent is preferably 1: (2 to 5), more preferably 1: (2-3).
The method for recovering the strip acid is described in the following by combining a counter-current extraction flow chart shown in figure 1, and comprises the following specific steps: the method comprises the following steps of (1) enabling iron-containing back extraction waste acid and an extracting agent to enter from the 3 rd stage of a countercurrent extraction box, mixing in a mixing chamber, allowing the waste acid and the extracting agent to flow into a clarification chamber, standing and clarifying to obtain a back extraction acid aqueous phase (namely, recovered back extraction acid) and an iron-containing extraction organic phase (namely, an iron-containing extracting agent), wherein the back extraction acid aqueous phase flows to the 1 st stage and flows out from the 1 st stage, and the iron-containing extraction organic phase flows from the 3 rd stage to the 8 th stage; and the stripping agent enters from the 7 th stage and performs stripping on the iron-containing extraction organic phase to obtain iron-containing wastewater and a regenerated organic phase (regenerated extracting agent), wherein the iron-containing wastewater flows out of the 6 th stage, the regenerated organic phase flows to the 8 th stage and flows out of the 8 th stage, and then the iron-containing wastewater flows back to the 3 rd stage of the countercurrent extraction tank from the 3 rd stage for recycling.
The technical solution of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. It is to be understood that the described embodiments are merely exemplary of the invention, and not restrictive of the full scope of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
The back extraction waste acid is recovered by adopting a counter-current extraction flow chart shown in figure 1.
The iron-containing back-extraction waste acid is industrial P 507 And iron-containing back extraction waste acid generated in the back extraction section of the extraction system, wherein the content of Fe is 2g/L, and the acid concentration is 5.16mol/L.
The iron-containing back extraction waste acid (feed flow rate 5L/min) and the extractant (30 v/v% N) 235 +70v/v% sulfonated kerosene) was fed from stage 3 of the countercurrent extraction tank at a flow ratio of 1. Water (with feed flow of 6L/min) flows from stage 7 to stage 6, and the iron-containing extraction organic phase is subjected to back extraction to obtain iron-containing wastewater (flowing out from stage 5) and regenerated organic phase (flowing out from stage 8 and flowing back from stage 3 to countercurrentRecycled in the extraction tank).
The iron-containing back extraction waste acid, the recovered back extraction acid, and the acid concentration and iron ion concentration in the iron-containing waste water are shown in table 1:
TABLE 1 iron-containing stripping waste acid material content
| Item | Acid concentration (mol/L) | Fe concentration (g/L) |
| Spent acid containing iron | 5.16 | 2 |
| Recovering the stripping acid | 5.07 | <0.01 |
| Iron-containing wastewater | 0.8 | 9.8 |
| Difference of iron content | / | ＞1.99 |
| Iron removal rate | / | ＞99.5％ |
As can be seen from Table 1, the recovered strip acid obtained by the recovery method provided by the invention has Fe content of less than 0.01g/L, fe removal rate of more than 99.5%, obvious impurity removal effect and can be recycled.
Example 2
The process of example 1 was followed to produce a recovered strip acid, differing from example 1 only in that the spent iron-containing strip acid had an Fe content of 3.5g/L and an acid concentration of 5.47mol/L; the feed flow of the iron-containing back extraction waste acid is 4.5L/min; the flow ratio of the iron-containing back extraction waste acid to the extractant is 1; stirring and mixing for 4min; standing and clarifying for 10min; the feed rate of water was 7L/min.
The iron-containing back extraction waste acid, the recovered back extraction acid, and the acid concentration and iron ion concentration in the iron-containing waste water are shown in table 2:
TABLE 2 iron-containing stripping waste acid material content
| Item | Acid concentration (mol/L) | Fe concentration (g/L) |
| Spent acid containing iron back extraction | 5.47 | 3.5 |
| Recovery of stripping acid | 5.32 | <0.01 |
| Iron-containing wastewater | 0.74 | 16.5 |
| Difference of iron content | / | ＞3.49 |
| Iron removal rate | / | ＞99.71 |
As can be seen from Table 2, the recovered strip acid obtained by the recovery method provided by the invention has the Fe content of less than 0.01g/L, the Fe removal rate of more than 99.71%, the impurity removal effect is obvious, and the recovered strip acid can be recycled.
Example 3
The recovered strip acid was prepared according to the method of example 1, differing from example 1 only in that iron-containing strip waste acid in which the Fe content was 4.78g/L and the acid concentration was 5.39mol/L; the feed flow of the iron-containing back extraction waste acid is 4L/min; the flow ratio of the iron-containing back extraction waste acid to the extracting agent is 1; stirring and mixing for 5min; standing and clarifying for 12min; the feed rate of water was 6L/min.
The iron-containing spent acid from the back extraction, the recovered back-extracted acid, and the acid concentration and iron ion concentration in the iron-containing wastewater are shown in table 3:
TABLE 3 iron-containing stripping waste acid material content
| Item | Acid concentration (mol/L) | Fe concentration (g/L) |
| Spent acid containing iron back extraction | 5.39 | 4.78 |
| Recovering the stripping acid | 5.24 | <0.01 |
| Iron-containing wastewater | 0.6 | 23.8 |
| Difference of iron content | / | ＞4.77 |
| Iron removal rate | / | ＞99.79 |
As can be seen from Table 3, the recovered strip acid obtained by the recovery method provided by the invention has the Fe content of less than 0.01g/L, the Fe removal rate of more than 99.79 percent, the impurity removal effect is obvious, and the recovered strip acid can be recycled.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and amendments can be made without departing from the principle of the present invention, and these modifications and amendments should also be considered as the protection scope of the present invention.
Claims (10)
1. A method for recovering back extraction waste acid comprises the following steps:
carrying out countercurrent extraction on the iron-containing back extraction waste acid by using an extracting agent to obtain recovered back extraction acid and an iron-containing extracting agent; the extracting agent is trioctyl decyl tertiary amine and sulfonated kerosene.
2. The recovery method of claim 1, wherein the flow ratio of the iron-containing spent stripping acid to the extractant is 1: (5-10).
3. The recovery method according to claim 1 or 2, wherein the volume fraction of the trioctyl-decyl tertiary amine in the extractant is 20 to 30%.
4. The recovery process of claim 1 or 2, wherein the iron-containing spent acid comprises spent acid from the hydrometallurgical industry for stripping iron.
5. The recovery method according to claim 1, wherein the number of extraction stages of the countercurrent extraction is 6 to 10.
6. The recycling method according to claim 5, wherein in the countercurrent extraction process, the iron-containing spent acid from the back extraction and the extractant are fed at the same level, and the feeding level is 2 to 4.
7. The recovery method according to claim 1, wherein the countercurrent extraction comprises mixing and standing clarification in this order;
the mixing time is 1-8 min;
the standing and clarifying time is 3-20 min.
8. The recovery process of claim 1, further comprising extractant regeneration after the counter-current extraction, the extractant regeneration comprising the steps of: and performing back extraction on the iron-containing extractant by using a back extractant to obtain a regenerated extractant and iron-containing wastewater.
9. The recovery process of claim 9, wherein the stripping agent is water.
10. The recovery method according to claim 8 or 9, wherein the injection grade of the stripping agent is 7 th to 9 th.
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| CN110844963A (en) * | 2019-11-21 | 2020-02-28 | 神华准能资源综合开发有限公司 | Method for separating and recovering aluminum-containing high-iron-salt-acid wastewater |
| CN113120941A (en) * | 2019-12-31 | 2021-07-16 | 中冶瑞木新能源科技有限公司 | Method for extracting high-purity scandium oxide from scandium-containing nickel cobalt hydroxide in short process |
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2022
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| JPS62247884A (en) * | 1986-04-18 | 1987-10-28 | Kurita Water Ind Ltd | Treatment of iron ion-containing liquid |
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