CN110551895A - Separation method of aged P 507 - Google Patents

Separation method of aged P 507 Download PDF

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Publication number
CN110551895A
CN110551895A CN201810564717.7A CN201810564717A CN110551895A CN 110551895 A CN110551895 A CN 110551895A CN 201810564717 A CN201810564717 A CN 201810564717A CN 110551895 A CN110551895 A CN 110551895A
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CN
China
Prior art keywords
aged
separating
extractant
saponified
liquid
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Pending
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CN201810564717.7A
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Chinese (zh)
Inventor
许开华
张爱青
李炳忠
乔少华
伍一根
许东伟
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Grammy (jiangsu) Cobalt Industry Ltd By Share Ltd
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Grammy (jiangsu) Cobalt Industry Ltd By Share Ltd
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Application filed by Grammy (jiangsu) Cobalt Industry Ltd By Share Ltd filed Critical Grammy (jiangsu) Cobalt Industry Ltd By Share Ltd
Priority to CN201810564717.7A priority Critical patent/CN110551895A/en
Publication of CN110551895A publication Critical patent/CN110551895A/en
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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
    • C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
    • C22B3/26—Treatment or purification of solutions, e.g. obtained by leaching by liquid-liquid extraction using organic compounds
    • C22B3/38—Treatment or purification of solutions, e.g. obtained by leaching by liquid-liquid extraction using organic compounds containing phosphorus
    • C22B3/384—Pentavalent phosphorus oxyacids, esters thereof
    • C22B3/3846—Phosphoric acid, e.g. (O)P(OH)3

Abstract

The invention discloses a separation method of aged P 507, which is realized by the following steps of 1, adding a P 507 extracting agent into liquid alkali, stirring and reacting to obtain a saponified P 507 extracting agent, 2, adding a purifying liquid into a saponified P 507 extracting agent obtained in the step 1, extracting and separating to obtain a P 507 saturated organic matter, and 3, adding activated clay into a P 507 saturated organic matter obtained in the step 2, filtering to obtain aged P 507.

Description

separation method of aged P 507
Technical Field
The invention belongs to the technical field of P 507 regeneration, and particularly relates to a separation method of aged P 507.
Background
P 507 is the most common extractant for industrially separating mixed rare earth, when in actual use, an organic phase is usually formed by P 507 kerosene or sulfonated kerosene, because the P507 organic phase is continuously and periodically recycled, the P507 in the organic phase inevitably changes gradually to generate an aging phenomenon, after the aging P 507 is mixed with the normal P507, the aging P 507 is continuously dissolved back into water from solvent oil in the extraction process, so that the organic components of the extracted aqueous solution are increased, the COD is higher, the viscosity of the whole extractant is increased, the phase separation time is increased in the extraction process, and liquid alkali is consumed in saponification, so that the production cost is increased.
disclosure of Invention
In view of the above, the main objective of the present invention is to provide a method for separating aged P 507, which solves the problems of the prior art that the COD is higher and the extraction cost is high due to the increase of organic components in the extracted aqueous solution.
In order to achieve the aim, the technical scheme of the invention is realized by a separation method of aged P 507, which comprises the following steps:
Step 1, adding a P 507 extractant into liquid caustic soda, and stirring for reaction to obtain a saponified P 507 extractant;
step 2, adding a purified liquid into the saponified P 507 extracting agent obtained in the step 1, extracting and separating to obtain a P 507 saturated organic matter;
And 3, adding activated clay into the P 507 saturated organic matter obtained in the step 2, and filtering to obtain aged P 507.
In the step 1, the P 507 volume percent of the P 507 extractant is 25-30%, and the solvent oil volume percent is 70-75%.
Preferably, the mass ratio of the aged P 507 to the normal P 507 in the P 507 is 1 (2-4).
Preferably, in the step 1, 30-32% of liquid alkali is used for saponification of the P 507.
Preferably, the solvent oil in the step 1 is at least one of No. 260 solvent oil and No. 300 solvent oil.
Preferably, in the step 1, the reaction time is 3-5 min.
preferably, in the step 2, the purifying liquid is iron-removing purifying liquid; the iron-removing purification liquid comprises 50-70 g/L, Cu 2-2 g/L, Mn 10-20 g/L, Ca 0.2-0.8 g/L of Co, and the rest metal ions are less than 0.5 g/L.
Preferably, in the step 2, the extraction time is 20-30 min.
preferably, in the step 3, the mass of the activated clay added is 5-10 of the mass of the aged P 507 raffinate.
Preferably, in the step 3, the activated clay comprises, by weight, 60-65% of SiO 2 60, 15-20% of Al 2 O 3 15, 1-5% of Fe 2 O 3 1, 0.1-0.2% of FeO, 0.1-0.2% of TiO, 2-3% of CaO, 5-7% of MgO, 0.1-0.3% of MnO, 0.7-0.9% of K 2 O, 0.1-0.3% of Na 2 O, and 0.01-0.05% of P 2 O 5 0.01.
Compared with the prior art, the method has the advantages that the aged P 507 in the P 507 extractant is separated, the extraction rate of cobalt is effectively improved, the consumption of liquid caustic soda is greatly reduced, organic components of an extracted aqueous solution are reduced, COD (chemical oxygen demand) is reduced, the viscosity of the whole extractant is reduced in the extraction process, and accordingly the phase separation time is greatly shortened.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
The invention provides a separation method of aged P 507, which is realized by the following steps:
Step 1, adding a P 507 extractant (wherein the volume percentage of P 507 in the P 507 extractant is 25-30%, the volume percentage of solvent oil is 70-75%, and the mass ratio of aged P 507 to normal P 507 in P 507 is 1 (2-4)) into liquid alkali, and stirring for reaction for 3-5min to obtain a saponified P 507 extractant;
Wherein 30-32% liquid alkali is adopted to saponify P 507 during saponification, and the solvent oil is at least one of No. 260 solvent oil and No. 300 solvent oil;
And 2, adding an iron-removing purification solution into the saponified P 507 extraction agent obtained in the step 1, extracting for 20-30 min, and separating cobalt to obtain a P 507 saturated organic matter, wherein the iron-removing purification solution comprises 50-70 g/L, Cu 2-8 g/L, Mn 10-20 g/L, Ca 0.2.2-0.8 g/L of Co, and the rest metal ions are less than 0.5 g/L.
step 3, adding activated clay with the mass of 5-10 of the mass of the aged P 507 raffinate into the saturated P 507 organic matter obtained in the step 2, and filtering to obtain aged P 507;
The activated clay comprises, by weight, 60-65% of SiO 2 60, 15-20% of Al 2 O 3 15, 1-5% of Fe 2 O 3 1, 0.1-0.2% of FeO, 0.1-0.2% of TiO, 2-3% of CaO, 5-7% of MgO, 0.1-0.3% of MnO, 0.7-0.9% of K 2 O, 0.1-0.3% of Na 2 O and 0.01-0.05% of P 2 O 5 0.01.
the method effectively improves the extraction rate of cobalt, greatly reduces the consumption of liquid caustic soda, reduces the organic components of the extracted aqueous solution, reduces COD (chemical oxygen demand) and the viscosity of the whole extractant in the extraction process simultaneously by separating the aged P 507 in the P 507 extractant, thereby greatly shortening the phase separation time.
Example 1
Step 1, adding a P 507 extractant (wherein the volume percentage of P 507 in the P 507 extractant is 25%, the volume percentage of No. 260 solvent oil is 75%, and the mass ratio of aged P 507 to normal P 507 in P 507 is 1: 3) into liquid alkali, and stirring for reaction for 4min to obtain a saponified P 507 extractant;
And 2, adding an iron-removing purification solution into the saponified P 507 extraction agent obtained in the step 1, extracting for 25min, and separating cobalt to obtain a P 507 saturated organic matter, wherein the iron-removing purification solution comprises Co 60g/L, Cu 5g/L, Mn 15/L, Ca 0.5.5 g/L, and the rest metal ions are less than 0.5 g/L.
And 3, adding 8 mass of activated clay with the mass of aged P 507 raffinate into the saturated organic matter P 507 obtained in the step 2, and filtering to obtain aged P 507, wherein the activated clay comprises the following components, by weight, SiO 2 62.34%, Al 2 O 3 17.24.24%, Fe 2 O 3 2.73.73%, FeO 0.12%, TiO 0.15%, CaO 2.09%, MgO 5.44%, MnO 0.15%, K 2 O0.72%, Na 2 O0.72%, and P 2 O 5 0.03.03%.
example 2
Step 1, adding a P 507 extractant (wherein the volume percentage of P 507 in the P 507 extractant is 30%, the volume percentage of No. 260 solvent oil is 70%, and the mass ratio of aged P 507 to normal P 507 in P 507 is 1: 2) into liquid alkali, and stirring for reaction for 3min to obtain a saponified P 507 extractant;
And 2, adding iron-removing purified liquid into the saponified P 507 extracting agent obtained in the step 1, extracting for 30mim, and separating cobalt to obtain P 507 saturated organic matters, wherein the iron-removing purified liquid comprises 70g/L, Cu 2g/L, Mn 20/L, Ca 0.2g/L of Co and the balance of metal ions less than 0.5 g/L.
Step 3, adding activated clay with the mass of 5 of the aged P 507 raffinate into the saturated P 507 organic matter obtained in the step 2, and filtering to obtain aged P 507;
wherein the activated clay comprises the following components, by weight, SiO 2 62.34%, Al 2 O 3 17.24.24%, Fe 2 O 3 2.73.73%, FeO 0.12%, TiO 0.15%, CaO 2.09%, MgO 5.44%, MnO 0.15%, K 2 O0.72%, Na 2 O0.72%, and P 2 O 5 0.03.03%.
Example 3
step 1, adding a P 507 extractant (wherein the volume percentage of P 507 in the P 507 extractant is 25%, the volume percentage of No. 260 solvent oil is 75%, and the mass ratio of aged P 507 to normal P 507 in P 507 is 1: 4) into liquid alkali, and stirring for reaction for 5min to obtain a saponified P 507 extractant;
And 2, adding an iron-removing purification solution into the saponified P 507 extraction agent obtained in the step 1, extracting for 20min, and separating cobalt to obtain a P 507 saturated organic matter, wherein the iron-removing purification solution comprises 50g/L, Cu 8g/L, Mn 10/L, Ca 0.8.8 g/L of Co and the balance of metal ions less than 0.5 g/L.
Step 3, adding activated clay with the mass of 10 of the aged P 507 raffinate into the saturated P 507 organic matter obtained in the step 2, and filtering to obtain aged P 507;
Wherein the activated clay comprises the following components, by weight, SiO 2 62.34%, Al 2 O 3 17.24.24%, Fe 2 O 3 2.73.73%, FeO 0.12%, TiO 0.15%, CaO 2.09%, MgO 5.44%, MnO 0.15%, K 2 O0.72%, Na 2 O0.72%, and P 2 O 5 0.03.03%.
Example 4
Step 1, adding a P 507 extractant (wherein the volume percentage of P 507 in the P 507 extractant is 25%, the volume percentage of No. 260 solvent oil is 75%, and the mass ratio of aged P 507 to normal P 507 in P 507 is 1: 3) into liquid alkali, and stirring for reaction for 4min to obtain a saponified P 507 extractant;
and 2, adding an iron-removing purification solution into the saponified P 507 extraction agent obtained in the step 1, extracting for 30min, and separating cobalt to obtain a P 507 saturated organic matter, wherein the iron-removing purification solution comprises 70g/L, Cu 2g/L, Mn 20/L, Ca 0.2.2 g/L of Co and less than 0.5g/L of other metal ions.
Step 3, adding activated clay with the mass of 10 of the aged P 507 raffinate into the saturated P 507 organic matter obtained in the step 2, and filtering to obtain aged P 507;
wherein the activated clay comprises the following components, by weight, SiO 2 62.34%, Al 2 O 3 17.24.24%, Fe 2 O 3 2.73.73%, FeO 0.12%, TiO 0.15%, CaO 2.09%, MgO 5.44%, MnO 0.15%, K 2 O0.72%, Na 2 O0.72%, and P 2 O 5 0.03.03%.
Example 5
Step 1, adding a P 507 extractant (wherein the volume percentage of P 507 in the P 507 extractant is 30%, the volume percentage of No. 260 solvent oil is 70%, and the mass ratio of aged P 507 to normal P 507 in P 507 is 1: 2) into liquid alkali, and stirring for reaction for 3min to obtain a saponified P 507 extractant;
And 2, adding an iron-removing purification solution into the saponified P 507 extraction agent obtained in the step 1, extracting for 20min, and separating cobalt to obtain a P 507 saturated organic matter, wherein the iron-removing purification solution comprises 50g/L, Cu 8g/L, Mn 10/L, Ca 0.8.8 g/L of Co and the balance of metal ions less than 0.5 g/L.
And 3, adding 8 mass of activated clay with the mass of aged P 507 raffinate into the saturated organic matter P 507 obtained in the step 2, and filtering to obtain aged P 507, wherein the activated clay comprises the following components, by weight, SiO 2 62.34%, Al 2 O 3 17.24.24%, Fe 2 O 3 2.73.73%, FeO 0.12%, TiO 0.15%, CaO 2.09%, MgO 5.44%, MnO 0.15%, K 2 O0.72%, Na 2 O0.72%, and P 2 O 5 0.03.03%.
Example 6
Step 1, adding a P 507 extractant (wherein the volume percentage of P 507 in the P 507 extractant is 25%, the volume percentage of No. 260 solvent oil is 75%, and the mass ratio of aged P 507 to normal P 507 in P 507 is 1: 4) into liquid alkali, and stirring for reaction for 5min to obtain a saponified P 507 extractant;
and 2, adding an iron-removing purification solution into the saponified P 507 extraction agent obtained in the step 1, extracting for 25min, and separating cobalt to obtain a P 507 saturated organic matter, wherein the iron-removing purification solution comprises 50-70 g/L, Cu 2-8 g/L, Mn 10-20 g/L, Ca 0.2.2-0.8 g/L of Co, and the rest metal ions are less than 0.5 g/L.
step 3, adding activated clay with the mass of 5 of the aged P 507 raffinate into the saturated P 507 organic matter obtained in the step 2, and filtering to obtain aged P 507;
Wherein the activated clay comprises the following components, by weight, SiO 2 62.34%, Al 2 O 3 17.24.24%, Fe 2 O 3 2.73.73%, FeO 0.12%, TiO 0.15%, CaO 2.09%, MgO 5.44%, MnO 0.15%, K 2 O0.72%, Na 2 O0.72%, and P 2 O 5 0.03.03%.
Examples of the experiments
The cobalt extraction rates calculated in examples 1-6 above were compared with the cobalt extraction rates calculated in the comparative examples, and the results are shown in the following table:
from the above table, it can be seen that by adopting the technical scheme of the invention, the extraction rate of cobalt can be effectively improved, so that the same amount of cobalt is extracted, the consumption of liquid caustic soda is greatly reduced, the non-recyclable aged P 507 is effectively removed, and the extraction phase-splitting time is also greatly improved.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the scope of the present invention.

Claims (10)

1. A separation method of aged P 507, characterized in that the method is realized by the following steps:
Step 1, adding a P 507 extractant into liquid caustic soda, and stirring for reaction to obtain a saponified P 507 extractant;
Step 2, adding a purified liquid into the saponified P 507 extracting agent obtained in the step 1, extracting and separating to obtain a P 507 saturated organic matter;
And 3, adding activated clay into the P 507 saturated organic matter obtained in the step 2, and filtering to obtain aged P 507.
2. the method for separating the aged P 507, according to claim 1, wherein in the step 1, the P 507 extractant contains 25-30% by volume of P 507 and 70-75% by volume of mineral spirit.
3. The method for separating the aged P 507, according to claim 2, wherein the mass ratio of the aged P 507 to the normal P 507 in the P 507 is 1 (2-4).
4. The method for separating aged P 507, according to claim 3, wherein in step 1, 30-32% liquid alkali is used for saponification of P 507.
5. The method for separating aged P 507, according to claim 4, wherein the mineral spirit in step 1 is at least one of No. 260 mineral spirit and No. 300 mineral spirit.
6. The method for separating aged P 507, according to claim 5, wherein the reaction time in step 1 is 3-5 min.
7. the method for separating aged P 507, according to claim 6, wherein in step 2, the purifying liquid is a deironing purifying liquid, the deironing purifying liquid comprises Co 50-70 g/L, Cu 2-8 g/L, Mn 10-20 g/L, Ca 0.2.2-0.8 g/L, and the balance of metal ions is less than 0.5 g/L.
8. The method for separating the aged P 507, according to claim 7, wherein the extraction time in step 2 is 20-30 min.
9. The method for separating the aged P 507, according to claim 8, wherein the activated clay added in step 3 has a mass of 5-10% of the mass of the aged P 507 raffinate.
10. The method for separating the aged P 507 according to any one of claims 1-9, wherein in step 3, the activated clay comprises, by weight, SiO 2 60-65%, Al 2 O 3 15-20%, Fe 2 O 3 1-5%, FeO 0.1-0.2%, TiO 0.1-0.2%, CaO 2-3%, MgO 5-7%, MnO 0.1-0.3%, K 2 O0.7-0.9%, Na 2 O0.1-0.3%, and P 2 O 5 0.01.01-0.05%.
CN201810564717.7A 2018-06-04 2018-06-04 Separation method of aged P 507 Pending CN110551895A (en)

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Cited By (1)

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115354167A (en) * 2022-08-10 2022-11-18 格林美（江苏）钴业股份有限公司 Method for reducing COD (chemical oxygen demand) in raffinate in cobalt-nickel extraction production process
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Application publication date: 20191210