CN113088692A - Extractant for extracting naphthenic acid and yttrium extraction process - Google Patents
Extractant for extracting naphthenic acid and yttrium extraction process Download PDFInfo
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- CN113088692A CN113088692A CN202110367835.0A CN202110367835A CN113088692A CN 113088692 A CN113088692 A CN 113088692A CN 202110367835 A CN202110367835 A CN 202110367835A CN 113088692 A CN113088692 A CN 113088692A
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B59/00—Obtaining rare earth metals
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Abstract
The invention provides an extractant for extracting substituted naphthenic acid and an yttrium extraction process, which are applied to the technical field of novel extractant composite formula, wherein Shina-10 is adopted to substitute the naphthenic acid, Shina-10 is taken as the extractant, isooctyl naphthenate and tributyl phosphate are taken as additives, sulfonated kerosene is taken as a diluent to be compounded into a novel extractant, namely C10 extractant, which replaces the naphthenic acid extractant, and the C10 extractant has the advantages of high extraction phase separation speed, high extraction separation coefficient, small water solubility, good stability and high safety.
Description
Technical Field
The invention relates to the technical field of novel extractant composite formula, in particular to an extractant for extracting naphthenic acid and an yttrium extraction process.
Background
The rare earth industry uses naphthenic acid as extractant, which is used as main material in the process of separating yttrium by liquid-liquid extraction. Naphthenic acid is a byproduct from the petroleum refining industry, and the naphthenic acid in petroleum is directly converted into hydrocarbon substances after the petroleum refining adopts an advanced hydrocracking process, so that the naphthenic acid byproduct is not produced, the market source of purchasing the naphthenic acid by rare earth separation enterprises is stopped, and the enterprises urgently need a naphthenic acid substitute to meet the process requirement of liquid-liquid extraction separation of yttrium.
Disclosure of Invention
The invention discloses a novel extractant, which is a novel extractant replacing naphthenic acid extractant compounded by using Shina-10 (tertiary carbonic acid) as an extractant, isooctyl naphthenate, isooctyl alcohol and tributyl phosphate as additives and sulfonated kerosene as a diluent, and is defined as a C10 extractant. The C10 extractant has the advantages of high extraction phase separation speed, high extraction separation coefficient, small water solubility, good stability, high safety and the like, and completely meets the process requirements of liquid-liquid extraction separation of yttrium.
The invention adopts the following technical means for solving the technical problems:
the invention provides an extractant for extracting alternative naphthenic acid and an yttrium extraction process, comprising the following steps:
an extractant for extracting naphthenic acid is prepared from shina-10 as extractant, isooctyl naphthenate, isooctyl alcohol and tributyl phosphate as additives, and sulfonated kerosene as diluent.
Further, shina-10 comprises a monocarboxylic acid having a tertiary carbonized highly branched structure on the α -carbon atom, and is a colorless, transparent liquid having no peculiar smell and having a chemical formula of C10H20O2。
Further, the shina-10 structural formula:
further, the isooctyl naphthenate is yellow brown transparent liquid without special odor and has a chemical formula of C7H9OOC8H18。
Further, the isooctyl alcohol is colorless and transparent liquid without special odor, and the chemical formula of the isooctyl alcohol is C8H18OH。
Further, the tributyl phosphate is colorless transparent liquid without special odor, and the chemical formula of the tributyl phosphate is C12H27PO4。
Furthermore, the sulfonated kerosene is colorless, tasteless and transparent liquid formed by sulfonating the kerosene.
Further, the novel extracting agent is characterized by comprising the following components in a composite ratio:
and the acid value of the composite formula is as follows: 2.0 to 4.0 mol/L.
Further, the novel extracting agent is used for an organic phase charging tank and a continuous tank of a liquid-liquid extraction yttrium separation process.
An yttrium extraction process based on a C10 extractant employing the alternative naphthenic acid extraction extractant of claim 9 comprising:
(1) preparing a C10 extractant, compounding Shina-10/isooctyl naphthenate/isooctyl alcohol/tributyl phosphate/sulfonated kerosene 60ml/10ml/10ml/10ml/10ml into 100ml of a C10 extractant for later use, and measuring the volume acid value of the C10 extractant to be 3.2 mol/L; preparing an organic phase HA for rare earth extraction, preparing an organic phase HA100ml for later use according to a C10 extractant/isooctanol/sulfonated kerosene of 20ml/10ml/70ml, and measuring the volume acid value of the organic phase HA to be 0.64 mol/L; preparing rare earth feed liquid RE, taking chlorinated mixed heavy rare earth feed liquid RE100ml used in a production field, wherein the PH value is 3, and the total concentration of rare earth is 1.2M; preparing other materials, 8mol/L NaOH alkaline solution for saponification and 5mol/L HCI solution for back extraction;
(2) in the extraction test, the organic phase HA60ml is added into a 250ml conical separating funnel, 8mol/LNaOH4.2ml is added into the separating funnel according to the saponification degree of 85 percent, and the mixture is saponified for 3 minutes by hand shaking; taking the rare earth feed liquid RE40ml according to the comparison ratio of O/W (oxygen/water ratio) of 3/2, adding the rare earth feed liquid into a separating funnel, carrying out hand-cranking extraction for 3 minutes, then standing for phase separation, recording the first phase separation time, cutting out the extracted water phase below after phase separation, putting the extracted water phase into a100ml beaker, detecting the COD value of the extracted water phase, and carrying out spectral analysis on the rare earth components of the extracted water phase; then adding 5mol/L of HCl20ml into a separating funnel, carrying out hand-shaking back extraction for 3 minutes, standing for phase separation, recording the second phase separation time, and cutting out the lower back extraction water phase into a100ml beaker after phase separation; similarly, 5mol/L of HCl20ml is added into a separating funnel to carry out a second back extraction test, the third phase separation time is recorded, a second back extraction water phase is cut out after phase separation and is combined with the first back extraction water phase, and finally the rare earth components are subjected to spectral analysis;
(3) and (3) analyzing test results, namely acquiring the extraction phase separation time, the stripping phase separation time, the raffinate phase COD value, the rare earth component conditions and the separation coefficient of the extraction aqueous phase and the stripping aqueous phase in the test of the step (2) through spectral analysis, and determining the yttrium separated by the C10 extractant.
The invention provides an extractant for extracting naphthenic acid and an yttrium extraction process, which have the following beneficial effects:
the invention adopts Shina-10 to replace naphthenic acid, uses Shina-10 as an extractant, uses isooctyl naphthenate, isooctyl alcohol and tributyl phosphate as additives, and uses sulfonated kerosene as a diluent to compound a novel extractant, namely C10 extractant which replaces naphthenic acid extractant, and the C10 extractant has the advantages of high extraction phase separation speed, high extraction separation coefficient, small water solubility, good stability and high safety.
Drawings
FIG. 1 is a schematic process flow diagram of one embodiment of the yttrium extraction process of the present invention replacing the extractant used for naphthenic acid extraction.
The implementation, functional features and advantages of the present invention will be further described with reference to the accompanying drawings.
Detailed Description
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 technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. 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.
The invention provides an extractant for extracting naphthenic acid and an yttrium extraction process, which specifically comprises the following steps:
an extractant for extracting naphthenic acid is prepared from shina-10 as extractant, isooctyl naphthenate, isooctyl alcohol and tributyl phosphate as additives, and sulfonated kerosene as diluent.
The shina-10 comprises a monocarboxylic acid having a highly branched structure with a tertiary carbon atom on the alpha-carbon atom, is a colorless, transparent liquid without peculiar smell, and has a chemical formula of C10H20O2. The shina-10 structural formula:
the isooctyl naphthenate is a yellow brown transparent liquid without special odor and has a chemical formula of C7H9OOC8H18。
The isooctyl alcohol is colorless transparent liquid without special odor and has a chemical formula of C8H18OH。
The tributyl phosphate is colorless transparent liquid without special odor and has a chemical formula of C12H27PO4。
The sulfonated kerosene is colorless, tasteless and transparent liquid formed by sulfonating kerosene.
The new extractant is used in the organic phase filling and continuing tank of liquid-liquid extraction yttrium separating process.
In the case of the example 1, the following examples are given,
the novel extractant comprises the following components in a composite proportioning range:
and the acid value of the composite formula is as follows: 2.0 to 4.0 mol/L.
Specifically, the compound proportion of each component of the novel extracting agent is as follows:
the novel extractant is prepared according to the formula, the extractant is defined as a C10 extractant, and the extraction operation of yttrium based on the C10 extractant adopts the following steps:
referring to FIG. 1, a schematic flow diagram of an yttrium extraction process is shown;
s1, preparing a C10 extracting agent, compounding the extracting agent into 100ml of a C10 extracting agent for later use according to the conditions that Shina-10/isooctyl naphthenate/isooctyl alcohol/tributyl phosphate/sulfonated kerosene is 60ml/10ml/10ml/10ml/10ml, and measuring the volume acid value of the extracting agent to be 3.2 mol/L; preparing an organic phase HA for rare earth extraction, preparing an organic phase HA100ml for later use according to a C10 extractant/isooctanol/sulfonated kerosene of 20ml/10ml/70ml, and measuring the volume acid value of the organic phase HA to be 0.64 mol/L; preparing rare earth feed liquid RE, taking chlorinated mixed heavy rare earth feed liquid RE100ml used in a production field, wherein the PH value is 3, and the total concentration of rare earth is 1.2M; preparing other materials, 8mol/L NaOH alkaline solution for saponification and 5mol/L HCI solution for back extraction;
specifically, in the process of preparing the rare earth material liquid RE, the chlorinated mixed heavy rare earth material liquid RE used in the production field is produced by spectral analysis, and the ratio of each component is obtained according to reference table 1:
| RE | Dy | HO | Er | Tm | Yb | Lu | Y |
| (％) | 1.72 | 4.49 | 11.59 | 2.66 | 10.63 | 1.62 | 67.29 |
TABLE 1
In the process of preparing the C10 extractant, Shina-10/isooctyl naphthenate/isooctyl alcohol/tributyl phosphate/sulfonated kerosene 60ml/10ml/10ml/10ml is prepared according to the parts, and then the mixture is compounded, and the acid value in the volume solution is adjusted to be 3.2mol/L, so that the C10 extractant is prepared.
In the process of preparing the organic phase HA for rare earth extraction, preparing an organic phase HA100ml for later use according to the weight of a C10 extractant/isooctanol/sulfonated kerosene being 20ml/10ml/70ml, and adjusting the volume acid value of the organic phase HA to be 0.64 mol/L;
s2, an extraction test, namely adding the organic phase HA60ml into a 250ml conical separating funnel, adding 8mol/LNaOH4.2ml into the separating funnel according to the saponification degree of 85%, and performing hand-shaking saponification for 3 minutes; taking the rare earth feed liquid RE40ml according to the comparison ratio of O/W (oxygen/water ratio) of 3/2, adding the rare earth feed liquid into a separating funnel, carrying out hand-cranking extraction for 3 minutes, then standing for phase separation, recording the first phase separation time t1, cutting out the lower extracted aqueous phase after phase separation, putting the lower extracted aqueous phase into a100ml beaker, detecting the COD (chemical oxygen demand) value of the aqueous phase and carrying out spectral analysis on the rare earth components of the aqueous phase; then adding 5mol/L of HCl20ml into a separating funnel, carrying out hand-shaking back extraction for 3 minutes, standing for phase separation, recording the time t2 of a second phase separation, cutting out a next back extraction water phase after phase separation, and putting the next back extraction water phase into a100ml beaker; similarly, adding 5mol/L of HCl20ml into a separating funnel to perform a second back extraction test, recording the third phase separation time t3, cutting out a second back extraction water phase after phase separation, combining the second back extraction water phase with the first back extraction water phase, and finally performing spectral analysis on rare earth components of the mixture;
specifically, referring to table 2, the COD values in the above steps are shown in the corresponding time:
table 2 referring to table 3, is a spectral quantitative table of rare earth components after the spectral analysis extraction test:
| RE | Dy | HO | Er | Tm | Yb | Lu | Y |
| extract aqueous phase (%) | 1.87 | 4.84 | 14.88 | 4.45 | 19.72 | 3.51 | 50.73 |
| Raffinate aqueous phase (%) | 1.24 | 3.11 | 6.78 | 0.85 | 1.68 | 0.32 | 86.02 |
| Coefficient of separation betaRE/Y | 2.56 | 2.64 | 3.72 | 8.87 | 19.90 | 18.59 |
TABLE 3
And S3, analyzing test results, obtaining extraction phase separation time, stripping phase separation time, a raffinate phase COD value, rare earth component conditions and separation coefficients of the extraction aqueous phase and the stripping aqueous phase in the S2 test through spectral analysis, and determining the yttrium separated by the C10 extracting agent.
In conclusion, the experimental data show that the C10 extractant has a remarkable effect on yttrium extraction. Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (10)
1. An extractant for extracting naphthenic acid is characterized in that shina-10 is used as an extractant, isooctyl naphthenate, isooctyl alcohol and tributyl phosphate are used as additives, and sulfonated kerosene is used as a diluent to compound the extractant.
2. The extractant for extracting alternative naphthenic acid according to claim 1, wherein the shina-10 comprises monocarboxylic acid with tertiary carbonization and highly branched structure on alpha-carbon atom, is colorless transparent liquid without special odor, and has chemical formula C10H20O2。
3. The extractant for extraction of alternative naphthenic acids according to claim 1, characterized in that the shina-10 has the structural formula:
4. the extractant for extracting naphthenic acid as claimed in claim 1, wherein the isooctyl naphthenate is yellow brown transparent liquid without special odor and has chemical formula C7H9OOC8H18。
5. The extractant for extracting naphthenic acid as claimed in claim 1, wherein the isooctyl alcohol is colorless transparent liquid without special odor, and has chemical formula C8H18OH。
6. The extractant for extracting naphthenic acid as claimed in claim 1, wherein the tributyl phosphate is colorless transparent liquid without special odor and has chemical formula C12H27PO4。
7. The extractant for extracting naphthenic acid as claimed in claim 1, wherein the sulfonated kerosene is colorless, odorless and transparent liquid obtained by sulfonating kerosene.
8. The extractant for extracting the alternative naphthenic acid according to any one of claims 1 to 7, which is characterized in that the novel extractant comprises the following components in a composite ratio:
and the acid value of the composite formula is as follows: 2.0 to 4.0 mol/L.
9. The extractant for extracting naphthenic acid as claimed in claim 8, wherein the new extractant is used in organic phase charging tank and continuous tank of liquid-liquid extraction separation yttrium process.
10. An yttrium extraction process based on a C10 extractant, wherein the C10 extractant uses the alternative naphthenic acid extraction extractant of claim 9, comprising:
(1) preparing a C10 extractant, compounding Shina-10/isooctyl naphthenate/isooctyl alcohol/tributyl phosphate/sulfonated kerosene 60ml/10ml/10ml/10ml/10ml into 100ml of a C10 extractant for later use, and measuring the volume acid value of the C10 extractant to be 3.2 mol/L; preparing an organic phase HA for rare earth extraction, preparing an organic phase HA100ml for later use according to a C10 extractant/isooctanol/sulfonated kerosene of 20ml/10ml/70ml, and measuring the volume acid value of the organic phase HA to be 0.64 mol/L; preparing rare earth feed liquid RE, taking chlorinated mixed heavy rare earth feed liquid RE100ml used in a production field, wherein the PH value is 3, and the total concentration of rare earth is 1.2M; preparing other materials, 8mol/L NaOH alkaline solution for saponification and 5mol/L HCI solution for back extraction;
(2) in the extraction test, the organic phase HA60ml is added into a 250ml conical separating funnel, 8mol/LNaOH4.2ml is added into the separating funnel according to the saponification degree of 85 percent, and the mixture is saponified for 3 minutes by hand shaking; taking the rare earth feed liquid RE40ml according to the comparison ratio of O/W (oxygen/water ratio) of 3/2, adding the rare earth feed liquid into a separating funnel, carrying out hand-cranking extraction for 3 minutes, then standing for phase separation, recording the first phase separation time, cutting out the extracted water phase below after phase separation, putting the extracted water phase into a100ml beaker, detecting the COD value of the extracted water phase, and carrying out spectral analysis on the rare earth components of the extracted water phase; then adding 5mol/L of HCl20ml into a separating funnel, carrying out hand-shaking back extraction for 3 minutes, standing for phase separation, recording the second phase separation time, and cutting out the lower back extraction water phase into a100ml beaker after phase separation; similarly, 5mol/L of HCl20ml is added into a separating funnel to carry out a second back extraction test, the third phase separation time is recorded, a second back extraction water phase is cut out after phase separation and is combined with the first back extraction water phase, and finally the rare earth components are subjected to spectral analysis;
(3) and (3) analyzing test results, namely acquiring the extraction phase separation time, the stripping phase separation time, the raffinate phase COD value, the rare earth component conditions and the separation coefficient of the extraction aqueous phase and the stripping aqueous phase in the test of the step (2) through spectral analysis, and determining the yttrium separated by the C10 extractant.
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| CN113730954A (en) * | 2021-09-09 | 2021-12-03 | 福建省长汀金龙稀土有限公司 | Method for recovering isooctanol and sulfonated kerosene from waste organic of naphthenic acid system for extracting and separating yttrium |
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