CN111573734A - Novel extracting agent and method for extracting tungsten from phosphotungstic heteropoly acid and converting tungsten into ammonium tungstate/sodium tungstate solution - Google Patents
Novel extracting agent and method for extracting tungsten from phosphotungstic heteropoly acid and converting tungsten into ammonium tungstate/sodium tungstate solution Download PDFInfo
- Publication number
- CN111573734A CN111573734A CN202010565992.8A CN202010565992A CN111573734A CN 111573734 A CN111573734 A CN 111573734A CN 202010565992 A CN202010565992 A CN 202010565992A CN 111573734 A CN111573734 A CN 111573734A
- Authority
- CN
- China
- Prior art keywords
- tungsten
- organic phase
- heteropoly acid
- extractant
- volume
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G41/00—Compounds of tungsten
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Abstract
The invention discloses a novel extracting agent and a method for extracting tungsten from a phosphotungstic acid solution, wherein the novel extracting agent consists of 0.1-0.4 part by volume of butyl acetate, 0.2-0.4 part by volume of n-butyl alcohol and 0.3-0.6 part by volume of sulfonated kerosene, can quickly extract tungsten in phosphotungstic acid under an acidic condition and convert the tungsten into an ammonium tungstate/sodium tungstate solution, and provides a new path for converting tungsten into ammonium tungstate/sodium tungstate; meanwhile, the concentration of the phosphotungstic heteropoly acid extracted by the method is higher, and the extraction effect can reach more than 90 percent; compared with the ion exchange method, the water quantity is greatly saved.
Description
Technical Field
The invention relates to the field of metallurgy, in particular to a novel extracting agent and a method for extracting tungsten from phosphotungstic heteropoly acid and converting the tungsten into ammonium tungstate/sodium tungstate solution.
Background
At present, most of tungsten smelting is alkaline leaching and purification and concentration are realized through ion exchange; in the prior art, more amine anion exchange resin is used for adsorbing tungsten, and then ammonia solution is adopted for elution. As the alkalinity can not be thoroughly analyzed relative to the amido on the anion exchange resin, in order to obtain the ammonium tungstate solution with high concentration, high-concentration ammonia water is adopted for desorption, but the desorption rate is lower, so that the desorption solution with high concentration is more difficult to obtain, and the problem of lower resin utilization rate is caused. Meanwhile, the requirement of alkaline ion exchange on tungsten feed liquid (namely, phosphorus-tungsten heteropoly acid solution) is high, and the concentration of tungsten in the tungsten feed liquid is required to be less than (30 g/l); if the concentration of the tungsten feed liquid is higher than (30g/l), water is needed to dilute the tungsten feed liquid, so that the waste of water resources is caused.
Disclosure of Invention
In order to solve the technical problems, the invention provides a novel extracting agent and a method for extracting tungsten from phosphotungstic heteropoly acid and converting the tungsten into ammonium tungstate/sodium tungstate solution. The method can rapidly extract tungsten in the phosphotungstic heteropoly acid under an acidic condition and convert the tungsten into ammonium tungstate/sodium tungstate, and a new path is provided for converting the tungsten into the ammonium tungstate/sodium tungstate; meanwhile, the concentration of the phosphotungstic heteropoly acid extracted by the method is higher, and the extraction effect can reach more than 90 percent; compared with the ion exchange method, the water quantity is greatly saved.
The invention is realized by the following technical scheme:
a method for extracting tungsten from phosphotungstic heteropoly acid and converting the tungsten into ammonium tungstate/sodium tungstate solution comprises the steps of extracting the phosphotungstic heteropoly acid solution by using a novel extracting agent to obtain tungsten, and hydrolyzing the tungsten by using ammonia to obtain the ammonium tungstate solution or hydrolyzing the tungsten by using alkali liquor to obtain the sodium tungstate solution; the novel extractant is composed of 0.1-0.4 part of butyl acetate, 0.2-0.4 part of n-butyl alcohol and 0.3-0.6 part of sulfonated kerosene by volume.
Preferably, the novel extracting agent consists of 0.1 to 0.15 portion of butyl acetate, 0.3 to 0.4 portion of n-butyl alcohol and 0.45 to 0.55 portion of sulfonated kerosene by volume portion.
Preferably, the novel extracting agent consists of 0.15 part by volume of butyl acetate, 0.3-0.4 part by volume of n-butyl alcohol and 0.45-0.55 part by volume of sulfonated kerosene.
Preferably, the novel extracting agent consists of 0.15 part by volume of butyl acetate, 0.35 part by volume of n-butyl alcohol and 0.5 part by volume of sulfonated kerosene.
The butyl acetate is used for extracting tungsten, and the n-butyl alcohol has the function of preventing tungsten precipitation; sulfonated kerosene is used as diluent to increase fluidity.
The addition amount of the extracting agent is more than 1-2 times of the volume of the phosphotungstic acid solution. The dosage of the extracting agent has obvious influence on the extraction effect, and when the concentration of the phosphotungstic heteropoly acid is higher, the volume ratio of the extracting agent is larger; however, when the concentration of the phosphotungstic heteropoly acid is lower (less than or equal to 50g/l), the volume of the extracting agent cannot be reduced, and the extraction rate of 90 percent can be achieved only by the minimum requirement that the extracting agent is equal to the phosphotungstic heteropoly acid solution. Once the concentration of the phosphotungstic heteropoly acid is more than 50g/l, the extraction effect can be ensured only when the volume ratio of the extracting agent to the phosphotungstic heteropoly acid is more than or equal to 2:1, and the extraction effect of the novel extracting agent to the phosphotungstic heteropoly acid is more than 90 percent. Preferably, the concentration of the phosphotungstic heteropoly acid is 50g/l to 250 g/l.
More preferably, the addition amount of the extracting agent is 2-5 times (volume) of the phosphotungstic heteropoly acid solution.
For example, when the phosphotungstic heteropoly acid concentration is less than 50g/l, the volume ratio of the extracting agent to the phosphotungstic heteropoly acid solution is more than 2: 1; or when the concentration of the phosphotungstic heteropoly acid is more than 250g/l, the volume ratio of the extracting agent to the phosphotungstic heteropoly acid solution is more than 5: 1.
the extraction process of the invention adopts magnetic stirring, stirring for 2-10 minutes, standing for 1-10 minutes, and separating liquid.
The magnetic stirring speed is 1000-2000rpm, preferably 2000 rpm.
The method for converting tungsten into sodium tungstate comprises the following steps:
the extractant is called a blank organic phase, and the organic matter obtained after the blank organic phase is mixed with phosphotungstic heteropoly acid and extracted is called a loaded organic phase (organic phase after tungsten extraction); mixing and stirring the loaded organic phase and sodium hydroxide lye with the concentration of 50-100g/l according to the volume ratio of 10-2:1 (preferably 5:1), separating liquid, wherein the lower layer is back-extracted sodium tungstate solution, and the loaded organic phase is changed into a blank organic phase as the upper layer; the blank organic phase can be returned to the process for re-extraction.
The concentration of alkali liquor can be adjusted, the volume ratio of back extraction is 2: 1-10: 1, and the concentration of the alkali liquor is not beyond the range, and the back extraction is specifically adjusted according to the required residual alkalinity of sodium tungstate and the concentration of tungsten tungstate; the volume of the alkali liquor needed by (100g/l) high-alkalinity back extraction is less than that of the low alkalinity (50 g/l).
The method for converting tungsten into ammonium tungstate comprises the following steps:
the extractant is called a blank organic phase, and the organic matter obtained after the blank organic phase is mixed with heteropoly acid and extracted is called a loaded organic phase (organic phase after tungsten extraction); uniformly pouring the loaded organic phase into ammonia water, and performing mixing and stirring according to the volume ratio of 10-2:1, preferably 5:1 (the loaded organic phase: the ammonia water) to obtain an ammonium tungstate solution by back extraction; meanwhile, the loaded organic phase is changed into a blank organic phase as an upper layer; the blank organic phase can be returned to the process for re-extraction.
In the process of converting the ammonium tungstate solution, attention must be paid to a mixing mode of the loaded organic phase and the ammonia water, and if the loaded organic phase and the ammonia water are mixed reversely, a large amount of ammonium tungstate solids are separated out.
Has the advantages that:
1. the extraction agent of the invention has 3 components with different and indispensable effects, butyl acetate is used for extracting tungsten, n-butyl alcohol is used for preventing tungsten precipitation, sulfonated kerosene is used as a diluent to increase fluidity, and the three components are compounded to generate synergistic effect.
2. The novel extractant can quickly extract tungsten in phosphotungstic heteropoly acid under an acidic condition, and then reacts with ammonia water to convert the tungsten into ammonium tungstate, so that a new path is provided for converting the tungsten into the ammonium tungstate. In the process of converting ammonium tungstate/sodium tungstate, the extracting agent can be returned to the process again for repeated use, so that the cost is reduced.
3. The concentration of the phosphotungstic heteropoly acid extracted by the novel extracting agent is higher (50-250 g/l), and the extraction effect can reach more than 90%; even if the concentration is higher than 250g/l, higher extraction rate can be realized by directly increasing the addition amount of the extracting agent. Compared with the ion exchange method for extracting high-concentration phosphotungstic heteropoly acid, the method greatly saves water, can quickly extract, has short standing time and is easy to operate, thereby being more suitable for industrialized use.
Detailed Description
The following detailed description of specific embodiments of the invention is provided, but it should be understood that the scope of the invention is not limited to the specific embodiments.
Example (b): composition of novel extractant
The preparation method comprises the following steps: the substances in table 1 were mixed and stirred by magnetic force at 2000 rpm.
TABLE 1
Examples | Ethyl acetate (ml) | N-butanol (ml) | Sulfonated kerosene (ml) |
Example 1 | 15 | 35 | 50 |
Example 2 | 40 | 20 | 40 |
Example 3 | 40 | 30 | 30 |
Example 4 process for the conversion of tungsten to sodium tungstate according to the invention:
the extractant is called a blank organic phase, and the organic phase obtained after the blank organic phase is mixed with phosphotungstic heteropoly acid and extracted is called a loaded organic phase (organic phase after tungsten extraction); mixing and stirring the loaded organic phase and sodium hydroxide alkali liquor with the concentration of 50g/l according to the volume ratio of 5:1, separating liquid, wherein the lower layer is back-extracted sodium tungstate solution, and the loaded organic phase is changed into a blank organic phase as the upper layer; the blank organic phase can be returned to the process for re-extraction.
Example 5 process for the conversion of tungsten to sodium tungstate according to the invention:
the extractant is called a blank organic phase, and the organic phase obtained after the blank organic phase is mixed with phosphotungstic heteropoly acid and extracted is called a loaded organic phase (organic phase after tungsten extraction); mixing and stirring the loaded organic phase and sodium hydroxide alkali liquor with the concentration of 100g/l according to the volume ratio of 10:1 (preferably 5:1), separating liquid, wherein the lower layer is a back-extracted sodium tungstate solution, and the loaded organic phase is changed into a blank organic phase as an upper layer; the blank organic phase can be returned to the process for re-extraction.
Example 6 process for the conversion of tungsten to sodium tungstate according to the invention:
the extractant is called a blank organic phase, and the organic phase obtained after the blank organic phase is mixed with phosphotungstic heteropoly acid and extracted is called a loaded organic phase (organic phase after tungsten extraction); mixing and stirring the loaded organic phase and sodium hydroxide alkali liquor with the concentration of 70g/l according to the volume ratio of 5:1, separating liquid, wherein the lower layer is back-extracted sodium tungstate solution, and the loaded organic phase is changed into a blank organic phase as the upper layer; the blank organic phase can be returned to the process for re-extraction.
Example 7 process for the conversion of tungsten to ammonium tungstate according to the invention:
the extractant is called a blank organic phase, and the organic matter obtained after the blank organic phase is mixed and extracted with the heteropoly acid is called a loaded organic phase (organic phase after tungsten extraction); uniformly pouring the loaded organic phase into ammonia water, and performing mixing and stirring according to the volume ratio of 5:1 (loaded organic phase: ammonia water) to obtain an ammonium tungstate solution; meanwhile, the loaded organic phase is changed into a blank organic phase as an upper layer; the blank organic phase can be returned to the process for re-extraction.
Example 8 the process of the invention for converting tungsten to ammonium tungstate:
the extractant is called a blank organic phase, and the organic matter obtained after the blank organic phase is mixed and extracted with the heteropoly acid is called a loaded organic phase (organic phase after tungsten extraction); uniformly pouring the loaded organic phase into ammonia water, and performing mixing and stirring according to the volume ratio of 10:1 (the loaded organic phase: the ammonia water) to obtain an ammonium tungstate solution; meanwhile, the loaded organic phase is changed into a blank organic phase as an upper layer; the blank organic phase can be returned to the process for re-extraction.
Test example 1, influence of the amount of the novel extractant on the tungsten extraction rate;
1. test method
(1, preparing a plurality of extracting agents according to the volume ratio of 0.15:0.35: 0.5;
(2, in the experimental process, 100ml of phosphotungstic acid feed liquid is taken, the prepared extracting agent is taken according to the proportion in the table 2 and put into a 1000ml beaker, magnetic stirring is started firstly to stir the extracting agent (the stirring intensity is adjusted to 2000rpm at most), 100ml of phosphotungstic acid feed liquid is poured into the beaker to be mixed and stirred for 5 minutes, stirring and clarification are stopped for 3 minutes after the time is up, the extracted feed liquid is separated from the bottom by a separating funnel (the feed liquid is positioned at the bottom and is called raffinate), then the content of residual tungsten in the phosphotungstic acid feed liquid is analyzed, the extraction rate is calculated, and the extraction rate is (the concentration of phosphotungstic acid tungsten-the concentration of residual tungsten)/the concentration of phosphotungstic acid tungsten 100%)
2. And (3) test results: the effect of the concentration of the phosphotungstic heteropoly acid of the phosphotungstic acid of the extracting agent on the tungsten extraction effect under the mixture ratio (0.15:0.35:0.5) is verified according to the experimental process; results the experimental data are shown in Table 2
TABLE 2
As can be seen from the data in Table 2, the number of the novel extractant is 4-11, and the extraction effect of the novel extractant on the phosphotungstic heteropoly acid is more than 90%; however, as the concentration of the phosphotungstic heteropoly acid tungsten is increased, the tungsten extraction effect is relatively reduced, and at the moment, the extraction effect of more than 90 percent can be realized only by adjusting the volume ratio of the phosphotungstic heteropoly acid to the extractant. For example, the phosphotungstic heteropoly acid with the concentration of 500g/l of the phosphotungstic heteropoly acid of serial numbers 11 and 12 has the volume of 5 times of the volume of the extractant, the extraction effect is only 50 percent, the extraction effect can be recovered only by increasing the volume ratio to 10 times because the extracted effective components are saturated and can not extract more tungsten. Numbers 0-4, volume of extractant when phosphotungstic heteropoly acid concentration becomes lower (less than or equal to 50 g/l): the volume of the phosphotungstic heteropoly acid is 1-2: 1; the minimum volume ratio is 1:1 no matter how much the phosphotungstic heteropoly acid concentration is reduced. Therefore, when the phosphotungstic heteropoly acid concentration is > 50g/l, the extractant volume must be satisfied: the volume of the phosphotungstic heteropoly acid is more than or equal to 2:1, and the extraction rate can reach more than 90 percent. The highest concentration of heteropoly acid tungsten can not exceed 300g/l from an industrial angle; therefore, the ratio of the usage amount of the extracting agent to the phosphotungstic heteropoly acid is 2-5:1 from the industrial point of view. The concentration of the phosphotungstic heteropoly acid is less than 50g/l, and the volume ratio of the extracting agent to the phosphotungstic heteropoly acid solution is more than 2: 1; or the concentration of the phosphotungstic heteropoly acid is more than 250g/l, and the volume ratio of the extracting agent to the phosphotungstic heteropoly acid solution is more than 5:1, the product is obtained.
Example 2, the effect of the extractant components on tungsten extraction;
1. the method comprises the following steps: the influence of the 3 components on the tungsten extraction effect of the phosphotungstic heteropoly acid is considered, the volume ratio of one component is fixed, and the volume ratio of one component is gradually increased to 80 percent from 10 percent; the volume ratio of the other two substances is 1: 1; the sum of the volume ratios is 1; preparing various proportions of organic substances for experiments;
2. the experimental process comprises the following steps: taking 100ml of phosphotungstic heteropoly acid feed liquid of phosphorus tungsten, taking 400ml of prepared extractant in a 1000ml beaker, and firstly starting magnetic stirring to stir the extractant (the stirring intensity is adjusted to the maximum); 100ml of phosphotungstic heteropoly acid feed liquid is poured into the mixture and stirred for 5 minutes; stopping stirring and clarifying for 3 minutes after the time is up; separating the extracted feed liquid from the bottom by using a separating funnel (the feed liquid is positioned at the bottom and is called raffinate); then analyzing the tungsten content of raffinate, and calculating the extraction rate; (extraction rate ═ concentration of phosphotungstic heteropoly acid tungsten-concentration of raffinate tungsten)/concentration of phosphotungstic heteropoly acid tungsten 100%)
3. As a result: the experimental data are as follows in table 3:
table 3 effect of butyl acetate volume fraction on extraction:
ratio of butyl acetate | N-butanol proportion | Proportion of sulfonated kerosene | Concentration g/l of heteropoly acid tungsten | Raffinate tungsten concentration g/l | Extraction ratio (%) |
10% | 45% | 45% | 205 | 50 | 75.61 |
20% | 40% | 40% | 205 | 25 | 87.80 |
30% | 35% | 35% | 205 | 18 | 91.22 |
40% | 30% | 30% | 205 | 15 | 92.68 |
50% | 25% | 25% | 205 | 5 | 97.56 |
60% | 20% | 20% | 205 | 6 | 97.07 |
70% | 15% | 15% | 205 | 3 | 98.54 |
80% | 10% | 10% | 205 | 5 | 97.56 |
Table 3: the tungsten extraction effect is improved along with the increase of the volume ratio of the butyl acetate component, and the butyl acetate is the main component in the extracting agent for extracting tungsten; however, as the concentration of ethyl acetate increases, more impurities appear in the back-extracted ammonium tungstate solution, impurities are removed abnormally, elements cannot be removed to an index range, and finally the elements of the obtained product exceed the standard. The amount of ethyl acetate used is a very important indicator.
TABLE 4 influence of n-butanol pure volume fraction on extraction rate
As can be seen from the data in Table 4, the extraction effect is also reduced along with the increase of the n-butanol dosage, and it can be seen that the n-butanol dosage has no significant influence on the extraction effect. The extractant is normally divided into 2 layers after extraction; the extractant is positioned at the upper layer, the raffinate is positioned at the lower layer, and a clear interface is formed; if the third phase appears, the third phase is positioned at the bottommost layer and has the same color as the extracting agent. From the volume of the third phase in table 3, the volume of the third phase gradually decreases with the increase of the proportion of n-butanol, and it can be seen that the n-butanol function prevents organic precipitation after tungsten extraction.
Table 5 sulfonated kerosene volume fraction versus extraction rate effect:
the data in table 5 show that the extraction effect is significantly reduced with the increase of the dosage of the sulfonated kerosene, and it can be seen that the sulfonated kerosene is not the main component of the tungsten extraction of the present invention.
Test example 3 screening test for extractant ratio
The method comprises the following steps: as in test example 1, 200g/l of feed liquid was used in a uniform concentration of the pre-extraction liquid.
As a result: see Table 6
TABLE 6
As can be seen from the numbers 6 and 7 in Table 6, the best results were obtained when the amounts of butyl acetate, n-butanol and sulfonated kerosene were 0.1 to 0.15 parts, 0.3 to 0.4 parts and 0.45 to 0.55 parts, respectively, from the viewpoint of the extraction yield, the volume of the third layer, the separation rate and the impurity removal. Therefore, the volume ratio of butyl acetate, n-butanol and sulfonated kerosene is preferably 0.15: (0.3-0.4): (0.45-0.55).
Test example 4 screening of parameters of the extraction Process of the invention
The method comprises the following steps: taking a plurality of 200g/l heteropoly acid materials; 1 beaker of 800 ml; one magnetic stirrer; (0.15:0.35:0.5) a plurality of extracting agents; the volume ratio of the extracting agent to the heteropoly acid is 4: 1, mixing; mixing for 5min under different stirring frequencies; and verifying the influence of the stirring strength on the extraction effect.
As a result: see table 7.
TABLE 7
Volume of heteropoly acid | Volume of extractant | Speed of agitation (rpm) | Raffinate tungsten g/l | Extraction rate |
100 | 400 | 100 | 35.00 | 82.50% |
100 | 400 | 500 | 28.00 | 86% |
100 | 400 | 1000 | 22.00 | 89% |
100 | 400 | 1500 | 21.00 | 89.50% |
100 | 400 | 2000 | 19.00 | 90.50% |
As can be seen from Table 7, the magnetic stirring speed is the highest at 1000-.
The foregoing descriptions of specific exemplary embodiments of the present invention have been presented for purposes of illustration and description. It is not intended to limit the invention to the precise form disclosed, and obviously many modifications and variations are possible in light of the above teaching. The exemplary embodiments were chosen and described in order to explain certain principles of the invention and its practical application to enable one skilled in the art to make and use various exemplary embodiments of the invention and various alternatives and modifications as are suited to the particular use contemplated. It is intended that the scope of the invention be defined by the claims and their equivalents.
Claims (10)
1. A novel extracting agent is composed of, by volume, 0.1-0.4 part of butyl acetate, 0.2-0.4 part of n-butyl alcohol and 0.3-0.6 part of sulfonated kerosene, and can extract a tungsten-containing solution.
2. The extractant as claimed in claim 1, which consists of 0.1-0.15 part of butyl acetate, 0.3-0.4 part of n-butanol and 0.45-0.55 part of sulfonated kerosene by volume, preferably 0.15 part of butyl acetate, 0.3-0.4 part of n-butanol and 0.45-0.55 part of sulfonated kerosene.
3. The extractant as claimed in claim 2, which consists of 0.15 part by volume of butyl acetate, 0.35 part by volume of n-butanol and 0.50 part by volume of sulfonated kerosene.
4. The extractant of any one of claims 1 to 3, characterized in that: the tungsten-containing solution is a phosphotungstic heteropoly acid solution.
5. The extractant of claim 4, wherein: the volume ratio of the extracting agent to the phosphorus-tungsten heteropoly acid solution is more than or equal to 1-2: 1.
6. the extractant of claim 5, wherein: the volume ratio of the extracting agent to the phosphorus-tungsten heteropoly acid solution is 2-5: 1.
7. the extractant of claim 4, wherein the phosphotungstic heteropoly acid concentration is from 50g/l to 250 g/l.
8. The extractant as claimed in claim 4, characterized in that, at concentrations of phosphotungstic heteropoly acid < 50g/l, the volume ratio of extractant to phosphotungstic heteropoly acid solution is > 2: 1; or when the concentration of the phosphotungstic heteropoly acid is more than 250g/l, the volume ratio of the extracting agent to the phosphotungstic heteropoly acid solution is more than 5: 1.
9. a method for extracting tungsten from phosphotungstic heteropoly acid by using a novel extracting agent is characterized by comprising the following steps: the novel extractant is put into the phosphotungstic heteropoly acid solution, magnetically stirred for 2 to 10 minutes at the speed of 1000-2000rpm and kept stand for 1 to 10 minutes.
10. A method for extracting a tungsten-converted ammonium tungstate/sodium tungstate solution from phosphotungstic heteropoly acid by using a novel extracting agent is characterized by comprising the following steps: the novel extractant is called a blank organic phase, and the organic matter obtained after the blank organic phase is mixed with the heteropoly acid and extracted is called a loaded organic phase; mixing and stirring the loaded organic phase and sodium hydroxide lye with the concentration of 50-100g/l according to the volume ratio of 10-2:1 (preferably 5:1), separating liquid, wherein the lower layer is back-extracted sodium tungstate solution, and the loaded organic phase is changed into a blank organic phase as the upper layer; returning the blank organic phase to the process for re-extraction; or
The novel extractant is called a blank organic phase, and the organic matter obtained after the blank organic phase is mixed with the heteropoly acid and extracted is called a loaded organic phase; uniformly pouring the loaded organic phase into ammonia water, and performing mixing and stirring according to the volume ratio of 10-2:1 (preferably 5:1) to obtain an ammonium tungstate solution; meanwhile, the loaded organic phase is changed into a blank organic phase as an upper layer; the blank organic phase is returned to the process for re-extraction.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN202010565992.8A CN111573734B (en) | 2020-06-19 | 2020-06-19 | Extractant and method for extracting tungsten from phosphotungstic heteropoly acid and converting tungsten into ammonium tungstate/sodium tungstate solution |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN202010565992.8A CN111573734B (en) | 2020-06-19 | 2020-06-19 | Extractant and method for extracting tungsten from phosphotungstic heteropoly acid and converting tungsten into ammonium tungstate/sodium tungstate solution |
Publications (2)
Publication Number | Publication Date |
---|---|
CN111573734A true CN111573734A (en) | 2020-08-25 |
CN111573734B CN111573734B (en) | 2022-08-19 |
Family
ID=72110720
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN202010565992.8A Active CN111573734B (en) | 2020-06-19 | 2020-06-19 | Extractant and method for extracting tungsten from phosphotungstic heteropoly acid and converting tungsten into ammonium tungstate/sodium tungstate solution |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN111573734B (en) |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN113720987A (en) * | 2021-08-11 | 2021-11-30 | 信丰华锐钨钼新材料有限公司 | Method for removing tungsten, molybdenum, phosphorus and polyacid in tungsten smelting macroporous resin desorption solution |
CN115821073A (en) * | 2022-12-09 | 2023-03-21 | 厦门钨业股份有限公司 | Method for extracting tungsten from acidic tungsten-containing feed liquid |
Citations (8)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
GB9828020D0 (en) * | 1998-12-18 | 1999-02-10 | Bp Chem Int Ltd | Synthesis of heteropolyacids |
CN1978328A (en) * | 2005-11-30 | 2007-06-13 | 中国石油化工股份有限公司 | Method for preparing heteropoly acid containing tungsten from tunsten powder |
CN102080161A (en) * | 2010-12-24 | 2011-06-01 | 中南大学 | Method for comprehensively recovering tungsten and phosphorus from high phosphorus white tungsten ores |
CN103805793A (en) * | 2013-09-13 | 2014-05-21 | 江西理工大学 | Method for decomposing scheelite |
CN104711422A (en) * | 2015-03-16 | 2015-06-17 | 中南大学 | Method for extracting and separating tungsten and molybdenum in high-phosphorus mixed solution containing tungsten and molybdenum |
CN106976912A (en) * | 2017-04-10 | 2017-07-25 | 中南大学 | A kind of method for preparing phosphorus heteropoly tungstic acid solution |
CN110357796A (en) * | 2019-07-03 | 2019-10-22 | 山东万山集团有限公司 | The preparation method of continuous extraction process and extractant, naphthalene sulfonic acids and water-reducing agent |
CN111298476A (en) * | 2020-03-11 | 2020-06-19 | 厦门钨业股份有限公司 | Phosphotungstic heteropoly acid extracting agent, extracting method and application of aromatic hydrocarbon solvent oil |
-
2020
- 2020-06-19 CN CN202010565992.8A patent/CN111573734B/en active Active
Patent Citations (8)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
GB9828020D0 (en) * | 1998-12-18 | 1999-02-10 | Bp Chem Int Ltd | Synthesis of heteropolyacids |
CN1978328A (en) * | 2005-11-30 | 2007-06-13 | 中国石油化工股份有限公司 | Method for preparing heteropoly acid containing tungsten from tunsten powder |
CN102080161A (en) * | 2010-12-24 | 2011-06-01 | 中南大学 | Method for comprehensively recovering tungsten and phosphorus from high phosphorus white tungsten ores |
CN103805793A (en) * | 2013-09-13 | 2014-05-21 | 江西理工大学 | Method for decomposing scheelite |
CN104711422A (en) * | 2015-03-16 | 2015-06-17 | 中南大学 | Method for extracting and separating tungsten and molybdenum in high-phosphorus mixed solution containing tungsten and molybdenum |
CN106976912A (en) * | 2017-04-10 | 2017-07-25 | 中南大学 | A kind of method for preparing phosphorus heteropoly tungstic acid solution |
CN110357796A (en) * | 2019-07-03 | 2019-10-22 | 山东万山集团有限公司 | The preparation method of continuous extraction process and extractant, naphthalene sulfonic acids and water-reducing agent |
CN111298476A (en) * | 2020-03-11 | 2020-06-19 | 厦门钨业股份有限公司 | Phosphotungstic heteropoly acid extracting agent, extracting method and application of aromatic hydrocarbon solvent oil |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN113720987A (en) * | 2021-08-11 | 2021-11-30 | 信丰华锐钨钼新材料有限公司 | Method for removing tungsten, molybdenum, phosphorus and polyacid in tungsten smelting macroporous resin desorption solution |
CN115821073A (en) * | 2022-12-09 | 2023-03-21 | 厦门钨业股份有限公司 | Method for extracting tungsten from acidic tungsten-containing feed liquid |
Also Published As
Publication number | Publication date |
---|---|
CN111573734B (en) | 2022-08-19 |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
CN111573734B (en) | Extractant and method for extracting tungsten from phosphotungstic heteropoly acid and converting tungsten into ammonium tungstate/sodium tungstate solution | |
CN109868363A (en) | The method of extraction and separation tungsten from molybdate solution | |
CN105271413A (en) | Method for extracting tungsten from phosphotungstic acid/phosphotungstate solution | |
CN100441203C (en) | Method for preparing astragalus root saponin | |
CN108624885A (en) | A kind of spent acid and the method for alkaline etching liquid processing | |
CN103146938B (en) | Extraction and separation method of uranium | |
CN105925797B (en) | A kind of method and system for decomposing white tungsten fine ore | |
CN103397184A (en) | Method for separating uranium and iron from tertiary amine organic phase by back extraction | |
CN111041241A (en) | Preparation method of nuclear grade pure zirconium nitrate | |
CN105002366B (en) | A kind of method of the recovering rare earth from neutralization slag caused by neodymium iron boron waste material recovering rare earth process | |
CN1880489B (en) | Non-saponifiable extraction full-separating process for high concentration rare earth solution | |
CN109593976A (en) | A method of extraction manganese | |
CN102887534A (en) | Method for recovering reagent level anhydrous sodium sulfate from raffinate obtained in process of extracting nickel from nickel sulfate solution | |
CN109179480A (en) | The method for extracting scandium oxide | |
CN106555054A (en) | A kind of separation and recovery method of thorium and uranium | |
CN114672650B (en) | Method for extracting scandium from titanium white waste acid by using bisphosphonic acid extractant | |
CN101503760B (en) | Method for extracting zinc from zinc oxide ore ammonia leaching solution | |
CN101156664B (en) | Method for distilling fucoidin from sea tangle caustic refining liquid | |
CN205687982U (en) | A kind of system decomposing white tungsten fine ore | |
TW421606B (en) | Method of purifying substances by extraction from a liquid medium | |
CN108585025B (en) | Recovery method of silver oxide slag | |
CN111074070B (en) | Method for extracting yttrium from marine rare earth sulfuric acid leaching solution and extracted organic phase | |
CN1212411C (en) | Ce extraction from nitric acid rare earth solution | |
CN114561557B (en) | Process for rapidly dissolving nickel beans | |
CN105525094A (en) | Method for extracting tungsten from alkaline crude sodium tungstate solution |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
PB01 | Publication | ||
PB01 | Publication | ||
SE01 | Entry into force of request for substantive examination | ||
SE01 | Entry into force of request for substantive examination | ||
GR01 | Patent grant | ||
GR01 | Patent grant |