CN111298476A - Phosphotungstic heteropoly acid extracting agent, extracting method and application of aromatic hydrocarbon solvent oil - Google Patents
Phosphotungstic heteropoly acid extracting agent, extracting method and application of aromatic hydrocarbon solvent oil Download PDFInfo
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- CN111298476A CN111298476A CN202010167888.3A CN202010167888A CN111298476A CN 111298476 A CN111298476 A CN 111298476A CN 202010167888 A CN202010167888 A CN 202010167888A CN 111298476 A CN111298476 A CN 111298476A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/04—Solvent extraction of solutions which are liquid
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/04—Solvent extraction of solutions which are liquid
- B01D11/0492—Applications, solvents used
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- C—CHEMISTRY; METALLURGY
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- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G41/00—Compounds of tungsten
- C01G41/003—Preparation involving a liquid-liquid extraction, an adsorption or an ion-exchange
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Abstract
The invention discloses a phosphotungstic heteropoly acid extracting agent, an extracting method and application of aromatic hydrocarbon solvent oil, wherein the phosphotungstic heteropoly acid extracting agent comprises the following components: the main extracting agent and aromatic solvent oil, wherein the aromatic solvent oil is used as a diluent. The phosphotungstic heteropoly acid extracting agent avoids adopting sulfonated kerosene, and can effectively reduce the consumption of the extracting agent.
Description
Technical Field
The invention belongs to the field of preparation of phosphotungstic heteropoly acid, and particularly relates to a phosphotungstic heteropoly acid extracting agent, an extraction method of phosphotungstic heteropoly acid and application of aromatic hydrocarbon solvent oil.
Background
In an organic medium, the molar catalytic activity of the heteropoly acid with stronger acidity is far greater than that of sulfuric acid, and the heteropoly acid also has the advantages of relative stability, no toxicity, difficult generation of side reaction and the like, can be used as a novel catalytic material, and has wide application prospect. Among them, phosphotungstic heteropoly acid is most widely used in heteropoly acid, and is representative.
The diluent used by the existing phosphotungstic heteropoly acid extracting agent is usually sulfonated kerosene, and the sulfonated kerosene is easy to volatilize, so that the extracting agent is large in loss, the process is strong in smell, and hidden troubles are brought to environmental protection. There is a need to find a new component to replace sulfonated kerosene to solve the drawbacks of the prior art.
Disclosure of Invention
The present invention is directed to solving at least one of the problems of the prior art.
Therefore, the invention provides a phosphotungstic heteropoly acid extracting agent which can effectively reduce consumption.
The invention also provides an extraction method of the phosphotungstic heteropoly acid, which has the advantages of convenient operation, environmental protection and the like.
The invention also provides an application of the aromatic hydrocarbon solvent oil, and the aromatic hydrocarbon solvent oil can be used as a diluent of an extracting agent in the extraction process of the phosphotungstic heteropoly acid, can replace sulfonated kerosene, and has the advantages of difficult volatilization, contribution to the extraction process and the like.
A phosphotungstic heteropoly acid extractant according to an embodiment of the first aspect of the invention consists of: the main extracting agent and aromatic solvent oil, wherein the aromatic solvent oil is used as a diluent.
According to the phosphotungstic heteropoly acid extracting agent disclosed by the embodiment of the invention, aromatic hydrocarbon solvent oil is adopted to be used as a diluent of the extracting agent in the extracting process of the phosphotungstic heteropoly acid, the aromatic hydrocarbon solvent oil has the characteristics of high boiling point and high flash point compared with sulfonated kerosene, the aromatic hydrocarbon solvent oil is not easy to volatilize and is more environment-friendly, the viscosity of the aromatic hydrocarbon solvent oil is lower than that of the sulfonated kerosene, namely the aromatic hydrocarbon solvent oil has better fluidity and is more beneficial to the extracting process.
According to one embodiment of the invention, the primary extractant is a mixture of lipid compounds and alcohol compounds.
According to one embodiment of the invention, the main extractant consists of n-butanol and butyl acetate.
According to one embodiment of the invention, the volume ratio of the aromatic hydrocarbon solvent oil to the n-butyl alcohol to the butyl acetate is 0.4-0.6: 0.2-0.35: 0.1 to 0.25.
According to one embodiment of the present invention, the volume ratio of the aromatic hydrocarbon solvent oil, the n-butanol and the butyl acetate is 0.5: 0.35: 0.15.
according to one embodiment of the invention, the aromatic mineral spirit is aromatic No. 200 mineral spirit.
The extraction method of the phosphotungstic heteropoly acid according to the embodiment of the second aspect of the invention comprises the following preparation steps: s1, preparing a phosphotungstic heteropoly acid extracting agent for later use, wherein the phosphotungstic heteropoly acid extracting agent consists of a main extracting agent and aromatic solvent oil; s2, carrying out reverse continuous contact on the phosphotungstic heteropoly acid solution and the phosphotungstic heteropoly acid extracting agent, leading out the mixed phosphotungstic heteropoly acid solution and the phosphotungstic heteropoly acid extracting agent, standing and layering.
According to an embodiment of the present invention, in step S2, the phosphotungstic heteropoly acid solution and the phosphotungstic heteropoly acid extractant are subjected to reverse continuous contact in a pH balance medium.
According to an embodiment of the present invention, the step S2 includes: s21, adding the phosphotungstic heteropoly acid extractant into CO under the condition of pressurization2Stirring in the fluid; s22, mixing with CO2The phosphotungstic heteropoly acid extracting agent is in reverse continuous contact with the phosphotungstic heteropoly acid solution, and the pressure of the phosphotungstic heteropoly acid solution is less than that of the phosphotungstic heteropoly acid extracting agent.
According to the application of the aromatic hydrocarbon solvent oil in the third aspect of the invention, the aromatic hydrocarbon solvent oil is used as a diluent of the extracting agent in the process of extracting the phosphotungstic heteropoly acid.
Additional aspects and advantages of the invention will be set forth in part in the description which follows and, in part, will be obvious from the description, or may be learned by practice of the invention.
Drawings
The above and/or additional aspects and advantages of the present invention will become apparent and readily appreciated from the following description of the embodiments, taken in conjunction with the accompanying drawings of which:
FIG. 1 is a flow diagram of a phosphotungstic heteropoly acid extraction process according to an embodiment of the present invention;
FIG. 2 is a graph comparing the results of tungsten extraction with the extractant of example 4 versus comparative example 1;
FIG. 3 is a graph comparing the amount of extractant consumed in example 4 with that of comparative example 1.
Detailed Description
Embodiments of the present invention will be described in detail below, the embodiments described with reference to the drawings being illustrative, and the embodiments of the present invention will be described in detail below.
The following describes a phosphotungstic heteropoly acid extractant according to an embodiment of the present invention, consisting of the following components: the main extracting agent and aromatic solvent oil, wherein the aromatic solvent oil is used as a diluent.
Therefore, aromatic hydrocarbon solvent oil adopted in the phosphotungstic heteropoly acid extracting agent provided by the embodiment of the invention can be used as a diluent of the extracting agent in the extracting process of the phosphotungstic heteropoly acid, compared with sulfonated kerosene, the aromatic hydrocarbon solvent oil has the characteristics of high boiling point and high flash point, is not easy to volatilize and is more environment-friendly, and the viscosity of the aromatic hydrocarbon solvent oil is lower than that of the sulfonated kerosene, namely the aromatic hydrocarbon solvent oil has better fluidity and is more beneficial to the extracting process.
According to one embodiment of the invention, the primary extractant is a mixture of lipid compounds and alcohol compounds.
Optionally, the primary extractant consists of n-butanol and butyl acetate.
In some embodiments of the present invention, the volume ratio of the aromatic hydrocarbon solvent oil, the n-butanol and the butyl acetate is 0.4 to 0.6: 0.2-0.35: 0.1 to 0.25.
Further, the volume ratio of the aromatic hydrocarbon solvent oil, the n-butanol and the butyl acetate is 0.5: 0.35: 0.15.
according to one embodiment of the invention, the aromatic mineral spirit is aromatic No. 200 mineral spirit.
The specific gravity of the aromatic hydrocarbon No. 200 solvent oil and the conventional sulfonated kerosene is shown in table 1 below.
TABLE 1
| Name (R) | Density of | Appearance of the product | Boiling point | Flash point | Viscosity of the oil |
| Aromatic solvent oil | 0.79 | Colorless and transparent | 200℃～250℃ | 81℃ | 1.6 |
| Sulfonated kerosene | 0.8 | Colorless and transparent | 37.8℃～204℃ | 65.5 | 1.8 |
As can be seen from table 1 above, solvent a has: the characteristics of high boiling point and high flash point show that the solvent A is not easy to volatilize and is more environment-friendly; the viscosity of the solvent A is lower than that of the sulfonated kerosene, which shows that the fluidity is better and is more beneficial to the extraction process;
the extraction method of the phosphotungstic heteropoly acid provided by the embodiment of the invention comprises the following preparation steps:
s1, preparing a phosphotungstic heteropoly acid extracting agent for later use, wherein the phosphotungstic heteropoly acid extracting agent consists of a main extracting agent and aromatic solvent oil.
S2, carrying out reverse continuous contact on the phosphotungstic heteropoly acid solution and the phosphotungstic heteropoly acid extracting agent, leading out the mixed phosphotungstic heteropoly acid solution and the phosphotungstic heteropoly acid extracting agent, standing and layering. By adopting reverse continuous contact, the mixing degree between the phosphotungstic heteropoly acid solution and the phosphotungstic heteropoly acid extracting agent can be improved, and the extraction efficiency is improved.
Further, in the step S2, the phosphotungstic heteropoly acid solution and the phosphotungstic heteropoly acid extracting agent are continuously contacted in a reverse direction in a pH balance medium.
Optionally, the step S2 includes:
s21, adding the phosphotungstic heteropoly acid extractant into CO under the condition of pressurization2Stirring in the fluid.
S22, mixing with CO2The phosphotungstic heteropoly acid extracting agent is in reverse continuous contact with the phosphotungstic heteropoly acid solution, the pressure intensity of the phosphotungstic heteropoly acid solution is smaller than that of the phosphotungstic heteropoly acid extracting agent, the mixing degree and the mixing effect between the phosphotungstic heteropoly acid solution and the phosphotungstic heteropoly acid extracting agent can be further improved through pressure intensity difference, and the extraction efficiency and the extraction effect are further improved.
According to the application of the aromatic hydrocarbon solvent oil disclosed by the embodiment of the invention, the aromatic hydrocarbon solvent oil is used as a diluent of an extracting agent in the extraction process of the phosphotungstic heteropoly acid.
The phosphotungstic heteropoly acid extractant and the extraction method of the examples of the present invention will be described in detail below with reference to specific embodiments.
Example 1
(1) Preparation of phosphotungstic heteropoly acid extractant
The phosphotungstic heteropoly acid extractant consists of a main extractant and aromatic hydrocarbon solvent oil, wherein the main extractant consists of n-butyl alcohol and butyl acetate, and the volume ratio of the aromatic hydrocarbon solvent oil to the n-butyl alcohol to the butyl acetate is 0.4: 0.35: 0.25.
(2) extraction of phosphotungstic heteropoly acids
And (2) carrying out reverse continuous contact on the phosphotungstic heteropoly acid solution and the phosphotungstic heteropoly acid extracting agent prepared in the step (1), leading out the mixed phosphotungstic heteropoly acid solution and the phosphotungstic heteropoly acid extracting agent, standing for 12h, and layering.
Example 2
(1) Preparation of phosphotungstic heteropoly acid extractant
The phosphotungstic heteropoly acid extractant consists of a main extractant and aromatic hydrocarbon solvent oil, wherein the main extractant consists of n-butyl alcohol and butyl acetate, and the volume ratio of the aromatic hydrocarbon solvent oil to the n-butyl alcohol to the butyl acetate is 0.5: 0.25: 0.25.
(2) extraction of phosphotungstic heteropoly acids
And (2) carrying out reverse continuous contact on the phosphotungstic heteropoly acid solution and the phosphotungstic heteropoly acid extracting agent prepared in the step (1) in a pH balance medium, wherein the pH balance medium is inorganic acid or inorganic alkali, leading out the mixed phosphotungstic heteropoly acid solution and the phosphotungstic heteropoly acid extracting agent, standing for 10h, and layering.
Example 3
(1) Preparation of phosphotungstic heteropoly acid extractant
The phosphotungstic heteropoly acid extractant consists of a main extractant and aromatic hydrocarbon solvent oil, wherein the main extractant consists of n-butyl alcohol and butyl acetate, and the volume ratio of the aromatic hydrocarbon solvent oil to the n-butyl alcohol to the butyl acetate is 0.5: 0.25: 0.25.
(2) extraction of phosphotungstic heteropoly acids
Firstly, extracting agent of phosphotungstic heteropoly acid in CO under the condition of pressurization2Stirring in the fluid under the pressure of 8-10 MPa.
Then, will be mixed with CO2The phosphotungstic heteropoly acid extracting agent is in reverse continuous contact with the phosphotungstic heteropoly acid solution, and the pressure intensity of the phosphotungstic heteropoly acid solution is smaller than that of the phosphotungstic heteropoly acid extracting agent.
And finally, leading out the mixed phosphotungstic heteropoly acid solution and the phosphotungstic heteropoly acid extracting agent, standing for 10 hours, and layering.
Wherein CO may be mixed2The phosphotungstic heteropoly acid extracting agent is led into an upright reaction vessel from bottom to top through a reaction pump, a phosphotungstic heteropoly acid solution is led into the reaction vessel from top to bottom, and the mixed phosphotungstic heteropoly acid solution and the phosphotungstic heteropoly acid extracting agent are led out from the middle part of the reaction vessel and are kept stand.
Alternatively, CO may be mixed with2The phosphotungstic heteropoly acid extractant is horizontally led in from left to right through a reaction pumpThe phosphotungstic heteropoly acid solution is led into the reaction vessel from the right side to the left side, the mixed phosphotungstic heteropoly acid solution and the phosphotungstic heteropoly acid extracting agent are led out from the middle part of the reaction vessel, and the reaction vessel is kept still.
Example 4
Preparation of phosphotungstic heteropoly acid extractant
The phosphotungstic heteropoly acid extracting agent consists of aromatic hydrocarbon solvent oil, n-butyl alcohol and butyl acetate, wherein the volume ratio of the aromatic hydrocarbon solvent oil to the n-butyl alcohol to the butyl acetate is 0.5: 0.35: 0.15, the aromatic solvent oil is aromatic No. 200 solvent oil.
Comparative example 1
The phosphotungstic heteropoly acid extracting agent consists of sulfonated kerosene, n-butyl alcohol and butyl acetate, wherein the volume ratio of the sulfonated kerosene, the n-butyl alcohol and the butyl acetate is 0.5: 0.35: 0.15 is configured as an extractant.
Experimental testing
The tungsten extraction capacity, the strip liquor dephosphorization degree and the extractant consumption condition of the extractants prepared in example 4 and comparative example 1 are respectively tested under the same conditions, and specifically, whether the two extractants affect the extraction and strip results under the same conditions or not is compared, and the consumption of the two extractants is compared.
(1) Comparison of tungsten extraction Capacity
The extraction results of the extractant corresponding to the example 4 and the extractant corresponding to the comparative example 1 on tungsten are shown in figure 2, and it can be seen from figure 2 that the extraction effects are similar and have little difference under the same heteropoly acid concentration; under the condition of the same proportion, the concentration of the heteropoly acid is reduced, which shows that the extraction effect of the extractant is basically not influenced by adopting the aromatic solvent oil to replace the sulfonated kerosene.
(2) Contrast of stripping solution
The same amount of the extractant corresponding to the comparative example 1 and the same amount of the extractant corresponding to the example 4 were taken, extracted under the same conditions, and then back-extracted to obtain back-extracted solutions respectively, and the phosphorus removal effects of the two back-extracted solutions were compared as shown in the following table 2, wherein it should be noted that the same amount of magnesium sulfate solution was added to the extractant corresponding to the comparative example 1 and the extractant corresponding to the example 4 in the conventional process during the test.
TABLE 2
| Stripping solution | Wo3(g/l) | Ammonia (g/l) | Mg(g/l) | P(g/l) |
| Comparative example 1 | 222 | 70 | 234 | 0.012 |
| Example 4 | 220 | 68 | 250 | 0.015 |
It can be seen from table 2 that the phosphorus removal effect of the extractant corresponding to comparative example 1 is similar to that of the extractant corresponding to example 4 under the same conditions, which indicates that the quality of the back extraction solution obtained after back extraction is not affected by using the aromatic solvent oil instead of sulfonated kerosene.
(3) Consumption comparison
The consumption of the extractant corresponding to comparative example 1 compared to that of example 4 is shown in fig. 3, and it can be seen from fig. 3 that the two extractants of the same mass are reduced differently over time, wherein the extractant of comparative example 1 is reduced to a greater extent than the extractant of example 4, i.e., the consumption of the extractant of example 4 is lower in the same case.
In the description herein, references to the description of the term "one embodiment," "some embodiments," "an illustrative embodiment," "an example," "a specific example," or "some examples" or the like mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above do not necessarily refer to the same embodiment or example.
While embodiments of the invention have been shown and described, it will be understood by those of ordinary skill in the art that: various changes, modifications, substitutions and alterations can be made to the embodiments without departing from the principles and spirit of the invention, the scope of which is defined by the claims and their equivalents.
Claims (10)
1. The phosphotungstic heteropoly acid extracting agent is characterized by comprising the following components:
the main extracting agent and aromatic solvent oil, wherein the aromatic solvent oil is used as a diluent.
2. The phosphotungstic heteropoly acid extractant of claim 1, wherein the primary extractant is a mixture consisting of lipid compounds and alcohol compounds.
3. The phosphotungstic heteropoly acid extractant of claim 2, wherein the primary extractant consists of n-butanol and butyl acetate.
4. The phosphotungstic heteropoly acid extractant of claim 3, wherein the volume ratio of the aromatic hydrocarbon solvent oil, the n-butanol and the butyl acetate is 0.4-0.6: 0.2-0.35: 0.1 to 0.25.
5. The phosphotungstic heteropoly acid extractant of claim 4, wherein the volume ratio of the aromatic hydrocarbon solvent oil, the n-butanol and the butyl acetate is 0.5: 0.35: 0.15.
6. the phosphotungstic heteropoly acid extractant of claim 1, wherein the aromatic hydrocarbon solvent oil is aromatic hydrocarbon solvent oil No. 200.
7. The extraction method of phosphotungstic heteropoly acid is characterized by comprising the following preparation steps:
s1, preparing a phosphotungstic heteropoly acid extracting agent for later use, wherein the phosphotungstic heteropoly acid extracting agent consists of a main extracting agent and aromatic solvent oil;
s2, carrying out reverse continuous contact on the phosphotungstic heteropoly acid solution and the phosphotungstic heteropoly acid extracting agent, leading out the mixed phosphotungstic heteropoly acid solution and the phosphotungstic heteropoly acid extracting agent, standing and layering.
8. The method of claim 7, wherein in step S2, the phosphotungstic heteropoly acid solution and the phosphotungstic heteropoly acid extractant are in reverse continuous contact in a pH balance medium.
9. The extraction method of phosphotungstic heteropoly acid as claimed in claim 7, wherein the step S2 includes:
s21, adding the phosphotungstic heteropoly acid extractant into CO under the condition of pressurization2Stirring in the fluid;
s22, mixing with CO2The phosphotungstic heteropoly acid extracting agent is in reverse continuous contact with the phosphotungstic heteropoly acid solution, and the pressure of the phosphotungstic heteropoly acid solution is less than that of the phosphotungstic heteropoly acid extracting agent.
10. The application of the aromatic hydrocarbon solvent oil is characterized in that the aromatic hydrocarbon solvent oil is used as a diluent of an extracting agent in the extraction process of phosphotungstic heteropoly acid.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111573734A (en) * | 2020-06-19 | 2020-08-25 | 厦门钨业股份有限公司 | Novel extracting agent and method for extracting tungsten from phosphotungstic heteropoly acid and converting tungsten into ammonium tungstate/sodium tungstate solution |
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|---|---|---|---|---|
| GB1013364A (en) * | 1962-10-26 | 1965-12-15 | Blair Burwell | Extraction of tungsten from tungsten-bearing ores |
| CN105349781A (en) * | 2015-12-09 | 2016-02-24 | 中国科学院上海有机化学研究所 | Method for removing iron through solvent extraction |
| CN106082343A (en) * | 2016-08-26 | 2016-11-09 | 中南大学 | A kind of purification process of phosphotungstic acid crystal |
| CN106277060A (en) * | 2016-08-26 | 2017-01-04 | 中南大学 | A kind of preparation method of phosphotungstic acid |
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2020
- 2020-03-11 CN CN202010167888.3A patent/CN111298476B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1013364A (en) * | 1962-10-26 | 1965-12-15 | Blair Burwell | Extraction of tungsten from tungsten-bearing ores |
| CN105349781A (en) * | 2015-12-09 | 2016-02-24 | 中国科学院上海有机化学研究所 | Method for removing iron through solvent extraction |
| CN106082343A (en) * | 2016-08-26 | 2016-11-09 | 中南大学 | A kind of purification process of phosphotungstic acid crystal |
| CN106277060A (en) * | 2016-08-26 | 2017-01-04 | 中南大学 | A kind of preparation method of phosphotungstic acid |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111573734A (en) * | 2020-06-19 | 2020-08-25 | 厦门钨业股份有限公司 | Novel extracting agent and method for extracting tungsten from phosphotungstic heteropoly acid and converting tungsten into ammonium tungstate/sodium tungstate solution |
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