CN100542950C - Solvent extration is removed the method for impurity iron in the salt acid system raw phosphoric acid - Google Patents
Solvent extration is removed the method for impurity iron in the salt acid system raw phosphoric acid Download PDFInfo
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- CN100542950C CN100542950C CNB2007100352250A CN200710035225A CN100542950C CN 100542950 C CN100542950 C CN 100542950C CN B2007100352250 A CNB2007100352250 A CN B2007100352250A CN 200710035225 A CN200710035225 A CN 200710035225A CN 100542950 C CN100542950 C CN 100542950C
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Abstract
The invention discloses a kind of solvent extration and remove the method for impurity iron in the salt acid system raw phosphoric acid: 1) remove organic matter: with the raw phosphoric acid that the hydrochloric acid method makes, be 100 by mass ratio: 0.5-5 adds gac, and the organic impurity in the raw phosphoric acid is carried out adsorbing and removing; 2) extraction of iron: be 1 by organic phase/water volume ratio in raw phosphoric acid: 3-8 adds tributyl phosphate (TBP), in 25-85 ℃ water-bath, mix two phase liquid after preheating 5-30 minute, vibrated 5-20 minute, standing demix, separate the iron content extraction phase, continuous extraction progression is 3 grades, removes impurity iron in the salt acid system raw phosphoric acid, gets deironing phosphoric acid.The present invention has following beneficial effect, the one, phosphoric acid by the ratio of three grades of extractions of organic phase less than 15%, and the percentage extraction height of impurity iron, impurity iron can separate from phosphoric acid fully, the content that raw phosphoric acid purifies back iron reaches industrial phosphoric acid first grade quality standard; The 2nd, be applicable to the extraction of impurity iron when raw phosphoric acid concentration is not high, running cost is low, helps the exploitation of poor phosphate rock resource; The 3rd, solubleness is little in the TBP extraction agent water that adopts, and the solvent after the extraction can recycle after handling through the diluted acid back extraction; The 4th, adopt in the ground phosphate rock and the deironing of back extraction acid solution, have atom utilization height, economically viable advantage, gained biphosphate calcium solution is reusable edible also.
Description
Technical field
The present invention relates to purify in the phosphoric acid by wet process technology of iron contamination, specially refer to the method for from the wet method crude phosphoric acid of poor phosphorus ore production, removing impurity iron with the salt acid system.
Background technology
Our times energy demand day is becoming tight, and the thermal phosphoric acid price rises steadily, and Wet-process Phosphoric Acid Production has the gesture that replaces thermal phosphoric acid production.But poor phosphorus ore proportion is increasing in the phosphate rock resource, foreign matter content height in the phosphoric acid by wet process, especially impurity such as iron, aluminium and magnesium can cause the formation of insoluble sludge and the increase of phosphoric acid viscosity, and the existence of iron has changed the color of product, badly influences the quality and the purposes of phosphoric acid.
Though it is multiple that the method for purification iron has, in the raw phosphoric acid of hydrochloric acid method preparation, Fe
3+With Cl
-Coordination forms FeCl
3Molecule or FeCl
4 -Anionic form, and each species associates with on every side phosphoric acid molecules, is difficult to reach effective isolating purpose by means such as ion-exchange and charcoal absorptions.The ability of EDTA complexing-adsorption method for purifying iron is strong, but its cost height.Solvent precipitation adopts water-soluble organic alcohol solvent, requires pending phosphoric acid P
2O
5The content height, the solvent usage quantity is big, and further separating with phosphoric acid needs distillation.
Summary of the invention
The purpose of this invention is to provide a kind of solvent extraction method of removing impurity iron in the salt acid system raw phosphoric acid.
The objective of the invention is to realize in the following way: a kind of solvent extration is removed the method for impurity iron in the salt acid system raw phosphoric acid:
1), removes organic matter: with the raw phosphoric acid that the hydrochloric acid method makes, be that 100:0.5-5 adds gac, the organic impurity in the raw phosphoric acid is carried out adsorbing and removing by mass ratio;
2), the extraction of iron: in raw phosphoric acid, be that 1:3-8 adds tributyl phosphate (tributyl phosphate by organic phase/water volume ratio, be called for short TBP), in 25-85 ℃ water-bath, mix two phase liquid after preheating 5-30 minute, vibrated 5-20 minute, standing demix separates the iron content extraction phase, and continuous extraction progression is 3 grades, remove impurity iron in the salt acid system raw phosphoric acid, get deironing phosphoric acid.
Isolating iron content extraction phase is carried out subsequent disposal:
1), the back extraction of iron: add the hydrochloric acid of 0.0001-0.001mol/L by organic phase/water volume ratio 1:0.3-3 in the iron content extraction phase, under 25-85 ℃, vibrated 5-20 minute, standing demix is isolated the iron content water, and continuous extraction progression is the 2-3 level;
2), use the ground phosphate rock deironing: add ground phosphate rock, temperature of reaction 50-100 ℃, pH=3-6, the solution of oxyhydroxide that precipitation separation taps a blast furnace and phosphoric acid calcium dihydrogen at the iron content aqueous phase.
The present invention has following beneficial effect, the one, TBP is strong to the extracting power of iron ion, iron is preferentially extracted in raw phosphoric acid solution, simultaneously by the phosphoric acid amount of three grades of extractions of organic phase less than 15%, impurity iron can separate from phosphoric acid fully, and the content that raw phosphoric acid purifies back iron reaches industrial phosphoric acid first grade quality standard (GB/T 2091-2003); The 2nd, be applicable to the extraction of impurity iron when raw phosphoric acid concentration is not high, running cost is low, helps the exploitation of poor phosphate rock resource; The 3rd, solubleness is little in the TBP extraction agent water that adopts, and is 0.42g/L in the time of 25 ℃, and the solvent after the extraction can recycle after handling through the diluted acid back extraction; The 4th, adopt in the ground phosphate rock and the deironing of back extraction acid solution, have atom utilization height, economically viable advantage, gained biphosphate calcium solution is reusable edible also.
Description of drawings
Fig. 1 is a process flow sheet of removing impurity iron in salt acid system raw phosphoric acid of the present invention.
Embodiment
The present invention will be further described below in conjunction with embodiment:
Embodiment 1:
1), with density d=1.3157, P
2O
5Content is that 7.02% salt acid system raw phosphoric acid is that 100:1 adds gac by mass ratio, and the organic impurity in the raw phosphoric acid is carried out adsorbing and removing; 2) in raw phosphoric acid, be that 1:5 adds tributyl phosphate, by organic phase/water volume ratio, preheating mixed two phase liquid after 10 minutes in 30 ℃ water-bath, vibrated 10 minutes, standing demix, separate the iron content extraction phase, continuous extraction progression is 3 grades, removes impurity iron in the salt acid system raw phosphoric acid, gets deironing phosphoric acid.
1), add the hydrochloric acid of 0.0001mol/L by organic phase/water volume ratio 1:1 in the iron content extraction phase isolating iron content extraction phase is handled:, 35 ℃ of vibrations 10 minutes down, standing demix is isolated the iron content water, and continuous extraction progression is 2 grades; 2), add ground phosphate rock, 60 ℃ of temperature of reaction, pH=4, the solution of oxyhydroxide that precipitation separation taps a blast furnace and phosphoric acid calcium dihydrogen at the iron content aqueous phase.
The clearance of iron in the mass percent concentration of iron ion in two-phase and thick acid when table 1 is three grades of extractions of embodiment 1 usefulness TBP:
Table 1
| Extraction progression | Aqueous phase Fe 3+(％) | Fe in the organic phase 3+(％) | Fe 3+Clearance (%) |
| The one-level extraction | 0.222 | 2.980 | 68.800 |
| The secondary extraction | 0.039 | 1.135 | 94.545 |
| Three grades of extractions | 0.000 | 0.193 | 100.000 |
Embodiment 2:
1), with density d=1.3157, P
2O
5Content is that 7.02% salt acid system raw phosphoric acid is that 100:1 adds gac by mass ratio, and the organic impurity in the raw phosphoric acid is carried out adsorbing and removing; 2) in raw phosphoric acid, be that 1:6 adds tributyl phosphate, by organic phase/water volume ratio, preheating mixed two phase liquid after 10 minutes in 40 ℃ water-bath, vibrated 10 minutes, standing demix, separate the iron content extraction phase, continuous extraction progression is 3 grades, removes impurity iron in the salt acid system raw phosphoric acid, gets deironing phosphoric acid.
1), add the hydrochloric acid of 0.0001mol/L by organic phase/water volume ratio 1:1 in the iron content extraction phase isolating iron content extraction phase is handled:, 35 ℃ of vibrations 10 minutes down, standing demix is isolated the iron content water, and continuous extraction progression is 2 grades; 2), add ground phosphate rock, 60 ℃ of temperature of reaction, pH=4, the solution of oxyhydroxide that precipitation separation taps a blast furnace and phosphoric acid calcium dihydrogen at the iron content aqueous phase.
The clearance of iron in the mass percent concentration of iron ion in two-phase and thick acid when table 2 is three grades of extractions of embodiment 2 usefulness TBP:
Table 2
| Extraction progression | Aqueous phase Fe 3+(％) | Fe in the organic phase 3+(％) | Fe 3+Clearance (%) |
| The one-level extraction | 0.192 | 3.565 | 72.721 |
| The secondary extraction | 0.033 | 1.207 | 95.338 |
| Three grades of extractions | 0.000 | 0.268 | 100.000 |
Claims (2)
1, a kind of solvent extration is removed the method for impurity iron in the salt acid system raw phosphoric acid, it is characterized in that:
1), removes organic matter: with the raw phosphoric acid that the hydrochloric acid method makes, be that 100:0.5-5 adds gac, the organic impurity in the raw phosphoric acid is carried out adsorbing and removing by mass ratio;
2), the extraction of iron: in raw phosphoric acid, be that 1:3-8 adds tributyl phosphate by organic phase/water volume ratio, in 25-85 ℃ water-bath, mix two phase liquid after preheating 5-30 minute, vibrated 5-20 minute, standing demix, separate the iron content extraction phase, continuous extraction progression is 3 grades, removes impurity iron in the salt acid system raw phosphoric acid, gets deironing phosphoric acid.
2, a kind of solvent extration according to claim 1 is removed the method for impurity iron in the salt acid system raw phosphoric acid, it is characterized in that: isolating iron content extraction phase is handled:
1), the back extraction of iron: add the hydrochloric acid of 0.0001-0.001mol/L by organic phase/water volume ratio 1:0.3-3 in the iron content extraction phase, under 25-85 ℃, vibrated 5-20 minute, standing demix is isolated the iron content water, and continuous extraction progression is the 2-3 level;
2), use the ground phosphate rock deironing: add ground phosphate rock, temperature of reaction 50-100 ℃, pH=3-6, the solution of oxyhydroxide that precipitation separation taps a blast furnace and phosphoric acid calcium dihydrogen at the iron content aqueous phase.
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| CNB2007100352250A CN100542950C (en) | 2007-06-27 | 2007-06-27 | Solvent extration is removed the method for impurity iron in the salt acid system raw phosphoric acid |
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| CNB2007100352250A CN100542950C (en) | 2007-06-27 | 2007-06-27 | Solvent extration is removed the method for impurity iron in the salt acid system raw phosphoric acid |
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| CN110655054B (en) * | 2018-06-29 | 2023-03-31 | 上海麟光新材料科技有限公司 | Preparation method of optical-grade aluminum dihydrogen phosphate |
| CN110759344A (en) * | 2019-11-29 | 2020-02-07 | 徐州天正活性炭厂 | Method for removing iron from phosphoric acid in production of activated carbon by phosphoric acid method |
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Non-Patent Citations (4)
| Title |
|---|
| 湿法磷酸净化的生产新工艺. 王邵东等.贵州化工，第30卷第2期. 2005 |
| 湿法磷酸净化的生产新工艺. 王邵东等.贵州化工，第30卷第2期. 2005 * |
| 盐酸法湿法磷酸中磷酸的协同萃取分离. 傅洵等.化学研究与应用，第14卷第3期. 2002 |
| 盐酸法湿法磷酸中磷酸的协同萃取分离. 傅洵等.化学研究与应用，第14卷第3期. 2002 * |
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