CN103332665B - A kind of method of imurity-removal ion from the organic solvent of load phosphoric acid - Google Patents
A kind of method of imurity-removal ion from the organic solvent of load phosphoric acid Download PDFInfo
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- CN103332665B CN103332665B CN201310285474.0A CN201310285474A CN103332665B CN 103332665 B CN103332665 B CN 103332665B CN 201310285474 A CN201310285474 A CN 201310285474A CN 103332665 B CN103332665 B CN 103332665B
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Abstract
The invention discloses the method for a kind of imurity-removal ion from the organic solvent of load phosphoric acid belonging to technical field of chemical separation.The method uses phosphoric acid salt or its aqueous solution 1:(10-400 in mass ratio) contact fully and mass transfer at 10-70 DEG C with the organic solvent of load phosphoric acid, but the organic solvent of the load phosphoric acid be purified that carries out being separated.The method single-stage just can realize higher metal ion clearance, and phosphoric acid loss rate is low simultaneously, can simplify the operation of phosphoric acid by wet process extraction phase purification and raise the efficiency.<!--1-->
Description
Technical field
The invention belongs to technical field of chemical separation, particularly a kind of method of imurity-removal ion from the organic solvent of load phosphoric acid.
Background technology
Phosphoric acid is as a kind of important mineral acid, and at chemical industry, food, the industries such as electronics have a wide range of applications.Current phosphoric acid production method mainly contains Re Fa and wet method two kinds.Thermal phosphoric acid obtains purer phosphoric acid through oxidative absorption after producing yellow phosphorus by electric furnace process, but technique power consumption is large, and cost is high, and production process produces a large amount of dust and toxic gas.Therefore, in phosphoric acid and phosphate production, thermal phosphoric acid technique just gradually replace by Wet Processes of Phosphoric Acid.Wet Processes of Phosphoric Acid mainly utilizes mineral acid (as sulfuric acid) decomposing phosphate rock stone to obtain raw phosphoric acid, then obtains phosphoric acid product through a series of purifying step.Foreign matter content due to raw phosphoric acid is high and complicated, and the level of purification process has great effect to production cost and quality product.The purifying method of current phosphoric acid by wet process mainly contains chemical precipitation method, solvent precipitation, ion-exchange-resin process, crystallization process and solvent extration.Due to solvent extration comparatively speaking production technique and equipment fairly simple, energy consumption is low, and throughput is large, good separating effect, environmental pollution is little, and production process is easy to automatization and serialization and is beneficial to comprehensive utilization of resources, and that applies in large-scale industrial production is the most extensive.
Solvent extraction technology is mainly concerned with extraction, washing, back extraction three steps.Extraction step can remove a large amount of foreign ion, but because phosphoric acid and water have very strong affinity interaction, still a lot of to the water in organic solvent and foreign ion by common extraction with phosphoric acid, and the task of purge step is exactly the foreign ion will removed as much as possible in the organic solvent of load phosphoric acid.In current production, general pure water or the higher phosphoric acid product of the purity that obtains of using is as washing composition, although the foreign ion in organic solvent effectively can be removed, but because the selectivity of washing composition to phosphoric acid and foreign ion is limited, deposit major defect both ways: one be need extremely compare with more theoretical stage under operate, high to the requirement of separating device; Two is that the loss of phosphoric acid productive rate is larger.Therefore, the method tool developing highly selective imurity-removal ion from the organic solvent of load phosphoric acid is of great significance.
Summary of the invention
The present invention is directed to wet phosphoric acid purifying process, propose a kind of method of imurity-removal ion from the organic solvent of load phosphoric acid.
A method for imurity-removal ion from the organic solvent of load phosphoric acid, uses phosphoric acid salt or its aqueous solution to contact fully and mass transfer with the organic solvent of load phosphoric acid, the organic solvent of the load phosphoric acid that then carrying out is separated is purified.
Described organic solvent is methyl iso-butyl ketone (MIBK), propyl carbinol, primary isoamyl alcohol or isopropyl ether.
In the organic solvent of described load phosphoric acid, phosphorus acid content is (with H
3pO
4wt% calculate) for the content of 2-20wt%, Fe be 5-300ppm.
Described phosphoric acid salt is one or more of sodium salt, sylvite or ammonium salt containing phosphate radical, phosphoric acid one hydrogen root or dihydrogen phosphate.
The concentration of described aqueous phosphatic is not less than 20% of saturation concentration.
The mass ratio of the organic solvent of described phosphoric acid salt or its aqueous solution and load phosphoric acid is 1:(10-400).
Described temperature of carrying out contact and mass transfer is fully 10-70 DEG C.
Beneficial effect of the present invention is: (1) phosphatic wide material sources, also can be monoammonium phosphate and the diammonium phosphate of producing coproduction in process phosphoric acid, substantially not increase production cost; (2) because the concentration of phosphate radical in phosphoric acid salt or its aqueous solution is high, by phosphate radical equilibrium-limited, during contact, phosphoric acid not easily runs off from the organic solvent of load phosphoric acid, is conducive to improving yield; (3) phosphoric acid salt has strong hydration, can reduce the water-content in organic solvent, is conducive to removing occurring to assist extraction effect to enter the foreign ion of organic solvent with water, is particularly conducive to the clearance improving metal ion; (4) no matter be phosphoric acid salt or its aqueous solution, the interfacial tension alternate with organic solvent is all higher, can complete fast and be separated, thus enhance productivity; (5) process choosing removing ion is high, can simplify the requirement to equipment, reduces equipment cost and running cost.
Embodiment
Below by specific examples, the present invention is further described.
Embodiment 1
(1) methyl iso-butyl ketone (MIBK) taking 300g load phosphoric acid is placed in 500ml Erlenmeyer flask, in mass ratio for 1:30 adds the lower primary ammonium phosphate saturated aqueous solution of 10g40 DEG C.
(2) vibrate 12h under 40 DEG C of constant-temperature tables, until the contact of two strands of materials and mass transfer fully after, the methyl iso-butyl ketone (MIBK) of the load phosphoric acid be purified that carries out after standing 5h being separated.
Embodiment 2
(1) primary isoamyl alcohol of 300g load phosphoric acid is claimed to be placed in 500ml Erlenmeyer flask, in mass ratio for 1:100 adds the aqueous solution that 3g contains 34% primary ammonium phosphate.
(2) vibrate 12h under 60 DEG C of constant-temperature tables, until the contact of two strands of materials and mass transfer fully after, the primary isoamyl alcohol of the load phosphoric acid be purified that carries out after standing 5h being separated.
Embodiment 3
(1) methyl iso-butyl ketone (MIBK) taking 300g load phosphoric acid is placed in 500ml Erlenmeyer flask, in mass ratio for 1:30 adds 10g primary ammonium phosphate solid.
(2) in the water bath with thermostatic control of 10 DEG C is stirred, stir 12h, until the contact of two strands of materials and mass transfer abundant after, standing 5h carries out being separated the methyl iso-butyl ketone (MIBK) of the load phosphoric acid be purified.
Embodiment 4
(1) isopropyl ether taking 300g load phosphoric acid is placed in 500ml Erlenmeyer flask, in mass ratio for 1:100 adds 3g primary ammonium phosphate solid.
(2) vibrate 12h under 40 DEG C of constant-temperature tables, until the contact of two strands of materials and mass transfer fully after, the isopropyl ether of the load phosphoric acid be purified that carries out after standing 5h being separated.
Embodiment 5
(1) methyl iso-butyl ketone (MIBK) taking 600g load phosphoric acid is placed in 1000ml Erlenmeyer flask, in mass ratio for 1:400 adds 1.5g potassium phosphate,monobasic solid.
(2) vibrate 12h under 40 DEG C of constant-temperature tables, until the contact of two strands of materials and mass transfer fully after, the methyl iso-butyl ketone (MIBK) of the load phosphoric acid be purified that carries out after standing 5h being separated.
Embodiment 6
(1) isopropyl ether taking 300g load phosphoric acid is placed in 500ml Erlenmeyer flask, in mass ratio for 1:10 adds 30g potassium primary phosphate solid.
(2) vibrate 12h under 25 DEG C of constant-temperature tables, until the contact of two strands of materials and mass transfer fully after, the isopropyl ether of the load phosphoric acid be purified that carries out after standing 5h being separated.
Embodiment 7
(1) primary isoamyl alcohol taking 300g load phosphoric acid is placed in 500ml Erlenmeyer flask, in mass ratio for 1:100 adds the aqueous solution that 3g contains 30% ammonium phosphate.
(2) vibrate 12h under 70 DEG C of constant-temperature tables, until the contact of two strands of materials and mass transfer fully after, the primary isoamyl alcohol of the load phosphoric acid be purified that carries out after standing 5h being separated.
Embodiment 8
(1) propyl carbinol taking 300g load phosphoric acid is placed in 500ml Erlenmeyer flask, adds the disodium-hydrogen saturated aqueous solution at 2g50 DEG C in mass ratio for 1:150.
(2) vibrate 12h under 50 DEG C of constant-temperature tables, until the contact of two strands of materials and mass transfer fully after, the propyl carbinol of the load phosphoric acid be purified that carries out after standing 5h being separated.
Embodiment 9
(1) methyl iso-butyl ketone (MIBK) taking 320g load phosphoric acid is placed in 500ml Erlenmeyer flask, contains 50% disodium-hydrogen and 50% SODIUM PHOSPHATE, MONOBASIC mixing salt solid in mass ratio for 1:80 adds 4g.
(2) vibrate 12h under 40 DEG C of constant-temperature tables, until the contact of two strands of materials and mass transfer fully after, the methyl iso-butyl ketone (MIBK) of the load phosphoric acid be purified that carries out after standing 5h being separated.
Embodiment 10
(1) propyl carbinol taking 400g load phosphoric acid is placed in 500ml Erlenmeyer flask, contains SODIUM PHOSPHATE, MONOBASIC solid in mass ratio for 1:200 adds 4g.
(2) vibrate 12h under 40 DEG C of constant-temperature tables, until the contact of two strands of materials and mass transfer fully after, the propyl carbinol of the load phosphoric acid be purified that carries out after standing 5h being separated.
Embodiment 11
(1) primary isoamyl alcohol taking 400g load phosphoric acid is placed in 500ml Erlenmeyer flask, in mass ratio for 1:200 adds the aqueous solution that 4g contains 14% SODIUM PHOSPHATE, MONOBASIC.
(2) vibrate 12h under 35 DEG C of constant-temperature tables, until the contact of two strands of materials and mass transfer fully after, the primary isoamyl alcohol of the load phosphoric acid be purified that carries out after standing 5h being separated.
Embodiment 12
(1) primary isoamyl alcohol taking 400g load phosphoric acid is placed in 500ml Erlenmeyer flask, in mass ratio for 1:200 adds the aqueous solution that 4g contains 34% SODIUM PHOSPHATE, MONOBASIC.
(2) vibrate 12h under 35 DEG C of constant-temperature tables, until the contact of two strands of materials and mass transfer fully after, the primary isoamyl alcohol of the load phosphoric acid be purified that carries out after standing 5h being separated.
The phosphoric acid of the organic solvent of each embodiment step (1) load phosphoric acid and impurity (in general, the removal realizing Fe is slightly difficult compared with other impurity, therefore with Fe is only to investigate object) content is as shown in table 1.The clearance data of the various embodiments described above impurity F e are as shown in table 2.
The phosphoric acid of the organic solvent of table 1 each embodiment step (1) load phosphoric acid and impurity (for Fe) content
The clearance of table 2 each embodiment washing process Fe
| Fe clearance/% | |
| Embodiment 1 | 98.7 |
| Embodiment 2 | 96.2 |
| Embodiment 3 | 98.8 |
| Embodiment 4 | 97.4 |
| Embodiment 5 | 92.9 |
| Embodiment 6 | 99.6 |
| Embodiment 7 | 95.3 |
| Embodiment 8 | 94.2 |
| Embodiment 9 | 97.1 |
| Embodiment 10 | 94.7 |
| Embodiment 11 | 93.3 |
| Embodiment 12 | 94.1 |
Claims (2)
1. the method for an imurity-removal ion from the organic solvent of load phosphoric acid, in the organic solvent of described load phosphoric acid, phosphorus acid content is 2-20wt%, it is characterized in that, phosphoric acid salt or its aqueous solution is used to contact fully and mass transfer with the organic solvent of load phosphoric acid, the organic solvent of the load phosphoric acid that then carrying out is separated is purified; The mass ratio of the organic solvent of phosphoric acid salt or its aqueous solution and load phosphoric acid is 1:(30-400); Described temperature of carrying out contact and mass transfer is fully 10-70 DEG C; Under this temperature condition, the concentration of described aqueous phosphatic is not less than 20% of saturated solution concentration under relevant temperature; Described phosphoric acid salt is one or more of sodium salt, sylvite or ammonium salt containing phosphate radical, phosphoric acid one hydrogen root or dihydrogen phosphate; Described organic solvent is methyl iso-butyl ketone (MIBK), propyl carbinol, primary isoamyl alcohol or isopropyl ether.
2. method according to claim 1, is characterized in that, in the organic solvent of described load phosphoric acid, the content of Fe is 5-300ppm.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4154805A (en) * | 1976-10-29 | 1979-05-15 | Toyo Soda Manufacturing Co., Ltd. | Phosphoric acid purification |
| CN1217705A (en) * | 1997-02-03 | 1999-05-26 | 吉乌里尼化学两合公司 | Wet-process technique for refiining phosphoric acid |
| CN1994871A (en) * | 2006-12-13 | 2007-07-11 | 云南省化工研究院 | Method for preparing technical grade phosphate using wet method phosphoric acid as raw material |
| CN101525131A (en) * | 2009-04-10 | 2009-09-09 | 武汉工程大学 | Method for extract phase phosphoric acid back extraction in the course of extracting wet-process phosphoric acid by an organic solvent method |
-
2013
- 2013-07-09 CN CN201310285474.0A patent/CN103332665B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4154805A (en) * | 1976-10-29 | 1979-05-15 | Toyo Soda Manufacturing Co., Ltd. | Phosphoric acid purification |
| CN1217705A (en) * | 1997-02-03 | 1999-05-26 | 吉乌里尼化学两合公司 | Wet-process technique for refiining phosphoric acid |
| CN1994871A (en) * | 2006-12-13 | 2007-07-11 | 云南省化工研究院 | Method for preparing technical grade phosphate using wet method phosphoric acid as raw material |
| CN101525131A (en) * | 2009-04-10 | 2009-09-09 | 武汉工程大学 | Method for extract phase phosphoric acid back extraction in the course of extracting wet-process phosphoric acid by an organic solvent method |
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