High-selectivity ion pair type extraction agent and method for extracting wet-process phosphoric acid by using same

A high-selectivity, ion-pairing technology, applied in chemical instruments and methods, liquid solution solvent extraction, phosphorus compounds, etc., can solve the problems of unsuitable boiling point of extractant, unrecoverable, difficult to carry out or other problems, and achieve good chemistry and physics. Stability, widening the range of component selection, and reducing the effect of volatilization loss

Active Publication Date: 2014-10-01
陈锂
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] 1. Primary phosphoric acid needs to undergo a series of chemical methods to remove impurities before extraction, such as sulfate and some metal ions, which makes the process complicated;
[0006] 2. During the extraction process, the viscosity of the raffinate is too high, agglomerates or inorganic salts are precipitated, making the extraction process difficult or blocking the pipeline;
[0008] 4. The boiling point of each component of the extraction agent is not suitable, and the solvent loss per ton of product is large
If the boiling point is too high, it will not be recovered and will be lost with the acid liquid, such as tributyl phosphate; if the boiling point is too low, it will lose a lot during the evaporation of the acid liquid, such as isopropanol, diisopropyl ether or diisopropyl ether, etc. , in order to reduce solvent volatilization, low temperature extraction is often used, the process is complicated and the energy consumption is high;
[0009] 5. The selectivity of the extractant to phosphoric acid is low, and the yield of phosphoric acid is low, and it can only be extracted when the acid concentration of the raw material is high, such as cyclohexanone, methyl isobutyl ketone, etc.
[0010] my country is a country with a large output of wet-process phosphoric acid, and various enterprises are also keen on developing wet-process phosphoric acid purification processes. Due to the above-mentioned problems, only a few enterprises have achieved industrialization of the extraction agent process mainly based on tributyl phosphate, but they are faced with the problem of extraction Problems such as large dose consumption, low selectivity, and high production cost

Method used

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  • High-selectivity ion pair type extraction agent and method for extracting wet-process phosphoric acid by using same

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] Embodiment 1: select more representative middle and low-grade phosphate rock leaching acid in Hubei Province as raw material, and the thick phosphoric acid composition of the raw material after concentration and clarification is shown in Table 1:

[0041] Table 1 raw material crude phosphoric acid composition

[0042] composition

Fe 3+

Mg 2+

Al 3+

Ca 2+

SO 4 2-

F -

SiO 2

Cl -

P 2 o 5

Quality score (%)

0.37

1.64

0.78

0.06

6.43

1.64

0.18

0.006

42.14%

[0043] (1) Rough purification: concentrate the clarified wet-process crude phosphoric acid to P 2 o 5 The mass fraction is 48%, measure the fluoride ion concentration in crude phosphoric acid, press n(F - ): n(Na 2 CO 3 )=1:1.3 Add sodium carbonate for defluorination, react at 70°C for 2 hours, settle, take the supernatant liquid and add activated carbon for decolorization, filter to obtain a crude purified pho...

Embodiment 2

[0051] Embodiment 2, with embodiment 1, difference is:

[0052] (1) Rough purification: concentrate the clarified wet-process crude phosphoric acid to P 2 o 5 The mass fraction is 30%. After reacting at 50°C for 3 hours, decolorize with activated carbon and filter to obtain a rough purified phosphoric acid solution; the defluorination rate is 78.2%.

[0053] (2) Extraction and purification: the thick purified phosphoric acid solution of step (1) gained is countercurrently added to extractant, extractant: the volume ratio=3: 1 of rough purified phosphoric acid, carry out 7 grades of extractions at normal temperature, at the entrance of rough purified phosphoric acid Add sulfuric acid in the sixth stage, so that the concentration of sulfuric acid in the raffinate phase reaches 9.2mol / L; the mass fractions of the components of the extractant are: 6% dioctadecyldimethylammonium chloride, 60% n-butanol, 60% isooctanol 34%.

[0054] Extraction phase: washing phase volume ratio=20...

Embodiment 3

[0056] Embodiment 3, with embodiment 1, difference is:

[0057] (1) Rough purification: concentrate the clarified wet-process crude phosphoric acid to P 2 o 5 The mass fraction is 42%. After reacting at 60°C for 3 hours, decolorize with activated carbon and filter to obtain a rough purified phosphoric acid solution; the defluorination rate is 76.7%.

[0058] (2) Extraction and purification: the thick purified phosphoric acid solution of step (1) gained is countercurrently added to extractant, extractant: the volume ratio=2: 1 of rough purified phosphoric acid, carry out 7 grades of extractions at normal temperature, at the entrance of rough purified phosphoric acid Add sulfuric acid in the sixth stage, so that the concentration of sulfuric acid in the raffinate phase reaches 4.0mol / L; 70%.

[0059] Extraction phase: washing phase volume ratio=15: 1; According to the extraction phase after washing: the volume ratio of aqueous phase=8: 1 adds pure water and carries out four-s...

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Abstract

The invention discloses a high-selectivity ion pair type extraction agent and a method for extracting wet-process phosphoric acid by using the high-selectivity ion pair type extraction agent. The high-selectivity ion pair type extraction agent is prepared from the following components in mass fraction: 1-10% of aliphatic amine or quaternary ammonium salt, 20-79% of normal butanol, and 20-79% of isooctyl alcohol, n-butyl ether or high-carbon ketone. The method comprises the steps of defluorinating and decolorizing wet-process crude phosphoric acid, performing 6-10-level counter-current extraction on the extraction agent and the crude phosphoric acid with the ratio of (2-5):1, adding sulfuric acid in a 6-level or 7-level crude phosphoric acid inlet, washing extract phase, reextracting with deionized water to obtain strip liquid, purifying the strip liquid and concentrating to obtain industrial grade phosphoric acid. According to the invention, the ion pair type organic matter with strong polarity is used as extraction agent polarity regulator, has high extraction capacity and stable performance, can be cycled for a long time, can be used for extraction at room temperature and is energy-saving; the initial mass fraction of P2O5 in strip liquid is more than 38.0, the evaporation capacity of concentrated acid is low, the extraction rate is more than 86%, and more than 19kg of extraction agent is consumed by 85% phosphoric acid per ton.

Description

technical field [0001] The invention belongs to the technical field of phosphoric acid preparation, and in particular relates to a highly selective ion-pair type extractant and a method for extracting wet-process phosphoric acid with it. Background technique [0002] Phosphoric acid mainly has two production processes: thermal method and wet method. Thermal phosphoric acid is obtained by oxidizing and absorbing yellow phosphorus by electric furnace method, and the resulting phosphoric acid has a high purity; wet phosphoric acid is decomposing phosphate rock by sulfuric acid, and the obtained product contains magnesium, calcium, iron, aluminum, sulfate, Various impurities such as fluorosilicate radicals and fluoride ions vary with different ore sources. Therefore, wet-process phosphoric acid is generally used to manufacture phosphate fertilizers, and it is difficult to prepare phosphate products for other industries. Since wet-process phosphoric acid has lower energy consump...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01D11/04C01B25/234
Inventor 陈锂
Owner 陈锂
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