Method of solvent extraction purification of wet method phosphoric acid produced from medium and low grade phosphosus ore

A wet-process phosphoric acid, low-grade technology, used in chemical instruments and methods, phosphorus compounds, inorganic chemistry, etc., can solve problems such as large liquids, reduced equipment capacity, inability to carry out, etc., to improve extraction rate, reduce burden, The effect of increasing the concentration

Active Publication Date: 2006-03-29
HUAZHONG NORMAL UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The method described in the Chinese patent CN1217705A needs to be operated at a temperature of 30-80°C, which in itself increases the consumption of energy and the volatilization of the extraction agent; and a large amount of solvents that are completely soluble in water are used during extraction, which makes the burden of solvent recovery considerable. heavy, resulting in higher production costs
[0015] Due to the high content of impurities Mg, Al, Fe, etc. in Hubei original acid, if it is concentrated to 45wt%~50t%P according to the method of US4377562 2 o 5 Phosphoric acid for extraction will cause the aqueous phase to become a mass of colloids or liquids with high viscosity and cannot be carried out
Adding sulfuric acid during extraction can indeed improve the fluidity of the aqueous phase, but almost every level needs to be added from the third level of the water phase inlet, which will increase the difficulty of the subsequent washing steps; for the washing of the extracted organic phase, US4377562 Ten-stage countercurrent washing is used, which not only requires a large equipment capacity, but also consumes a large amount of phosphoric acid used for washing; although it can reduce the impurity content in the product phosphoric acid, it will also seriously reduce the production capacity of the equipment, because the product phosphoric acid is used in large quantities for washing with acid

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  • Method of solvent extraction purification of wet method phosphoric acid produced from medium and low grade phosphosus ore

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Experimental program
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Effect test

Embodiment 1

[0037] The pretreated 42wt%P 2 o 5 The wet-process phosphoric acid is extracted with a mixed solvent of n-butanol and methyl isobutyl ketone, and the volume ratio of n-butanol: methyl isobutyl ketone in the mixed solvent is 3: 7, adding 3% isoamyl alcohol to increase the volume of the mixed solvent of alcohol and ketone Efficacy agent, after seven-stage countercurrent extraction, the extraction ratio O:A is 6:1, four-stage countercurrent washing, washing water with 600g / l H 3 PO 4 +60g / l Na 2 CO 3 The aqueous solution, washing ratio O:A is 6:1, three-stage countercurrent back extraction, back extraction ratio O:A is 6:1, concentration, deSO 4 2- , decolorized, filtered, and concentrated again to obtain 85wt% phosphoric acid. The test process conditions and product quality are shown in Table 1.

Embodiment 2

[0039] The pretreated 43wt%P 2 o 5 The wet-process phosphoric acid is extracted with a mixed solvent of n-butanol and methyl isobutyl ketone, and the volume ratio of n-butanol in the mixed solvent: methyl isobutyl ketone is 2: 8, adding 5% isoamyl alcohol to increase the volume of the mixed solvent of alcohol and ketone Efficacy agent, after seven-stage countercurrent extraction, the extraction ratio O:A is 2.5:1, five-stage countercurrent washing, washing water with 600g / l H 3 PO 4 +60g / l Na 2 CO 3 The aqueous solution, washing ratio O:A is 8.5:1, five-stage countercurrent back extraction, back extraction ratio O:A is 4:1, concentration, deSO 4 2- , decolorized, filtered, and concentrated again to obtain 85wt% phosphoric acid. The test process conditions and product quality are shown in Table 1.

Embodiment 3

[0041] The pretreated 43wt%P 2 o 5 The wet-process phosphoric acid is extracted with a mixed solvent of n-butanol and methyl isobutyl ketone, and the volume ratio of n-butanol in the mixed solvent: methyl isobutyl ketone is 3: 7, adding 4% isoamyl alcohol by volume of the mixed solvent of alcohol and ketone, After ten stages of countercurrent extraction, the extraction ratio O:A is 3:1, five stages of countercurrent washing, washing water with 600g / l H 3 PO 4 +60g / l Na 2 CO 3 , washing ratio O:A is 6.5:1, four-stage countercurrent back extraction, back extraction ratio O:A is 6:1, concentration, deSO 4 2- , decolorized, filtered, and concentrated again to obtain 85wt% phosphoric acid. The test process conditions and product quality are shown in Table 1.

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Abstract

A process for preparing wet phosphoric acid from medium-or low-grade phosphorus are through solvent extracting and purifying includes such steps as concentrating the crude wet phosphoric acid, defluorinating, desulfurizing, decoloring, filtering, counter current extracting in the mixture of n-butanol, methylisobutyl ketone and synergist by 7-10 stages while adding sulfuric acid at the 3rd or the 7th stage, counter current washing with phosphoric acid solution containing Na salt by 4-5 stages, counter-current reverse extracting of organic phase with distilled water by 3-5 stages, concentrating, recovering solvent, decoloring, filtering, adding the phosphoric acid solution of BaCO3 for removing ''SO4'' radicals, decoloring, filtering and concentrating.

Description

technical field [0001] The invention relates to the refining technology of wet-process phosphoric acid, in particular to the refining technology of solvent extraction wet-process phosphoric acid. Background technique [0002] At present, the world's energy shortage has caused the price of thermal phosphoric acid to rise continuously; in my country, phosphate rocks are mainly of medium and low grades, and the reserves of high-grade phosphoric rocks are not much, so wet-process phosphoric acid has gradually replaced thermal phosphoric acid. Wet-process phosphoric acid, especially the wet-process phosphoric acid produced with medium and low-grade phosphate rock, has high impurity content, and its purification is inevitable. There are many purification methods, such as chemical precipitation, ion exchange, crystallization, solvent precipitation, solvent extraction and so on. Among them, solvent extraction is the most effective method at present. For 42wt%~54wt%P 2 o 5 For hi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B25/234C01B25/235C01B25/237
Inventor 侯炎学黄华郭荣伟
Owner HUAZHONG NORMAL UNIV
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