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Extraction agent for preparing industrial phosphoric acid through hydrochloric acid method and extraction method thereof

A technology of industrial phosphoric acid and hydrochloric acid method, which is applied in chemical instruments and methods, phosphorus compounds, inorganic chemistry, etc. It can solve the problems that are not conducive to large-scale industrial production, the industrial production has not been realized, and the extraction efficiency is not high, so as to save energy consumption and solvent loss, moderate boiling point, and improved extraction efficiency

Active Publication Date: 2017-01-25
HUBEI SANNING CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the extractant used in this method can preferentially extract Fe 3+ with Cl - The complexes formed, resulting in the finished Fe phosphate 3+ On the other hand, it is necessary to carry out two concentration and two extractions, and after the second concentration, the temperature must be lowered to below 10°C before the second extraction can be carried out, resulting in high energy consumption
The shortcomings of large investment, low efficiency of impurity removal, high risk, and high energy consumption are not conducive to large-scale industrial production
Chinese patent 201110006702 discloses a method of one-step hydrochloric acid extraction to produce industrial phosphoric acid from medium and low-grade phosphate rocks. This method uses hydrochloric acid to decompose phosphate rocks, firstly prepare calcium dihydrogen phosphate chloride, and then add dilute phosphoric acid for beating, and then filter and purify Finally, it is beaten and dissolved with hydrochloric acid, extracted with tributyl phosphate, concentrated, and decolorized to obtain industrial phosphoric acid. This method has problems such as low extraction efficiency and large loss in practical application, and has not been realized in industrial production so far.

Method used

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  • Extraction agent for preparing industrial phosphoric acid through hydrochloric acid method and extraction method thereof
  • Extraction agent for preparing industrial phosphoric acid through hydrochloric acid method and extraction method thereof
  • Extraction agent for preparing industrial phosphoric acid through hydrochloric acid method and extraction method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0026] Take hydrochloric acid with a mass concentration of about 21% and add it to the acidolysis tank, and then add rock phosphate powder under stirring. React under strong stirring at 50° C. for 2 hours, and filter after the reaction to obtain an acidolysis solution.

[0027] Concentrate the clarified acid solution to H 3 PO 4 With a mass fraction of about 20%, add an appropriate amount of sodium carbonate for defluorination, react at 70°C for 2 hours, settle, take the supernatant, add activated carbon to decolorize, filter, and obtain a crude purified phosphoric acid solution.

[0028] The above crude purified phosphoric acid solution is countercurrently added to the extractant of the present invention, the volume ratio of extractant: crude purified phosphoric acid is 1:1, and six-stage countercurrent extraction is carried out at room temperature. The mass fraction of each component of the extractant is: 30% of tributyl phosphate, 40% of n-butanol, 20% of isopropyl ether,...

Embodiment 2

[0035] Take hydrochloric acid with a mass concentration of about 21% and add it to the acidolysis tank, and then add rock phosphate powder under stirring. React under strong stirring at 60°C for 0.5 hours, and filter after the reaction to obtain an acidolysis solution.

[0036] Concentrate the clarified acid solution to H 3 PO 4 With a mass fraction of about 25%, add an appropriate amount of sodium carbonate for defluorination, react at 70°C for 2 hours, settle, take the supernatant liquid and add activated carbon to decolorize it, and filter to obtain a crude purified phosphoric acid solution.

[0037] The above crude purified phosphoric acid solution is countercurrently added to the extractant of the present invention, the volume ratio of extractant: crude purified phosphoric acid is 2:1, and six-stage countercurrent extraction is carried out at room temperature. The mass fraction of each component of the extractant is: 15% of tributyl phosphate, 30% of isopropanol, 30% of...

Embodiment 3

[0044] Take hydrochloric acid with a mass concentration of about 21% and add it to the acidolysis tank, and then add rock phosphate powder under stirring. React under strong stirring at 50° C. for 2 hours, and filter after the reaction to obtain an acidolysis solution.

[0045] Concentrate the clarified acid solution to H 3 PO 4 With a mass fraction of about 20%, add an appropriate amount of sodium carbonate for defluorination, react at 70°C for 2 hours, settle, take the supernatant, add activated carbon to decolorize, filter, and obtain a crude purified phosphoric acid solution.

[0046] The above crude purified phosphoric acid solution is countercurrently added to the extractant of the present invention, the volume ratio of extractant: crude purified phosphoric acid is 3:1, and six-stage countercurrent extraction is carried out at room temperature. The mass fraction of each component of the extractant is: 40% of n-butanol, 30% of diisobutyl ketone, 20% of n-butyl ether, an...

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Abstract

The invention discloses an extraction agent for preparing industrial phosphoric acid through a hydrochloric acid method and an extraction method thereof. The extraction agent comprises, by mass, 10-50% of one or two of tributyl phosphate or tributoxy ethyl phosphate, 15-40% of one or multiple of n-butyl alcohol, isooctanol, cyclohexanol, isopropanol and isoamylol, 10-30% of one or two of n-butyl ether, isopropyl ether and diisopropyl ether, 5-30% of one or multiple of high-carbon ketone, aliphatic amine or quaternary ammonium salt and 1-10% of one or multiple of oil-based polyoxyethylene ether phosphate, octyl sodium sulfate, alpha-alkenyl sodium sulfonate, sodium lignin sulfonate, stearyl sulfo succinamide disodium and lauryl ammonium sulfate. The extraction agent is wide in application condition, low in solvent loss and convenient to recycle, and extraction rate can reach higher than 80%.

Description

technical field [0001] The invention relates to the technical field of phosphoric acid preparation, in particular to a composite extractant used in the preparation of industrial phosphoric acid by a hydrochloric acid method. Background technique [0002] Phosphoric acid is an important chemical raw material, which is widely used in chemical fertilizer, food, paint, electronic industry and other industries. Phosphoric acid mainly has two production processes: thermal method and wet method. Thermal phosphoric acid is obtained by oxidizing and absorbing yellow phosphorus after preparing yellow phosphorus by electric furnace method. The obtained phosphoric acid has high purity, but it requires high raw materials and consumes a lot of energy. Wet-process phosphoric acid uses acid to decompose phosphate rock and obtain phosphoric acid after solid-liquid separation. It has the advantages of wide adaptability and low energy consumption. Typical wet-process phosphoric acid uses sul...

Claims

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Application Information

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IPC IPC(8): C01B25/46
CPCC01B25/465C01B25/462C01B25/463C01B25/464
Inventor 田承涛肖林波张小元
Owner HUBEI SANNING CHEM
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