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Method for measuring residual phosphorus content in wet process phosphate phosphorus gypsum

A technology of phosphophosphogypsum and phosphorus content, which is applied in the direction of weighing by removing certain components, can solve the problems of human injury, environmental pollution, long heating and decomposition time, and corrosion of ventilation equipment, so as to reduce environmental pollution and avoid corrosion experiments The effect of small corrosion of equipment and equipment

Inactive Publication Date: 2017-05-10
YUNNAN PHOSPHATE CHEM GROUP CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] 3. Eutectic loss of phosphorus
[0015] 2. Great harm
Inverse regia releases a large amount of acidic and harmful gases during heating, which seriously corrodes ventilation equipment; especially the harm of nitrogen dioxide to the human body and the pollution of the environment cannot be ignored
[0016] 3. High energy consumption
The heating and decomposition time is too long, and the energy consumption is large

Method used

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  • Method for measuring residual phosphorus content in wet process phosphate phosphorus gypsum
  • Method for measuring residual phosphorus content in wet process phosphate phosphorus gypsum
  • Method for measuring residual phosphorus content in wet process phosphate phosphorus gypsum

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0042] Take 5 grams of phosphogypsum wet sample, wash it with water until it is neutral, transfer it to a beaker, add 60 mL of hydrochloric acid with a mass fraction of 6.5%, heat to a slight boil for 20 minutes, cool and transfer to a 250 mL volumetric flask, constant volume, shake well, and dry filter , discard the first 20 mL of filtrate. Accurately draw 25.00mL of the filtrate into a 300mL beaker, add 1+1 (made up of 68% reagent grade chemically pure concentrated nitric acid and water volume ratio 1:1) nitric acid 10mL, add water to about 100mL, heat to near boiling, remove Beaker, under constant stirring, add 20mL quincimolicone precipitation agent, carefully heat until the upper solution is clear. Remove the beaker, let it stand for cooling, and filter it with a sand core crucible that has been dried to constant weight. First filter the supernatant, then wash the precipitate 1-2 times by pouring method (approximately 25 mL of water each time), transfer all the precipita...

Embodiment 2

[0056] Take 5 grams of phosphogypsum wet sample, wash it with water until it is neutral, transfer it to a beaker, add 50 mL of hydrochloric acid with a mass fraction of 7%, heat to a slight boil for 20 minutes, transfer it to a 250 mL volumetric flask after cooling, constant volume, shake well, and dry filter , discard the first 20 mL of filtrate. Accurately draw 25.00mL of the filtrate into a 300mL beaker, add 10mL of 1+1 nitric acid, add water to about 100mL, heat to near boiling, remove the beaker, add 20mL of quinolimonone precipitant under constant stirring, and carefully heat to the upper layer solution clear. Remove the beaker, let it stand for cooling, and filter it with a sand core crucible that has been dried to constant weight. First filter the supernatant, then wash the precipitate 1-2 times by pouring method (approximately 25 mL of water each time), transfer all the precipitate to the crucible, and continue to wash the precipitate and the inner wall of the crucib...

Embodiment 3

[0062] Take 5 grams of phosphogypsum wet sample, wash it with water until it is neutral, transfer it to a beaker, add 50 mL of hydrochloric acid with a mass fraction of 7.5%, heat to a slight boil for 20 minutes, cool and transfer to a 250 mL volumetric flask, constant volume, shake well, and dry filter , discard the first 20 mL of filtrate. Accurately draw 25.00mL of the filtrate into a 300mL beaker, add 10mL of 1+1 nitric acid, add water to about 100mL, heat to near boiling, remove the beaker, add 20mL of quinolimonone precipitant under constant stirring, and carefully heat to the upper layer solution clear. Remove the beaker, let it stand for cooling, and filter it with a sand core crucible that has been dried to constant weight. First filter the supernatant, then wash the precipitate 1-2 times by pouring method (approximately 25 mL of water each time), transfer all the precipitate to the crucible, and continue to wash the precipitate and the inner wall of the crucible unt...

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Abstract

The invention discloses a method for measuring the residual phosphorus content in wet process phosphate phosphorus gypsum. The method comprises the following operation steps of (1) taking wet phosphorus gypsum samples; performing water washing to the neutral state; then, transferring the materials into a beaker; next, adding hydrochloric acid; heating the materials to a slight boiling state; cooling the materials to the room temperature; then, transferring the materials to a volume bottle; maintaining the constant volume; uniformly shaking the materials; directly performing filtering without washing; (2) sucking partial filter liquid into the breaker; adding dilute nitric acid; heating the materials to be about to boil; taking down the breaker; adding quimociac precipitators during stirring; slowing heating the materials until the upper layer solution is clear and bright; (3) taking down the breaker; performing still standing and cooling to room temperature; then, performing filtering; washing precipitates to be neutral; drying the precipitates; cooling the precipitates in a drier to the room temperature; performing weighing; calculating the mass percentage of phosphorus pentoxide in the sample. The method has the advantages that little low-concentration hydrochloric acid is used for replacing lefort aqua regia to realize the extraction of residual phosphorus in the phosphorus gypsum. The method provided by the invention has the advantages that the acid types are few; the consumption is low; the environment pollution and the equipment corrosion are low; the energy is saved; the time is saved, and the like.

Description

technical field [0001] The invention belongs to the technical field of residual phosphorus in phosphogypsum, and in particular relates to a method for measuring the residual phosphorus content in wet-process phosphoric acid gypsum. Background technique [0002] The residual phosphorus content in wet-process phosphoric acid phosphogypsum is an important index to measure the industrial technology of wet-process phosphoric acid, which is related to the consumption of wet-process phosphoric acid phosphate rock and the level of phosphorus recovery. The main forms of residual phosphorus in phosphogypsum include the following: [0003] 1. Water-soluble phosphorus [0004] It is mainly a small amount of phosphoric acid and soluble phosphate. This kind of residual phosphorus is caused by insufficient washing of phosphogypsum. Because the phosphogypsum used in the experiment has been fully washed, it is not considered. [0005] 2. Phosphate precipitation [0006] Because there are ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N5/04
CPCG01N5/04
Inventor 牛司江赵智波王云波
Owner YUNNAN PHOSPHATE CHEM GROUP CORP
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