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Method for preparing calcium fluoride from phosphorous ore-associated fluorine resources

A calcium fluoride and resource technology, applied in the field of phosphorus chemical industry, can solve the problems of high safety, environmental protection risks, limited application scope, inability to apply, etc., and achieve the effects of widening the range of raw materials, good dissolution effect and low loss rate

Inactive Publication Date: 2019-12-20
HUBEI XIANGYUN GROUP CHEM +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

These two patents can obtain calcium fluoride products, but they cannot be applied to deposits, scales, crystals and defluorinated substances, so the scope of application is limited, only limited to relatively pure fluosilicic acid
In addition, both patents require the use of difficult-to-recycle ammonia as the circulating medium, which poses greater safety and environmental risks, and requires higher safety and environmental protection devices; the by-product ammonia water needs to be heated and evaporated to achieve recycling and water balance , will inevitably increase energy consumption; expensive ammonia consumption will become another weakness of this type of method

Method used

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  • Method for preparing calcium fluoride from phosphorous ore-associated fluorine resources

Examples

Experimental program
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Effect test

Embodiment 1

[0042] Add 220g of potassium fluorosilicate prepared in advance with fluorosilicic acid to 220g of water to make a slurry, then add 490g of 48% (mass concentration, the same below) potassium hydroxide solution, stir and react at 90°C for 60min, and then filter to obtain Silica filter cake and solution, the filter cake is washed to obtain white carbon black products; the filtrate is added with fluorosilicic acid, a by-product of phosphate fertilizer, to adjust the pH to 8, and filtered to obtain refined potassium fluoride solution and filter cake (for washing) , the filter cake is returned to the fluorine extraction reaction, the lotion is combined with the potassium fluoride solution; 402 g of calcium hydroxide solid is added to the combined potassium fluoride solution, and after 20 minutes of reaction, filter, wash, and dry at 105 ° C to obtain calcium fluoride product, the filtrate is concentrated to 48% concentration and partly returns to the fluorine extraction reaction, an...

Embodiment 2

[0045] Add 220g of crystals to 220g of water to make a slurry, then add 463g of 48% potassium hydroxide solution, stir and react at 95°C for 60min, then filter to obtain a filter cake and solution, and the filter cake is washed as a raw material for compound fertilizer preparation; the filtrate Then add fluosilicic acid, a by-product of phosphate fertilizer, to adjust the pH to 7, and obtain refined potassium fluoride solution and filter cake (for washing) after filtration. Add 175g of calcium hydroxide solid to the potassium chloride solution, react for 30 minutes, filter, wash, and dry at 105°C to obtain the calcium fluoride product. The filtrate obtained 48% potassium hydroxide product after defluorination.

[0046] Obtain calcium fluoride 180g in this process, productive rate 97.5%, calcium fluoride content 98.1%, silicon dioxide content 0.08%, calcium carbonate content 0.97%, sulfur content 0.04%, P content 0.05%, arsenic is not detected, Organic matter was not detected....

Embodiment 3

[0048] Add 220g of sediment to 150g of water to make a slurry, then add 297g of 48% potassium hydroxide solution, stir and react at 80°C for 60 minutes, then filter to obtain filter cake and solution, and wash the filter cake as raw material for compound fertilizer preparation The filtrate is added to the phosphate fertilizer by-product fluosilicic acid to adjust the pH to 7, and after filtration, the refined potassium fluoride solution and filter cake (for washing) are obtained, and the filter cake is returned to the fluorine extraction reaction, and the washing solution is combined with the potassium fluoride solution; Add 1:1 (mass ratio of calcium hydroxide to water) calcium hydroxide emulsion 220g to the potassium fluoride solution, react for 30 minutes, filter, wash, dry at 105°C to obtain the calcium fluoride product, and concentrate the filtrate to 48% After the concentration, part returns to the fluorine extraction reaction, and the remaining filtrate is defluorinated,...

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Abstract

The invention discloses a method for preparing calcium fluoride from phosphorous ore-associated fluorine resources, and belongs to the technical field of phosphorus chemical engineering. The method comprises the steps: performing a reaction on a fluorine-containing compound and potassium hydroxide, performing solid-liquid separation after completion of the reaction so as to obtain a silicon-containing potassium fluoride solution, adding a fluorosilicic acid to the silicon-containing potassium fluoride solution so as to adjust the pH value, performing filter separation so as to obtain a potassium fluoride solution and silica-potassium fluorosilicate solid, returning the silica-potassium fluorosilicate solid to the first step, performing a reaction on the potassium fluoride solution an calcium hydroxide, performing solid-liquid separation after completion of the reaction so as to obtain calcium fluoride and a potassium hydroxide filtrate, recycling a part of the potassium hydroxide filtrate to the first step, and concentrating the remaining potassium hydroxide solution so as to obtain a potassium hydroxide product. The shortcoming that fluorine-containing compounds in by-products ofa wet preparation process of phosphoric acid cannot be utilized other than fluorosilicic acid in the prior art is overcome, full utilization of the fluorine-containing compounds is achieved, and meanwhile the waste fluorine-containing compounds can be processed into high-value calcium fluoride, potassium hydroxide and silicon dioxide.

Description

technical field [0001] The invention belongs to the technical field of phosphorus chemical industry, and in particular relates to a method for preparing calcium fluoride from phosphate rock associated fluorine resources. Background technique [0002] During the production process of wet-process phosphoric acid, a large amount of fluorine-containing compounds will be produced by-product, including fluosilicic acid obtained by absorbing tail gas, deposits in phosphoric acid storage tanks (hereinafter referred to as deposits), and scales in phosphoric acid delivery pipelines (hereinafter referred to as Scales), crystals in the return pipe of the phosphogypsum reservoir (hereinafter referred to as crystals), precipitates produced during the defluorination of dilute phosphoric acid (hereinafter referred to as defluorinated products), etc. In addition to industrial applications, such as processing into hydrogen fluoride, sodium fluorosilicate, ammonium fluoride and other products,...

Claims

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Application Information

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IPC IPC(8): C01F11/22C01D1/04C01D1/24C01B33/12C05G3/00
CPCC01B33/12C01D1/04C01D1/24C01F11/22C01P2006/80
Inventor 黄忠胡挺张险峰徐超余双强余莹查炎华
Owner HUBEI XIANGYUN GROUP CHEM
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