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Method for preparing fluoroboric acid using by-product fluosilicic acid with low concentration in wet method phosphoric acid production process

A wet-process phosphoric acid and fluosilicic acid technology, which is used in the removal of boron halide compounds and solid waste.

Active Publication Date: 2012-05-02
YUNNAN YUNTIANHUA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] The fluosilicic acid produced in the wet-process phosphoric acid production process contains a large amount of fluorine resources, and the preparation of fluoboric acid from fluosilicic acid is an important research direction for the recovery of fluorine resources. However, the concentration of fluosilicic acid produced by the wet-process phosphoric acid industry is increased by circulating and absorbing silicon tetrafluoride gas. The higher the concentration, the more unstable the fluosilicic acid, the more serious the corrosion of equipment, and the more impurities it contains. poor product quality
Utilize low-concentration fluosilicic acid to prepare fluoboric acid, the resulting silica grains are fine, easy to form sol, difficult to separate, and the recovery rate of fluorine is low
Concentrating with low-concentration fluorosilicic acid not only consumes a lot of energy, but also some fluorosilicic acid will decompose during the concentration process, a large amount of hydrogen fluoride gas will escape, and the generated silica gel will block the pipeline, which is extremely inconvenient

Method used

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  • Method for preparing fluoroboric acid using by-product fluosilicic acid with low concentration in wet method phosphoric acid production process
  • Method for preparing fluoroboric acid using by-product fluosilicic acid with low concentration in wet method phosphoric acid production process

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Weigh 480.0g of 6.67% fluorosilicic acid solution, put it in the reactor, add 3.3374g of silicon dioxide, start stirring to fully disperse the silicon dioxide in the fluorosilicic acid solution, preheat to 54°C, and adjust the stirring speed to 56r / min, weigh 20.67g of 99.7% boric acid (n=1.0), slowly add it into the reactor, the feeding time is 60min, the temperature of the slurry is raised to 80°C, constant temperature, after 2h of reaction, suction filtration under the condition of -0.078MPa , Obtain 345.6 g of filtrate. Concentrate at 75°C and -0.07MPa to obtain 38.70g of a 40.21% concentrate. Wash the filter cake three times with 250ml, and combine to obtain 274.2g of washing liquid. The technical indicators of the filtrate after concentration are shown in Table 1.

[0024] Table 1

[0025] project index Exterior colorless transparent liquid Fluoboric acid (HBF 4 ) mass score 40.21％ Free boric acid (H 3 BO 3 ) quality score ...

Embodiment 2

[0027] Weigh 250g of 9.28% fluosilicic acid solution, put it in the reactor, add 1.9278g of silicon dioxide, start stirring to fully disperse the silicon dioxide in the fluosilicic acid solution, preheat to 50°C, and adjust the stirring speed to 60r / min, weighed 15.72g of 99.7% boric acid (n=1.05), slowly added to the reactor, the feeding time was 65min, the temperature of the slurry was raised to 85°C, kept at constant temperature, and reacted for 2.5h, and then pumped under the condition of -0.050MPa Filtrate to obtain 192.5 g of the filtrate, which was concentrated at 70° C. and -0.065 MPa to obtain 27.35 g of a 40.06% concentrated solution. Wash the filter cake with 274.2 g of the washing solution obtained in Example 1 to obtain 264.2 g of the secondary washing solution, then rinse the filter cake twice with 100 ml of distilled water, and combine to obtain 89.3 g of the washing solution. The technical indicators of the filtrate after concentration are shown in Table 2.

...

Embodiment 3

[0032] Weigh 250g of 10.82% fluosilicic acid solution, put it in the reactor, add 1.6917g of silicon dioxide, start stirring to fully disperse the silicon dioxide in the fluosilicic acid solution, preheat to 53°C, and adjust the stirring speed to 50r / Min, weigh 16.59g of 99.7% boric acid (n=0.95), slowly add it into the reactor, the feeding time is 70min, the temperature of the slurry is raised to 90°C, keep the temperature constant, after reacting for 3h, suction filter under the condition of -0.050MPa , to obtain 224.2 g of filtrate, which was concentrated under the conditions of 80° C. and -0.06 MPa to obtain 34.62 g of 41.02% concentrated solution. Rinse the filter cake with the secondary washing of Example 1 and Example 2 to obtain 261.3 g of washing liquid three times, then rinse the filter cake twice with 100 ml of distilled water, combine to obtain washing liquid 103.7 g, and merge with the first washing liquid of Example 2 . The technical indicators of the filtrate ...

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Abstract

The invention discloses a method for preparing fluoboric acid from a byproduct, namely low-concentration hydrofluosilicic acid of phosphorous acid by a wet process and preparation of the fluoboric acid, and in particular relates to the method for preparing the fluoboric acid by inducing the crystallization by the byproduct, namely the low-concentration hydrofluosilicic acid of the phosphorous acid by the wet process. The method comprises the following steps that: a, the low-concentration hydrofluosilicic acid is sent into a reactor, silicon dioxide is added into the reactor to serve as an inoculating seed, and the stirring is performed; b, a suspension of the hydrofluosilicic acid and the silicon dioxide is preheated to a temperature which is more than 50 DEG C; c, solid boric acid is slowly added into the hydrofluosilicic acid, the ratio of the actual use level to the theoretical use level of the boric acid is between 0.95 and 1.05, and the adding time is between 60 and 70min; d, themixture reacts for 2 to 3h under the condition that the temperature is between 80 and 90 DEG C and the stirring speed is between 50 and 60r / min; e, the filtration is performed immediately after the reaction is stopped; and f, a filtrate is concentrated to a concentration which is more than or equal to 40 percent under the conditions of a temperature of between 50 and 80 DEG C, the pressure of between -0.06 and -0.07MPa, and the like, and is aged for 24 hours to obtain a finished product. The method reduces the feasible concentration of the hydrofluosilicic acid, ensures that dilute acid directly takes part in the reaction without being concentrated, shortens a process route, also avoids the decomposition of the hydrofluosilicic acid during the concentration, and improves the recovery rateof fluorine.

Description

technical field [0001] The invention relates to the preparation of fluoboric acid, in particular to a method for preparing fluoboric acid by inducing crystallization of low-concentration fluosilicic acid by-product of wet-process phosphoric acid. technical background [0002] The fluosilicic acid produced in the production process of wet-process phosphoric acid contains a large amount of fluorine resources. The preparation of fluoboric acid by using fluosilicic acid is an important research direction for the recovery of fluorine resources. Silicon fluoride gas is used to increase the concentration. The higher the concentration, the more unstable the fluorosilicic acid, the more serious the corrosion of the equipment, the more impurities it contains, and the poor quality of the resulting product. Utilizing low-concentration fluosilicic acid to prepare fluoboric acid, the resulting silica has fine grains, is easy to form sol, is difficult to separate, and has a low recovery r...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B35/06B09B3/00
Inventor 明大增李志祥黄壮昌
Owner YUNNAN YUNTIANHUA
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