A method for separating beryllium from beryllium-containing sludge based on mineral phase reconstruction

A sludge and mineral phase technology, applied in sludge treatment, chemical instruments and methods, water/sludge/sewage treatment, etc., can solve the problems of failure to detoxify beryllium-containing waste and re-release of beryllium, and achieve Low processing cost, mild reaction conditions, and the effect of reducing beryllium pollution

Active Publication Date: 2022-07-15
CENT SOUTH UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The above method or process mainly uses acid or acidic substances to leach the waste liquid in the slag, and then crushes and solidifies the slag, or directly crushes and solidifies the waste slag containing beryllium. Although it has a certain positive effect on the treatment of beryllium, the existing solidification method The object of treatment is not beryllium-containing sludge, and it has not been specifically designed based on the solid phase characteristics of beryllium-containing sludge, and solidifying beryllium in glassy slag or cement has not yet achieved complete detoxification of beryllium-containing waste. There is a risk of re-release of beryllium
[0005] In view of this, it is necessary to provide a method for separating beryllium from beryllium-containing sludge based on mineral phase reconstruction, to solve or at least alleviate the environmental hazards of beryllium-containing sludge in the above-mentioned prior art and the inability to separate beryllium from beryllium-containing sludge. Defects of efficient separation and recovery of beryllium in mud

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  • A method for separating beryllium from beryllium-containing sludge based on mineral phase reconstruction
  • A method for separating beryllium from beryllium-containing sludge based on mineral phase reconstruction
  • A method for separating beryllium from beryllium-containing sludge based on mineral phase reconstruction

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Experimental program
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Effect test

Embodiment 1

[0060] Sampling and analysis of beryllium-containing sludge:

[0061] The beryllium-containing sludge after drying and dehydration in a factory was taken, and the solid samples were digested with nitric acid and hydrochloric acid. The sludge mainly contains elements such as Ca, Si, O, S, among which Ca mainly exists in the form of calcium sulfate, and Si mainly exists in the form of silica.

[0062] The SEM-EDS image of the sample was measured (see figure 2 ), based on the image, it can be concluded that calcium sulfate and silica are two phases in the solid phase, wherein calcium sulfate is gypsum crystal, and silica is an amorphous flocculent aggregate. The XRD pattern of the sample was obtained again (see image 3 ), only the peak of calcium sulfate exists in the figure, and there is no peak of silica. Based on the two figures, it can be concluded that the silica in the solid phase is amorphous. Elemental distribution map of the electron probe of the sample (see Figu...

Embodiment 2

[0064]Put 1 kilogram of the beryllium-containing sludge sample described in Example 1 into a ball mill for wet ball milling pretreatment. After grinding to 400 mesh, it is fully mixed and stirred with 10 liters of 0.5 mol / L sulfuric acid to obtain a solid-liquid mixture. The liquid mixture was put into a hydrothermal kettle, and the hydrothermal kettle was sealed, heated to 120 ° C, and reacted for 4 hours. After the reaction was completed, it was allowed to stand and cool to room temperature. The hydrothermal kettle is opened, and the solid-liquid mixture is separated by means of filtration, centrifugation, etc., to obtain a beryllium-containing filtrate and a beryllium-depleted filter residue. The beryllium-containing filtrate is returned to the beryllium smelting process, and the filter residue is washed with water, filtered / centrifuged 3 times, and detoxified waste residue is obtained. The beryllium content in the beryllium-containing filtrate was measured, and the berylli...

Embodiment 3

[0080] The described beryllium-containing sludge sample in 1 kilogram of embodiment 1 is put into a ball mill for wet ball milling pretreatment, and after grinding to 300 meshes, mixed with 5 liters of sulfuric acid and hydrochloric acid (total concentration 1mol / L, v sulfuric acid: v hydrochloric acid=1:1) After fully mixing and stirring, the solid-liquid mixture was put into a hydrothermal kettle, and the hydrothermal kettle was sealed, heated to 180 ° C, and reacted for 3 hours. The hydrothermal kettle is opened, and the solid-liquid mixture is separated by means of filtration, centrifugation, etc., to obtain a beryllium-containing filtrate and a beryllium-depleted filter residue. The beryllium-containing filtrate is returned to the beryllium smelting process, and the filter residue is washed with water, filtered / centrifuged for 5 times, and detoxified waste residue is obtained. The beryllium content in the beryllium-containing filtrate was measured, and the beryllium conte...

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Abstract

The present invention provides a method for separating beryllium from beryllium-containing sludge based on mineral phase reconstruction, the beryllium-containing sludge comprising beryllium hydroxide-loaded amorphous silica and calcium sulfate, and the method comprises the steps of : S1, grinding the beryllium-containing sludge to obtain a ground product; mixing the ground product with an acid solution to obtain a solid-liquid mixture; S2, performing hydrothermal treatment on the solid-liquid mixture to make the The amorphous silica in the beryllium sludge undergoes mineral phase reconstruction, and the beryllium in the beryllium-containing sludge is further dissolved, thereby obtaining a mixed product reconstructed by the mineral phase; S3, the mixed products are sequentially carried out Cooling treatment and solid-liquid separation treatment are carried out to obtain beryllium-containing filtrate and filter residue after beryllium removal. The invention can avoid the pollution of the beryllium-containing sludge to the environment, and can efficiently separate and recover beryllium from the beryllium-containing sludge.

Description

technical field [0001] The invention relates to the separation and recovery of beryllium, in particular to a method for separating beryllium from beryllium-containing sludge based on mineral phase reconstruction. Background technique [0002] Beryllium oxide is an extremely important industrial material, mainly used for the production of functional material beryllium copper alloy in aerospace field, nuclear reaction buffer metal beryllium oxide, and beryllium oxide used in special ceramics. There are two industrial methods for preparing beryllium oxide: sulfuric acid method and fluorination method. At present, domestic beryllium oxide production enterprises mainly use the improved "Degusa" sulfuric acid process. See "China Beryllium Industry" P102-107, the specific process of the process is: high-grade beryl (BeO·Al2O 3 ·6SiO 2 ) and calcite (CaO) are mixed into an electric arc furnace and smelted at 1400-1500 ° C. The melt is quenched by water and ball-milled into a high...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C22B7/00C22B35/00C22B1/00C02F11/00C02F11/12C04B7/14
CPCC22B7/007C22B35/00C22B1/00C02F11/00C02F11/12C04B7/14Y02P40/10
Inventor 林璋刘炜珍李莉柯勇梁彦杰李婕颜旭
Owner CENT SOUTH UNIV
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