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A method for preparing uranium adsorption material using oil shale semi-coke as raw material

An oil shale semi-coke and adsorption material technology, which is applied to the preparation of uranium adsorption materials and the field of preparation of uranium adsorbents, can solve the problems of complex utilization methods, high cost, insufficient utilization of carbon components, etc., and avoid the volatilization of nitric acid. and decomposition, improve efficiency, inhibit volatilization and decomposition effects

Active Publication Date: 2018-04-17
HARBIN ENG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

These utilization methods are complex in process, high in cost, and do not fully utilize the carbon content in them

Method used

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  • A method for preparing uranium adsorption material using oil shale semi-coke as raw material
  • A method for preparing uranium adsorption material using oil shale semi-coke as raw material
  • A method for preparing uranium adsorption material using oil shale semi-coke as raw material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Step 1: After mixing 20ml of concentrated sulfuric acid and 20ml of concentrated nitric acid, slowly add 4g of oil shale semi-coke and put it in a microwave reactor. After the microwave is heated to 70℃, the temperature is controlled at 70℃ for 1h, and then 80℃, 90℃, 100℃ The temperature was controlled for 20 minutes at 110°C and the temperature for 5 minutes. After the reaction, the temperature was cooled to room temperature, and deionized water was slowly added. The volume ratio of the added deionized water to the original added sulfuric acid volume was 3:7; Stir at 70°C for 0.5-2h, filter, wash with deionized water to neutrality, and dry to obtain modified oil shale semi-coke A. Combine the filtrate and washing liquid to obtain acid B. The whole process adopts microwave heating, the reaction process is under normal pressure and is carried out under vigorous stirring conditions, and the reaction gas is introduced into the alkali solution for recovery. Under the conditi...

Embodiment 2

[0031] On the basis of Example 1, the difference is that 4g of oil shale semi-coke is slowly added to 33.33ml of concentrated sulfuric acid and 6.67ml of concentrated nitric acid.

[0032] Under the conditions of 273K and pH=6, the obtained modified oil shale semi-coke A has a uranium adsorption capacity greater than 448mg / g, and the removal rate of 100ppm uranium solution is 74%. The specific surface area of ​​the material is 67m 2 / g.

[0033] Compared with Example 1, the adsorption capacity of this embodiment is significantly improved, mainly due to the relative reduction in the amount of nitric acid, which reduces the damage to the carbon component, resulting in a reduction in the loss of carbon materials, so the uranium per unit mass of adsorbent Increased adsorption capacity. The decrease in removal rate may be due to the change in the balance coefficient of the material as the carbon content increases and the degree of oxidation changes. Therefore, by adjusting the ratio o...

Embodiment 3

[0035] On the basis of Example 1, the difference is that 4g of oil shale semi-coke is slowly added to 30ml of concentrated sulfuric acid and 10ml of concentrated nitric acid.

[0036] Under the conditions of 273K and pH=6, the obtained modified oil shale semi-coke A has a uranium adsorption capacity greater than 275mg / g, and the removal rate of 100ppm uranium solution is 81%.

[0037] This embodiment has good adsorption capacity and removal rate at the same time.

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Abstract

The invention provides a method for preparing a uranium-adsorbing material with oil shale semi-coke as the raw material. Concentrated sulfuric acid and concentrated nitric acid are mixed according to the volume size of 5:1-1:1, then oil shale semi-coke is added according to the solid-liquid ratio of 1:10, the mixture is placed in a microwave reactor and reacts at the temperature of 70 DEG C, 80 DEG C 90 DEG C, 100 DEG C and 110 DEG C respectively, the mixture is cooled to room temperature after reaction, deionized water with the volume ratio to originally added concentrated sulfuric acid being 3:7 is added, stirring is conducted for 0.5-4 h at 70-80 DEG C, the mixture is filtered, washed with deionized water to be neutral and dried, modified oil shale semi-coke A is obtained, and filter liquid and washing liquid are combined to obtain acid liquor B; bivalent metal ions are added to adjust the total mole number of trivalent and tetravalent metal ions and the total mole number of the bivalent metal ions in the acid liquor A to be 1:5-1:2, the pH of the solution is adjusted to be 12, stirring is conducted for 10-1000 min, filtering, washing and drying are conducted, and the uranium-adsorbing material is obtained. The obtained uranium-adsorbing material has good uranium-adsorbing performance, and the maximum uranium-adsorbing amount is larger than 150 mg / g under the conditions that the pH value is 6 and the temperature is 293 K.

Description

Technical field [0001] The present invention relates to a method for processing oil shale semi-coke. The present invention also relates to a method for preparing uranium adsorbent material, in particular to a method for preparing uranium adsorbent using oil shale semi-coke as raw material. Background technique [0002] Oil shale semi-coke has a huge output and serious pollution. my country’s oil shale resources are about 700 billion tons, equivalent to about 40 billion tons of shale oil. Fushun City will retort 4,000 tons of oil shale every day. The power plants in Huadian City consume 480,000 tons of oil shale every year. A large amount of shale semi-coke is produced, the amount is at least 8-10 times the oil production, which not only causes serious waste of resources, but also occupies a large amount of land and brings serious environmental pollution problems. How to make good use of shale semi-coke will directly affect the development and utilization of oil shale resources. ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J20/20B01J20/30B01J20/34G21F9/12
CPCB01J20/08B01J20/103B01J20/20B01J2220/42B01J2220/4806G21F9/12
Inventor 王君张宏森刘婧媛刘琦魏新涛李茹民
Owner HARBIN ENG UNIV