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Preparation method and application of functional single-walled carbon nanohorn

A single-wall carbon nanohorn, functionalized technology, applied in chemical instruments and methods, inorganic chemistry, radioactive purification, etc., can solve the problems of difficult separation of impurities, no good way to remove, small adsorption capacity, etc., and achieve high adsorption. The speed, the method is simple, the effect of high adsorption capacity

Active Publication Date: 2018-11-27
EAST CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In addition to many advantages of carbonaceous materials, carbon nanomaterials have larger specific surface area and more surface atoms than ordinary carbonaceous materials such as activated carbon and hydrothermal carbon due to their nanometer size, and also show other Excellent physical and chemical properties; as an adsorbent, it has obvious advantages in treating radioactive wastewater, but there are still some shortcomings: 1. Generally, carbon nanomaterials bring impurities during the preparation process and have problems of separation difficulties in practical applications (such as: There is no good way to remove the metal (salt) catalyst used in the preparation of carbon nanotubes), 2. The non-functionalized carbon nanomaterials have no selectivity for the adsorption of radioactive elements (such as: uranium, thorium), And the adsorption capacity is relatively small [such as: a. The saturated adsorption capacity of pure carbon nanotubes to uranium ions is only 41.48 mg / g (J. Radioanal. Nucl. Chem. 2017, 314 (3), 1747-1757); b. The saturated adsorption capacity of mesoporous carbon (CMK-3) for uranium ions is less than 10 mg / g (Ind.Eng.Chem.Res.2017, 56, 9821-9830); c. The saturation of uranium ions by graphene oxide (GO) Adsorption capacity 97.5mg / g (Chemical Engineering Journal 2014,255,604–612) etc.
Moreover, the three carbon nanomaterials a, b, and c have no selectivity for the adsorption of radioactive elements]

Method used

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  • Preparation method and application of functional single-walled carbon nanohorn

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Embodiment 1

[0028] A method for preparing functionalized single-walled carbon nanohorns, comprising the following steps:

[0029] Step 1: Modification of SWCNH

[0030] Disperse 100 mg of SWCNH into 150 mL of nitric acid solution and reflux at 100 ° C for 24 hours to obtain a carboxylated SWCNH (SWCNH-COOH) dispersion, which is centrifuged, washed and filtered with deionized water several times until the filtrate becomes neutral, Then vacuum-dry, then disperse the carboxylated single-walled carbon nanohorn in deionized water, and prepare a 0.5 mg / mL dispersion for subsequent use;

[0031] Step 2: Triethylenetetramine functionalized SWCNH (SWCNH-TETA)

[0032]Using carboxylated single-walled carbon nanohorn (SWCNH-COOH) and triethylenetetramine (TETA) as reaction raw materials, 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride ( EDC) / N-hydroxysuccinimide (NHS) as a catalyst, under the protection of nitrogen, the reaction temperature was controlled at 70 ° C, reacted for 12 hour...

Embodiment 2

[0034] A method for preparing functionalized single-walled carbon nanohorns, comprising the following steps:

[0035] Step 1: Modification of SWCNH

[0036] Disperse 150 mg of SWCNH into 200 mL of nitric acid solution and reflux at 120 ° C for 24 hours to obtain a carboxylated SWCNH (SWCNH-COOH) dispersion, which is centrifuged, washed and filtered with deionized water for several times until the filtrate becomes neutral, Then vacuum-dry, then disperse the carboxylated single-walled carbon nanohorn in deionized water, and prepare a 1.0 mg / mL dispersion for subsequent use;

[0037] Step 2: Triethylenetetramine functionalized SWCNH (SWCNH-TETA)

[0038] Using carboxylated single-walled carbon nanohorn (SWCNH-COOH) and triethylenetetramine (TETA) as reaction raw materials, 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride ( EDC) / N-hydroxysuccinimide (NHS) as a catalyst, under the protection of nitrogen, the reaction temperature was controlled at 80 ° C, reacted for 12...

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Abstract

A preparation method of a functional single-walled carbon nanohorn comprises the steps of modifying SWCNH at first, dispersing SWCHN in a nitric acid solution to obtain carboxylated SWCNH dispersion liquid, carrying out centrifuging, washing and filtering and vacuum drying, and then preparing the carboxylated SWCNH dispersion liquid into 0.5-1.0 mg / mL of dispersion liquid; and then functionalizingSWCNH, reacting at the temperature of 70-80 DEG C for 8-12 hours under protection of nitrogen by taking carboxylated SWCNH and triethylene tetramine as raw materials and taking 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride and N-hydroxysuccinimide as catalysts, cooling to the room temperature, centrifuging to remove supernatant liquid, and washing and drying under vacuum to obtain the product. Abundant amino and imine groups are grafted on the surface of SWCNH with large specific surface area to modify SWCNH, the prepared SWCNH-TETA composite material selectively adsorbs U ions,and the adsorbing capacity and adsorption speed are higher.

Description

technical field [0001] The invention belongs to the technical field of uranium separation and enrichment, and specifically relates to a preparation method and application of functionalized single-walled carbon nanohorns. Background technique [0002] Due to its economy, cleanliness and high efficiency, nuclear power generation has become the leading role of new energy and occupies an important position in my country's future energy development strategy. By 2020, my country's nuclear power installed capacity will reach 58 million kilowatts, so the annual demand for natural uranium is about 5800-8800 tons. However, my country's land uranium resources are scarce, accounting for only 2% of the world's total uranium resources, and uranium mines Low grade, mostly depleted uranium ore, so it is difficult to meet the future demand for uranium fuel supply in my country. The shortage of uranium resources makes the extraction of non-mineral uranium resources particularly urgent. Seawa...

Claims

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Application Information

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IPC IPC(8): B01J20/20B01J20/28B01J20/30G21F9/12
CPCB01J20/205B01J20/28007B01J20/28057G21F9/12
Inventor 王春艳刘峙嵘许剑平钱勇
Owner EAST CHINA UNIV OF TECH
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