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Supported active chalcogenide compound as well as preparation method and application thereof

A technology of active sulfur and complexes, applied in separation methods, chemical instruments and methods, other chemical processes, etc., can solve the problems of low adsorption rate, small adsorption capacity, small temperature window, etc., and achieve the improvement of adsorption capacity and adsorption rate, Applicable to the effect of large temperature window and low cost

Active Publication Date: 2022-07-05
CENT SOUTH UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] In order to overcome the obvious shortcomings of the existing chalcogenide mercury adsorption materials, such as small adsorption capacity, low adsorption rate, high cost, complicated preparation, and small temperature window, the present invention provides a loaded active sulfur with large adsorption capacity and large mercury removal temperature window. Family compound and its preparation method and application

Method used

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  • Supported active chalcogenide compound as well as preparation method and application thereof
  • Supported active chalcogenide compound as well as preparation method and application thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0057] Soak industrial selenium powder (purity 98%) in dilute acid solution for 5h, rinse with deionized water and ethanol for 3 times in turn, dry at 100°C, then crush and grind, pass through a 200-mesh sieve, and take off the sieve; prepare saturated sodium borohydride The reducing solution is added dropwise to the surface-treated industrial selenium powder at a ratio of 0.4g / mL, fully wetted and mixed evenly, and the constant temperature water bath is continuously stirred at 30°C for 30min to a paste, and the dosage is continued at 0.7g / mL. Sodium carbonate activator, stir for 60min to form a uniform slurry; add a large amount of acidic diluent to the slurry in a volume ratio of 1:50, adjust the acidity of the solution to pH=12, and continue to stir and age for 2h to prepare an active impregnation solution; The purchased commercial activated carbon (mass ratio of 0.05g / g to industrial selenium powder) was immersed in the active impregnation solution, continuously shaken for ...

Embodiment 2

[0062] Soak the medicinal selenium powder (purity 99.9%) in dilute acid solution for 3 hours, rinse with deionized water and ethanol for 3 times in turn, dry at 100°C, crush and grind, pass through a 200-mesh sieve, and take the undersize; take the reduced hydrazine reducing solution , the reducing solution was added dropwise to the surface-treated industrial selenium powder at a ratio of 0.32g / mL, fully wetted and mixed evenly, and the constant temperature water bath was continuously stirred at 45°C for 10min until it became a paste, and 0.2g / mL continued to add hydrogen peroxide. Sodium activator, stir for 20min to form a uniform slurry; add a large amount of acidic diluent to the slurry in a volume ratio of 1:60, adjust the acidity of the solution to pH=10, continue to stir and age for 2h to prepare an active impregnation solution; (Mass ratio of 0.03g / g with industrial selenium powder) was immersed in the active impregnation solution, continuously shaken for 6 hours, the tw...

Embodiment 3

[0065] Soak industrial sulfur powder (purity 98%) in dilute acid solution for 8 hours, rinse with deionized water and ethanol for 3 times in turn, dry at 90°C, crush and grind, pass through a 200-mesh sieve, and take off the sieve; prepare stannous chloride Saturate the reducing solution, add the reducing solution dropwise to the surface-treated sulfur powder at a ratio of 1 g / mL, fully wet and mix evenly, and continue stirring in a constant temperature water bath at 30 °C for 20 minutes to a paste, and continue to add hydrogen at a rate of 0.8 g / mL. Potassium oxide activator, stir for 20min to form a uniform slurry; add a large amount of acidic diluent to the slurry in a volume ratio of 1:30, adjust the acidity of the solution to pH=12, continue to stir and age for 1h to prepare an active impregnation solution; ZSM-5 molecular sieve (mass ratio of 0.1 g / g to sulfur powder) was immersed in the active impregnation solution, continuously shaken for 8 hours, centrifuged, washed tw...

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Abstract

The invention discloses a supported active chalcogenide compound as well as a preparation method and application thereof. The preparation method comprises the following steps: adding long-chain or annular inert sulfur powder, selenium powder, tellurium powder and other chalcogenide elementary substance powder particles into a saturated reduction solution, adding a chemical exciting agent to form uniform slurry, diluting and adjusting the pH value to prepare an active dipping solution, dipping a carrier into the active solution, and drying to obtain the active chalcogenide compound. The active chalcogenide compound is in contact with elemental mercury in flue gas or air, mercury is converted into a stable compound, and curing removal or enrichment of mercury is achieved. A long-chain or annular structure of an inert elementary substance is destroyed and broken by strong reduction and chemical excitation, and active sites are fully exposed, so that the activation energy of reaction with mercury is remarkably reduced. Compared with the traditional sulfur powder, the mercury saturation adsorption capacity and adsorption rate are improved by hundreds to thousands of times, and the applicable temperature window range is obviously enlarged. The preparation process is simple, the cost is low, a mercury removal product is environment-friendly and free of secondary pollution, and the method has a good industrial application prospect.

Description

technical field [0001] The invention belongs to the technical field of environmental pollution prevention and gas purification, and in particular relates to a supported active chalcogenide compound and a preparation method and application thereof. Background technique [0002] Mercury has a strong affinity with chalcogenides, which can fix mercury into mercury sulfide or mercury selenide. The ancient alchemy process used this principle. In the Eastern Han Dynasty Wei Boyang's "Chen Tong Qi", there was a saying, "The girl on the river is the most spiritual and most divine, she can fly when she gets fire, she can't see the dust, the ghost hides and the dragon hides, no one knows what exists, and the yellow bud is the root." , "Looking like white, making it Zhu" records. The "Heshang Girl" here refers to mercury, which will evaporate when heated. To fix the mercury, yellow buds (sulfur powder) must be added. After heating, red cinnabar (mercury sulfide) will be formed. The b...

Claims

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Application Information

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IPC IPC(8): B01J20/02B01J20/30B01D53/02
CPCB01J20/0262B01J20/0266B01D53/02B01D2257/602
Inventor 李海龙孟凡悦杨建平屈文麒杨泽群
Owner CENT SOUTH UNIV