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A kind of preparation method of high temperature CO2 calcium-based adsorbent doped with silicon nitride

A calcium-based adsorbent and silicon nitride technology, which is applied in chemical instruments and methods, separation methods, and other chemical processes, can solve the problems of reduced effective content of CaO, decreased cycle adsorption performance, and reduced cycle adsorption performance. High efficiency, high adsorption performance, and easy regeneration

Active Publication Date: 2019-06-11
KUNMING UNIV OF SCI & TECH
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Problems solved by technology

At present, researchers have studied methods such as adsorption, membrane separation, and ammonia water absorption to mitigate CO 2 However, due to the disadvantages of complex operation, low adsorption performance and high consumption, the above methods are not widely used.
Because CaO is cheap and easy to obtain, wide source, and high adsorption capacity, calcium-based adsorbent is the most widely used adsorbent at present, but calcium-based adsorbent itself also has many shortcomings. On the one hand, calcium-based adsorbent The sintering phenomenon of the adsorbent after repeated calcination leads to the decrease of the specific surface area and the decrease of the cycle adsorption performance; on the other hand, the industrial waste gas contains a certain amount of SO 2 , CaO and SO 2 CaSO produced by the reaction 4 It cannot be regenerated under the conditions of carbonation / calcination separation, so that the effective content of CaO is reduced, and the CO 2 Decreased cycle adsorption performance

Method used

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  • A kind of preparation method of high temperature CO2 calcium-based adsorbent doped with silicon nitride

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] Embodiment 1: with calcium gluconate Ca (C 6 h 11 o 7 ) 2 As CaO precursor, doped with Si prepared from sucrose 3 N 4 Preparation of doped high temperature CO 2 Calcium based sorbent.

[0042] A high-temperature CO doped with silicon nitride 2 The preparation method of calcium-based adsorbent specifically comprises the following steps:

[0043] (1) Put wood powder sucrose in a vacuum tube furnace, and feed inert gas N with a flow rate of 150mL / h into the tube furnace 2 , at a temperature of 700°C, the inert gas N 2 Carbonization reaction in the atmosphere for 2h to obtain carbon powder;

[0044] (2) Mix the carbon powder and tetraethyl orthosilicate evenly in step (1), wherein the C:Si molar ratio of the carbon powder and tetraethyl orthosilicate is 1.5:1, and add it dropwise at a stirring speed of 500r / min Ammonia water (the solid-to-liquid ratio g:mL of carbon powder and ammonia water is 1:0.5, NH in ammonia water 4+ The concentration of the solution is 1.47 ...

Embodiment 2

[0049] Embodiment 2: calcium gluconate Ca (C 6 h 11 o 7 ) 2 It is a CaO precursor, doped with Si prepared from red charcoal powder 3 N 4 Preparation of calcium-based sorbent.

[0050] A high-temperature CO doped with silicon nitride 2 The preparation method of calcium-based adsorbent specifically comprises the following steps:

[0051] (1) Put the mahogany charcoal powder in a vacuum tube furnace, and feed an inert gas N with a flow rate of 150mL / h into the tube furnace 2 Exhaust the air inside, and carbonize in an inert gas Ar atmosphere for 3 hours at a temperature of 750°C to obtain carbon powder;

[0052] (2) Mix the carbon powder and tetraethyl orthosilicate evenly in step (1), wherein the C:Si molar ratio of the carbon powder and tetraethyl orthosilicate is 1.5:1, and add it dropwise at a stirring speed of 600r / min Ammonia water (the solid-to-liquid ratio g:mL of carbon powder and ammonia water is 1.3:0.8, NH in ammonia water 4+ The concentration is 1.56mol / L), ...

Embodiment 3

[0057] Embodiment 3: take calcium gluconate as the CaO precursor, doped with Si prepared from bagasse 3 N 4 Preparation of calcium-based sorbent.

[0058] A high-temperature CO doped with silicon nitride 2 The preparation method of calcium-based adsorbent specifically comprises the following steps:

[0059] (1) Put the wood powder bagasse in a vacuum tube furnace, and feed an inert gas N with a flow rate of 150mL / h into the tube furnace 2 Exhaust the air inside, at a temperature of 800°C, the inert gas N 2 Carbonization reaction in the atmosphere for 4h to obtain carbon powder;

[0060] (2) Mix the carbon powder and tetraethyl orthosilicate evenly in step (1), wherein the C:Si molar ratio of the carbon powder and tetraethyl orthosilicate is 1.5:1, and add it dropwise at a stirring speed of 700r / min Ammonia water (the solid-to-liquid ratio g:mL of carbon powder and ammonia water is 1.6:1, NH in ammonia water 4+ The concentration is 1.65mol / L), the pH value of the mixed so...

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Abstract

The invention discloses a preparation method of silicon nitride-doped high-temperature CO2 calcium-based adsorbent and belongs to the field of CO2 high-temperature adsorption and separation. The preparation method comprises: using tetraethyl orthosilicate and wood powder as materials to prepare silicon nitride precursor by using sol-gel carbon thermal reduction via one-step process, using silicon nitride from the wood powder as an inertial support material, and preparing high-temperature CO2 calcium-based adsorbent via carbonizing, dipping, nitriding, calcining and doping; the doped calcium-based adsorbent has significantly improved CO2 cyclic adsorbing property. The materials herein are easy to obtain, the preparation method is simple, the CO2 adsorbing property is good, the problems of sintering proneness, low CaO conversion rate and lower adsorbing capacity of the high-temperature calcium-based adsorbent after multiple carbonation / calcining cycles are well improved, and the preparation method has a promising development prospect.

Description

technical field [0001] The invention relates to a high-temperature CO doped with silicon nitride 2 Preparation method of calcium-based adsorbent, belonging to CO 2 High temperature adsorption and separation field. Background technique [0002] Climate change caused by the greenhouse effect has become a global problem, CO 2 It is an important factor causing the greenhouse effect. 2014 Global CO 2 Emissions were 32.3 billion tons, although in 2015 CO 2 China's emissions have stabilized, even showing a 6% decline, but climate scientists have also warned that this stabilization is only temporary. At present, researchers have studied methods such as adsorption, membrane separation, and ammonia water absorption to mitigate CO 2 However, due to the disadvantages of complex operation, low adsorption performance, and high consumption, the above methods are not widely used. Because CaO is cheap and easy to obtain, wide source, and high adsorption capacity, calcium-based adsorbe...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J20/04B01J20/30B01D53/02
CPCB01D53/02B01D2253/10B01D2253/1124B01D2257/504B01J20/0259B01J20/041B01J2220/4806B01J2220/4812B01J2220/4825Y02C20/40
Inventor 陕绍云张亚芹何善传贾庆明蒋丽红苏红莹
Owner KUNMING UNIV OF SCI & TECH
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