CN113058550A - Carbon aerogel microsphere for adsorbing carbonyl sulfide and mercury and preparation method thereof - Google Patents

Carbon aerogel microsphere for adsorbing carbonyl sulfide and mercury and preparation method thereof Download PDF

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CN113058550A
CN113058550A CN202110301992.1A CN202110301992A CN113058550A CN 113058550 A CN113058550 A CN 113058550A CN 202110301992 A CN202110301992 A CN 202110301992A CN 113058550 A CN113058550 A CN 113058550A
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mercury
carbon aerogel
carbonyl sulfide
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张华伟
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Cabernet Suzhou Composite Materials Co ltd
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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    • B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
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    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
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    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
    • B01J20/28014—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their form
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2257/00—Components to be removed
    • B01D2257/30—Sulfur compounds
    • B01D2257/308—Carbonoxysulfide COS
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
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Abstract

The invention provides a carbon aerogel microsphere for adsorbing carbonyl sulfide and mercury and a preparation method thereof, and relates to the field of natural gas treatment. A carbon aerogel microsphere for adsorbing carbonyl sulfide and mercury comprises a core layer and a shell layer; the core layer comprises Sn-Cu active metal and nitrogen-doped carbon aerogel prepared by taking sodium alginate as a raw material. The preparation method of the carbon aerogel microspheres for adsorbing carbonyl sulfide and mercury comprises the following steps: dissolving sodium alginate in deionized water completely, adding nitrogen-containing cross-linking agent and Sn4+Salt, Cu2+Stirring and mixing after salting to form hydrogel microspheres; washing the hydrogel microspheres with deionized water, freeze-drying, and then adding N2Atmosphere(s)And carrying out high-temperature carbonization treatment to obtain the carbon aerogel microspheres for adsorbing carbonyl sulfide and mercury. The carbon aerogel microspheres for adsorbing carbonyl sulfide and mercury provided by the invention are low in cost, and high in removal efficiency by loading Sn/Cu active metal through nitrogen doping modification.

Description

Carbon aerogel microsphere for adsorbing carbonyl sulfide and mercury and preparation method thereof
Technical Field
The invention relates to the field of natural gas treatment, in particular to carbon aerogel microspheres for adsorbing carbonyl sulfide and mercury and a preparation method thereof.
Background
Because of the characteristics of high efficiency, environmental protection and the like, natural gas is being developed rapidly in recent years to meet the requirements of sustainable development and increasingly clean energyThe growing demand. However, a significant portion of the natural gas produced tends to have a certain amount of acid gases (H) present therein2S and COS, etc.) and mercury. Wherein COS, if left untreated, can lead to corrosion of the transmission lines and catalyst poisoning in catalytic processing of natural gas. Mercury in natural gas mainly exists in the form of HgO, and the accumulation of HgO is easy to corrode an aluminum heat exchanger through amalgam corrosion and a liquid metal embrittlement mechanism, so that faults and accidents of a factory are caused.
The desulfurization method of natural gas can be divided into a dry method and a wet method. However, wet desulfurization has the disadvantages of large energy consumption, high operation difficulty, high investment and very complicated process, which are needed for treating the formed desulfurizer waste liquid. The dry desulfurization process is a method for removing sulfides in natural gas by utilizing substances such as activated carbon, molecular sieves, metal oxides, metal organic framework Materials (MOFs) and the like through physical adsorption or chemical reaction. Compared with wet desulphurization, the dry desulphurization process has the advantages of low investment, high skid-mounted degree, small occupied area, large operation flexibility, low energy consumption and the like, and is more suitable for deep removal of gaseous sulfur in natural gas. For the removal of HgO, the main methods at present are direct adsorption removal and indirect oxidation removal. The method for indirectly removing the HgO by oxidation is to oxidize the HgO into oxidized mercury for removal, and the HgO oxidation indirect removal catalyst is mainly divided into a molecular sieve catalyst, a metal oxide catalyst and a metal catalyst.
However, the current research on the removal of COS and Hg from natural gas is mainly to remove a single substance by using different catalysts, and the respective catalysts also have corresponding disadvantages. For example, application number CN201610777977.3 discloses a fine iron oxide desulfurizer and its preparation and application methods, which has high desulfurization precision and sulfur capacity, and simple production process, but the desulfurizer has no good regenerability and is not suitable for high space velocity conditions. Application number CN201710816125.5 discloses a natural gas demercuration adsorbent and a preparation method thereof, wherein the natural gas demercuration adsorbent comprises Al2O382-95% of sulfur, 4-12% of sulfur and 1-6% of copper sulfide. At present, the development of the combined removal of sulfur and mercury in natural gas is carried outThe development trend of dye control has high research value.
In view of the above, the present invention is particularly proposed.
Disclosure of Invention
The first purpose of the invention is to provide carbon aerogel microspheres for adsorbing carbonyl sulfide and mercury.
The second purpose of the invention is to provide a preparation method of carbon aerogel microspheres for adsorbing carbonyl sulfide and mercury.
In order to achieve the purposes, the following technical scheme is adopted:
a carbon aerogel microsphere for adsorbing carbonyl sulfide and mercury comprises a core layer and a shell layer;
the core layer comprises Sn-Cu active metal, and the shell layer comprises nitrogen-doped carbon aerogel prepared by taking sodium alginate as a raw material.
The preparation method of the carbon aerogel microspheres for adsorbing carbonyl sulfide and mercury comprises the following steps:
dissolving sodium alginate in deionized water completely, adding nitrogen-containing cross-linking agent and Sn4+Salt, Cu2+Stirring and mixing after salting to form hydrogel microspheres;
washing the hydrogel microspheres with deionized water, putting the washed hydrogel microspheres into a freeze dryer for freeze drying, and then adding the hydrogel microspheres into N2And carrying out high-temperature carbonization treatment in the atmosphere to obtain the carbon aerogel microspheres for adsorbing carbonyl sulfide and mercury.
Preferably, the mass concentration of the sodium alginate aqueous solution is 0.5-5 wt%, and the mass ratio of the sodium alginate to the nitrogen-containing cross-linking agent is 1:0.1-1: 1.
Alternatively, the mass concentration of the aqueous solution of sodium alginate may be any value between 0.5 wt%, 1 wt%, 1.5 wt%, 2 wt%, 2.5 wt%, 3 wt%, 3.5 wt%, 4 wt%, 4.5 wt% and 5 wt%, and the mass ratio of sodium alginate to the nitrogen-containing crosslinking agent may be any value between 1:0.1, 1:0.2, 1:0.3, 1:0.4, 1:0.5, 1:0.6, 1:0.7, 1:0.8, 1:0.9 and 1: 1.
Preferably, the nitrogen-containing cross-linking agent is one of ethylenediamine, p-phenylenediamine and urea.
Preferably, in the carbon aerogel microspheres for adsorbing carbonyl sulfide and mercury, the loading amount of Sn is 10%, and the mass ratio of Sn/Cu is 0.2-1.0.
Alternatively, the Sn/Cu mass ratio may be any value between 0.2, 0.3, 0.4, 0.5, 0.6, 0.7, 0.8, 0.9, and 1.0.
Preferably, the Sn/Cu mass ratio is 0.2, 0.6 or 1.0.
Preferably, the stirring temperature is 30-60 ℃ and the stirring time is 6-12 h.
Alternatively, the temperature of the stirring may be any value between 30 ℃, 35 ℃, 40 ℃, 45 ℃, 50 ℃, 55 ℃ and 60 ℃, and the time may be any value between 6h, 7h, 8h, 9h, 10h, 11h and 12 h.
Preferably, the temperature of the freeze drying is-60 to-30 ℃ and the time is 24-72 h.
Alternatively, the temperature of the freeze-drying may be any value between-60 ℃, -55 ℃, -50 ℃, -45 ℃, -40 ℃, -35 ℃ and-30 ℃ for any value between 24h, 30h, 36h and 72 h.
Preferably, the temperature of the high-temperature carbonization is 500-;
alternatively, the temperature of the high-temperature carbonization can be any value between 500 ℃, 600 ℃, 700 ℃, 800 ℃ and 900 ℃;
preferably, the high-temperature carbonization temperature is 500 ℃, 700 ℃ or 900 ℃.
The invention has the beneficial effects that:
the carbon aerogel microsphere for adsorbing carbonyl sulfide and mercury provided by the invention has the advantages that the sodium alginate resource serving as the raw material is rich and renewable, the price is low, the sodium alginate resource is easy to obtain, the sodium alginate microsphere is easy to chelate with high-valence metal ions to form an egg box structure of alginic acid-metal aerogel, the regulation and control of a carbon layer structure and the increase of nitrogen-containing functional groups are realized through nitrogen doping modification, the carbonyl sulfide and mercury in natural gas can be jointly removed through loading Sn/Cu active metal, and the removal efficiency is high. The preparation method is clean and efficient, and the process is simple.
Drawings
To more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings that are required to be used in the embodiments will be briefly described below, and it should be understood that the following drawings only illustrate some embodiments of the present invention, and therefore should not be considered as limiting the scope of the present invention.
Fig. 1 shows the removal efficiencies of COS and Hg of the catalysts obtained at high-temperature carbonization temperatures of 500, 700 and 900 deg.c, respectively, in the preparation method of the present invention (the Sn loading is 10%, and Sn/Cu is 0.6).
Fig. 2 shows the removal efficiency of COS and Hg of the catalyst (carbonization temperature is 700 ℃ C. optimum) when the fixed Sn loading is 10% and Sn/Cu is 0.2, 0.6, 1.0 in the preparation method of the present invention.
FIG. 3 is a schematic diagram of nitrogen doping modification in the preparation method of the present invention.
Detailed Description
Embodiments of the present invention will be described in detail below with reference to specific examples, but those skilled in the art will appreciate that the following examples are only illustrative of the present invention and should not be construed as limiting the scope of the present invention. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
The experimental method for evaluating the activity of the catalyst of the invention is as follows:
and (4) evaluating the activity of carbonyl sulfide and mercury removal.
The activity of the catalyst is tested in a fixed bed reactor, the prepared catalyst is placed in a quartz tube reactor, a gas source is regulated, and the gas components in the gas flow are controlled as follows: 30% CH4，20％CO，40％H2400ppm COS and the balance nitrogen. And opening the mercury generator, controlling the water bath temperature of the mercury generator to be 30 ℃, starting to heat up, and introducing into the quartz tube reactor together. After the reaction is balanced, the concentration of COS at the opening is detected by a gas chromatograph and a flame photometric detector, the concentration of Hg is detected by an RA-915 mercury photometer, and the removal efficiency is analyzed and calculated.
And (3) COS evaluation method: the conversion rate can be calculated by measuring the concentration of COS after the reaction. The calculation formula is as follows:
Figure BDA0002986629450000051
evaluation method of Hg: the mercury removal efficiency can be obtained by varying the mercury content before and after the mercury removal. The calculation formula is as follows:
Figure BDA0002986629450000052
example 1
The embodiment provides a preparation method of a nitrogen-doped modified carbon aerogel material for synergistically removing carbonyl sulfide and mercury in natural gas, wherein the carbon aerogel material takes a porous carbon material with a high specific surface area, which is obtained by doping sodium alginate with nitrogen, as a carrier and loads an active metal Sn-Cu; the method is carried out according to the following steps:
(1) 2g of sodium alginate was completely dissolved in 100ml of deionized water. Adding 1g of urea and prepared Sn into the mixed solution4+、Cu2+Stirring the nitrate solution at 60 ℃ for 6 hours to obtain metal ion loaded nitrogen-doped hydrogel;
(2) washing the hydrogel with deionized water for 6 times, freeze drying at-30 deg.C for 24 hr to obtain aerogel, and placing the aerogel in a tubular furnace at 100% N2And carbonizing for 3 hours at 700 ℃ (the temperature rise rate is set to be 5 ℃/min) under the atmosphere to prepare the metal oxide supported nitrogen-doped carbon aerogel adsorption material.
In step (1), the loading of Sn was fixed at 10%, and Sn/Cu was 0.6.
The catalyst prepared in this embodiment was subjected to an evaluation experiment for removing activity of COS and Hg.
And (4) evaluating the desulfurization and demercuration activity. The experimental conditions are as follows: space velocity of 30000h-1The temperature was 200 ℃. The simulated gas comprises the following components: 30% CH4，20％CO，40％H2400ppm COS and the balance nitrogen. Supplying water using saturator system and using relative humidity(RH) represents the water content. The Hg generator provides Hg in simulated gas. The total flow rate was controlled to 1L/min using a mass flow controller.
The experimental results are as follows: the removal efficiency of COS can reach 97%, the removal efficiency of Hg can reach 95%, and the activity evaluation experiment efficiency is shown in figures 1 and 2.
The principle schematic diagram of nitrogen doping modification of the present application is shown in fig. 3.
Example 2
This example differs from example 1 in that: the carbonization temperature in the step (2) is 900 ℃.
The carbon aerogel material prepared in this example was subjected to an evaluation experiment for the removal activity of COS and Hg. The experimental result shows that the removal efficiency of COS can reach 89%, and the removal efficiency of Hg can reach 87%.
Example 3
This example differs from example 1 in that: the carbonization temperature in the step (2) is 500 ℃.
The carbon aerogel material prepared in this example was subjected to an evaluation experiment for the removal activity of COS and Hg. The experimental result shows that the removal efficiency of COS can reach 91 percent, and the removal efficiency of Hg can reach 90 percent.
As shown in fig. 1, it can be known from examples 1 to 3 that the carbonization temperature in the preparation process of the carbon aerogel material should be controlled at 700 ℃, different carbonization temperatures have an important influence on the formation of the pore structure of the carbon material in the preparation process of the coal tar material, and the quality of the pore structure of the material has a close relationship with the load of the subsequent metal, so as to finally influence the efficiency of the catalyst for removing COS and Hg cooperatively.
Example 4
This example differs from example 1 in that: the nitrogen-containing cross-linking agent used in the step (1) is ethylenediamine.
The carbon aerogel material prepared in this example was subjected to an evaluation experiment for the removal activity of COS and Hg. The experimental result shows that the removal efficiency of COS can reach 97 percent, and the removal efficiency of Hg can reach 95 percent.
Example 5
This example differs from example 1 in that: changing the Sn/Cu value in the step (1) to 0.6 to 0.2.
The carbon aerogel material prepared in this example was subjected to an evaluation experiment for the removal activity of COS and Hg. The experimental result shows that the removal efficiency of COS can reach 94 percent, and the removal efficiency of Hg can reach 91 percent.
Example 6
This example differs from example 1 in that: changing Sn/Cu in the step (1) to Sn/Cu of 0.6 to 1.0.
The carbon aerogel material prepared in this example was subjected to an evaluation experiment for the removal activity of COS and Hg. The experimental result shows that the removal efficiency of COS can reach 90 percent, and the removal efficiency of Hg can reach 90 percent.
Example 7
This example differs from example 1 in that: changing 1g of urea in the step (1) into 0.2g of urea.
The carbon aerogel material prepared in this example was subjected to an evaluation experiment for the removal activity of COS and Hg. The experimental results show that the removal efficiency of COS is 86% and the removal efficiency of Hg is 83%.
As shown in fig. 2, it can be seen from examples 1, 4, 5 and 6 that the carbon aerogel material catalyst prepared has high efficiency in removing COS and Hg from natural gas synergistically when the loading amount of Sn is 0.1 and the Sn/Cu is 0.6.
Finally, it should be noted that: the above embodiments are only used to illustrate the technical solution of the present invention, and not to limit the same; while the invention has been described in detail and with reference to the foregoing embodiments, it will be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; and the modifications or the substitutions do not make the essence of the corresponding technical solutions depart from the scope of the technical solutions of the embodiments of the present invention.
Furthermore, those skilled in the art will appreciate that while some embodiments herein include some features included in other embodiments, rather than other features, combinations of features of different embodiments are meant to be within the scope of the invention and form different embodiments. For example, in the claims above, any of the claimed embodiments may be used in any combination. The information disclosed in this background section is only for enhancement of understanding of the general background of the invention and should not be taken as an acknowledgement or any form of suggestion that this information forms the prior art already known to a person skilled in the art.

Claims (10)

1. A carbon aerogel microsphere for adsorbing carbonyl sulfide and mercury is characterized by comprising a core layer and a shell layer;
the core layer comprises Sn-Cu active metal, and the shell layer comprises nitrogen-doped carbon aerogel prepared by taking sodium alginate as a raw material.
2. A method for preparing the carbon aerogel microspheres for adsorbing carbonyl sulfide and mercury according to claim 1, comprising:
dissolving sodium alginate in deionized water completely, adding nitrogen-containing cross-linking agent and Sn4+Salt, Cu2+Stirring and mixing after salting to form hydrogel microspheres;
washing the hydrogel microspheres with deionized water, freeze-drying, and then adding N2And carrying out high-temperature carbonization treatment in the atmosphere to obtain the carbon aerogel microspheres for adsorbing carbonyl sulfide and mercury.
3. The preparation method of claim 2, wherein the mass concentration of the aqueous solution of sodium alginate is 0.5-5 wt%, and the mass ratio of sodium alginate to the nitrogen-containing cross-linking agent is 1:0.1-1: 1.
4. The method according to claim 2, wherein the nitrogen-containing crosslinking agent is one of ethylenediamine, paraphenylenediamine, and urea.
5. The preparation method of claim 2, wherein the carbon aerogel microspheres for adsorbing carbonyl sulfide and mercury has a loading of Sn of 10% and a Sn/Cu mass ratio of 0.2-1.0.
6. The production method according to claim 5, wherein the Sn/Cu mass ratio is 0.2, 0.6, or 1.0.
7. The method of claim 2, wherein the stirring is carried out at a temperature of 30-60 ℃ for 6-12 hours.
8. The method of claim 2, wherein the freeze-drying is carried out at a temperature of-60 to-30 ℃ for 24 to 72 hours.
9. The preparation method according to claim 2, wherein the high temperature carbonization temperature is 500-900 ℃, the heating rate is 5 ℃/min, and the time is 2-5 h.
10. The method according to claim 9, wherein the high-temperature carbonization temperature is 500 ℃, 700 ℃, or 900 ℃.
CN202110301992.1A 2021-03-22 2021-03-22 Carbon aerogel microsphere for adsorbing carbonyl sulfide and mercury and preparation method thereof Pending CN113058550A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113877529A (en) * 2021-11-02 2022-01-04 浙江工业大学 Preparation method and desulfurization application of cobalt-doped carbon aerogel
CN114653338A (en) * 2022-03-21 2022-06-24 青岛理工大学 Simultaneously removing CS in natural gas2Hg-blended nitrogen-doped metal ion loaded adsorbent and preparation method thereof

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113877529A (en) * 2021-11-02 2022-01-04 浙江工业大学 Preparation method and desulfurization application of cobalt-doped carbon aerogel
CN114653338A (en) * 2022-03-21 2022-06-24 青岛理工大学 Simultaneously removing CS in natural gas2Hg-blended nitrogen-doped metal ion loaded adsorbent and preparation method thereof
CN114653338B (en) * 2022-03-21 2024-03-19 青岛理工大学 Simultaneously removing CS in natural gas 2 Nitrogen-doped metal ion loaded adsorbent with Hg and preparation method thereof

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